ANKA Annual Report 2013 · ANKA Annual Report 2013 ANKA SYNCHROTRON RADIATION FACILITY ANKA Annual...

www.kit.eduKIT – University of the State Baden-Wuerttemberg and National Laboratory of the Helmholtz Association www.kit.edu

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ANKA SYNCHROTRON RADIATION FACILITY

www.anka.kit.edu

ANKA Annual Report 2013

ANKA is the Synchrotron Radiation Facility at the Karlsruhe Institute of Technology (KIT). As one of the large-scale facilities within the Helmholtz Association of German Research Centres ANKA is part of the national and European infrastructure offered to both academic and commercial scientifi c users for the performance of research and technological development activities.

Karlsruhe Institute of Technology (KIT) is the result of the merger in 2009 of the Universität Karlsruhe (TH) with Forschungszentrum Karlsruhe (FZK). The fusion of the two institiutions represents the logical continuation of the close long-standing cooperation between both research and education partners. With approx. 9.300 employees and an annual budget of around 750 million Euros, KIT is one of the world-wide leading centres in innovative science and technology.

With its 18 research centres, over 36,000 employees, and an annual budget of approx. 4 billion Euros, the Helmholtz Association of German Research Centres is Germany‘s largest research organisation. The Helmholtz Association contributes to the solution of the grand challenges of society, science and the economy by combining research and technology development with perspectives for innovative applications and provisions for tomorrow‘s world.

Karlsruhe Institute of Technology (KIT)ANKA - Synchrotron Radiation FacilityCampus NorthHermann-von-Helmholtz-Platz 176344 Eggenstein-Leopoldshafen

Directors: Prof. Dr. Tilo Baumbach,Prof. Dr. Clemens Heske,Prof. Dr. Anke-Susanne Müller

www.anka.kit.edu

2013 ANKA ANNuAl RepoRt | 3

Dear ANKA users, Colleagues and Supporters,

2013 has been an exciting year for ANKA! With the celebration of ten years of ANKA user operation, new staff, new beamlines/laboratories, and new meeting facilities, ANKA has taken further steps in the integration of its synchrotron radiation research activities and off-line laboratory capabilities into the research infrastructure at KIt. Furthermore, after the successful evaluation (“poF III”), not only of ANKA, but of the entire Helmholtz-Association of German Research Centers, ANKA is firmly established as a unique user facility within the German research landscape, especially with regard to the integration of research, technical innovation and education.

As a central KIt research facility, ANKA has further expanded its technical and methodological infrastructure with the completion of facilities for biological sample preparation and characterization (BIolab), detector development (DeteCtoRlab), and off-line X-ray diffraction and imaging. the completion in 2013 of the new conference rooms located in the west extension has given ANKA a long-needed venue for meetings and seminars.

planning and acquisition of the major aspects of the CAt-ACt beamline were completed, and the east side of the ANKA hall was extended to accommodate the new beamline. In early 2014, the first components (front-end) were delivered and, at the time of writing, the installation of the hutches is completed. In addition the specification and design stages of X-SpeC, which will provide soft and hard X-ray radiation for X-ray spectroscopy and in-situ studies, were completed in 2013.

Significant progress was made on the new compact versatile linear accelerator Flute (Ferninfrarot linac- und test-experiment/Far-infrared linac and test experiment), with 2013 seeing the refurbishment of the Flute experimental hall, control room, and ancillary areas, as well as the installation of the first accelerator components and the first successful test of the electron gun at the synchrotron elSA in Bonn.

one major activity in 2013 was the preparation and evaluation of plans for the third round of program-oriented Funding (poF III), which represents the main funding mechanism for German large-scale user facilities such as ANKA. Many of you were involved in this process – either directly, or simply through the great research you perform or have performed at ANKA. We greatly appreciate the help and support we have received from all of ANKA’s constituents – as users and their representatives (many thanks to the ANKA

users Committee!), as colleagues and volunteers to review our experimen-tal portfolio, as supporters and representatives in the numerous committee meetings, and last, but certainly not least, as ANKA staff – working extra hard to maintain high-quality user operation all-the-while the poF evalua-tion was underway. thank you very much for all your hard work and help!

As you will see from the Annual Report, ANKA is growing – in experimental capabilities, number of users, in output, and in many other metrics that can be applied. one factor becomes obvious: that ANKA is driven by a vibrant community of users, staff, and supporters, and that its unique situation of being embedded in a world-class infrastructure environment at KIt makes it a very special place to be for all of us!

Again, a heartfelt “thank you” to all our staff, colleagues, and especially our users, who in 2013 have again given their (your!) support to ensure that ANKA remains at the forefront of synchrotron radiation research - we look forward to a successful future together!

tilo Baumbach, Anke-Susanne Müller and Clemens Heske

ANKA News Snapshots in 2013 .........................6

Beamlines at ANKA .........................10

ANKA User Operation .........................12

Accelerator Science and Technology .........................16

KAPTURE .........................19

EOS .........................20

Compton .........................22

Low Emittance .........................24

FLUTE .........................25

Insertion Device Development .........................28

XAS .........................34

SUL-X .........................36

IR1 .........................40

IR2 .........................42

WERA .........................44

INE .........................46

UV-CD12 .........................48

NANO .........................50

SCD .........................52

PDIFF .........................54

MPI. ........................56

FLUO .........................57

TOPO-TOMO .........................58

IMAGE/XMIC .........................60

LIGA I, II, III .........................62

BioLab .........................66

KNMF Laboratory for Synchrotron Characterisation .........................68

ANKA Seminars 2013 .........................72

Publications 2013 .........................74

ANKA Annual Report 2013

Contents


sentative sample quantities which are required for in-depth mineralogical analyses of heterogeneous slag material can be collected with a high level of detail. All in all the jury was impressed by the article from the altogether nine German and Slovakian authors: “the article impresses by its large amounts of environmentally relevant data and analyses, which make the article exceptionally significant.” Since there are also disused mines in Germany with similar environmental problems, an extensive data gathering and analyses makes equal sense to examine the mineralogy and geochemistry of mining slag and if necessary analytically support renovation steps.

Nature: X-ray tomography on a living Frog embryoMay, 2013: Motion of individual cells within developing frog embryos resolved/X-ray tomography based on diffraction rather than absorp-tion/New methods for developmental biology

Classical X-ray radiographs provide information about internal, absorptive structures of organisms such as bones. Alternatively, making use of phase contrast, X-rays can also image soft tissues, for example during early embryonic development of vertebrates. Related to this a new X-ray method was presented recently in a Nature article published by a German-Ameri-can-Russian research collaboration team led by KIt. the researchers from KIt, Northwestern university, tomsk polytechnic and Argonne National laboratory recorded time-lapse sequences of developing embryos of the African clawed frog (Xenopus laevis) at a resolution sufficient to map individual cells. Rather than using classical absorption contrast the method relies on the phase-coherent diffraction of X-rays. three-dimensional reconstruction combined with flow-analysis enabled the cell tissue motion during gastrulation to be investigated. (DoI: 10.1038/nature12116).

Scientists examine fossil excrement using synchrotron X-ray microtomographyDecember 2013: The dung of herbivorous dinosaurs was most likely digested by cockroaches

the dung of herbivorous dinosaurs was most likely digested by cockroaches, as shown by Dr. peter Vršanský (Slovakian Academy of Sciences), Dr. thomas van de Kamp (IpS Imaging Group) and colleagues in an article recently published in the journal ploS oNe.Fossil excrement of a ca. 130 million years old cockroach encased in lebanese amber was examined using synchrotron X-ray microtomography at ANKA’s topo-toMo beamline. this non-invasive technique facilitates three-dimensional imaging of millimeter-sized structures. It became apparent that the droppings contained large particles of wood, whose appearance strongly suggested pre-digestion by a large herbivore. As flies and dung beetles were virtually non-existent during the time period, it seems plausible that cockroaches owned their ecological niche.

Atsushi Momose gives a talk at ANKAJanuary, 2013: Atsushi Momose: X-ray Phase Imaging Based on Grating Interferometry

Since the 1990s X-ray phase imaging methods have enabled us to observe weakly absorbing objects such as biological soft tissues and polymers. techniques such as X-ray talbot interferometry and X-ray talbot-lau interferometry have been attracting attention as new methods for X-ray phase imaging, especially because of their compatibility with laboratory sources, while other X-ray phase imaging have been performed at synchro-tron facilities. there is thus a big motivation to advance towards practical implementation of X-ray grating interferometry for clinical diagnosis and non-destructive testing. prof. Momose, supported by the Japan Science and technology Agency (JSt), has been developing medical systems for diagnosis of articular rheumatism and breast cancer in collaboration with a medical equipment manufacturer. Such a system is installed in a hospital and is now being used for clinical studies with patients. In addition, the first prototype developed at Momose’s laboratory is now provided for research and non-destructive testing by people from industry. In his talk prof. Momose gave details of the various developments with grating interferometry in his group including other applications with synchrotron radiation, such as microscopic talbot interferometry and four-dimensional X-ray phase tomography.

Abiturientinnen-tag at KItJanuary, 2013: Women and Science

once again this year beamline scientist Dr. Sondes Bauer presented her work at the NANo beamline to a group of young women visitors and demonstrated the complexities and automation of the state-of-the-art diffractometer in the experimental hutch. the girls were also given insights into Dr. Bauer’s research work and the application of synchrotron radiation in the nanosciences. Nicole Hiller, phD student at ANKA, gave a short presentation and overview of the world of synchrotrons, took the participants on a tour of the ANKA hall and answered questions.

Hawley Medal for ANKA users

April, 2013: The mineralogists and ANKA users Dr. Bronislav Lalinkská and Prof. Dr. Juraj Majzan receive an award by the renowned journal “The Canadian Mineralogist”

Since 1995 the Mineralogical Association Canada (MAC) honors the best article of the year in “the Canadian Mineralogist” with the Hawley Medal. From altogether 115 articles published in 2012 a three-person jury chose “Mineralogy of weathering products of Fe-As-Sb mine wastes and soils at several Sb deposits in Slovakia” for the award.together with their colleagues, Borislava lalinská-Voleková (uni. of Bratislava) and Juraj Majzlan (uni. of Jena) have investigated the slag of disused antimony mines in Slovakia. their main interest lay in the two elements arsenic and antimony and their influence on the environment. using microfocus X-Ray diffraction analysis (µ-XRD) the scientists prove in their award-winning article that under the prevailing physico-chemical parameters arsenic remains mobile and therefore has greater impact on the environment while antimony remains effectively bound in the slag. the analyses were carried out at the Sul-X beamline at ANKA together with Dr. Ralph Steininger and Dr. Jörg Göttlicher. High intensity focused X-Rays, as generated at synchrotron radiation sources like ANKA, make it possible to measure hundreds of data points in just few days. thus, statistically repre-

ANKA News Snapshots in 2013

8

User Operation

Beamlines in operation ANKA user operation

User Operation Appendix Lab ReportBeamline ReportAccelerator Report


Beamline Technical Application Status

LIGA I X-ray lithography, mask fabrication, patterning of thin microstructures Operational

LIGA II Deep X-ray lithography Operational

LIGA III ultra-deep X-ray lithography In commissioning


NANOHigh resolution X-ray diffraction and surface and interface scattering for in-situ processes investigation. Spectroscopic imaging using hard X-ray full field micros-copy

in commissioning with users

SCD Single crystal diffraction, SAD/MAD, ex-situ characterisation of (nanostructured) surfaces and interfaces

Operational

PDIFF X-ray powder diffraction, in-situ XRD Operational

MPI In-situ characterization of (nano-structured) surfaces, interfaces, thin films and multilayers with XRD, XRR, GID GISAXS, single crystal and powder diffraction.

Operational

FLUO X-ray fluorescence analysis (XRF), X-ray fluorescence microprobe (µ-XRF), total X-ray reflection fluorescence (tXRF)

Operational

TOPO-TOMO topography, tomography, radiographyOperational (TOPO)

In commissioning(TOMO)

IMAGE X-ray imagingUnder construc-tion


XAS extended X-ray absorption fine structure (eXAFS), X-ray absorption near-edge structure (XANeS), Q-XAFS

Operational

SUL-X X-ray diffraction (XRD), X-ray fluorescence analyis (XRF), X-ray absorption (XAFS),μ-focus, Q-XAFS

Operational

IR1 Infrared/tHz spectroscopy, ellipsometry (extreme conditions microspectroscopy under construction)

Operational

IR2 Infrared/tHz spectroscopy, microspectroscopy, imaging(near-field nanospectroscopy under construction)

Operational

WERA Soft X-ray spectroscopy, microscopy, and spectromicroscopy: peS, NeXAFS, SXMCD, imaging (peeM), µ-peS, µ-NeXAFS, µ-SXMCD

Operational

INE Spectroscopy of actinide samples, multiple spectroscopy techniques, microscopy, diffraction methods

Operational

UV-CD12 VuV / uV circular dichroism spectroscopy, oriented circular dichroism spectroscopy (oCD)

Operational

CAT-ACT High energy beamline for CAtalysis and ACtinide research Under construction

X-SPEC Soft and Hard X-ray Spectroscopy Under construction

10

Beamlines at ANKACurrent operational status

Microfabrication

Spectroscopy

Scattering and Imaging

User Operation

Beamlines in Operation | ANKA User Operation

Appendix Lab ReportBeamline ReportAccelerator Report


Michael Hagelstein: [email protected]

2013 in hours in %

user operation at 2.5 GeV 2404 57

Special user operation 373 9

Injection (0.5 GeV) 154 4

Start-up 490 12

Machine physics 760 18

Sum 4181 100

Figure 1: Summary of hours delivered for the various operational states of the ANKA machine

Figure 2: Distribution of proposals for 2013, classified according to affiliation of user groups

Figure 3: Distribution of proposals for 2013 classified according to the scientific fields

Figure 4: Number of publications from ANKA since 2005

User Operation

Beamlines in Operation | ANKA User Operation

Appendix Lab ReportBeamline ReportAccelerator Report

ANKA User OperationANKA offers several operation modes for users. For the majority of time the facility is operated at 2.5 GeV (uo: user operation) and to a lesser extent at lower energies of stored electrons (Suo: special user operation). electron en-ergies of 1.3 GeV, for example, are suited for the production of short pulses, which are both used for the generation of coherent tHz radiation and for ul-trafast X-ray science. other operation modes of the facility include machine operation (maintenance and development) and time for the assessment of safety systems.

In 2013 the storage ring was scheduled to provide approx. 110 days of 2.5 GeV user operation and a further 17 days for special user operation, at 1.3 GeV with short bunches. of the 110 days scheduled for regular user operation 13 days were lost due to two severe power cuts to the complete KIt north campus, which led to extended damage-recovery and start-up delays. Howev-er, by re-scheduling some of the planned machine-physics and start-up days it was possible to recover some of the lost time, so that finally the delivered to scheduled beam time was close to 96%. A summary of the number of hours delivered for the various operational modes is shown in Figure 1.

CALIPSO - Coordinated Access to Lightsources to Promote Standards and Optimization

the CAlIpSo integrated infrastructure initiative provides since June 2012 sup-port for eu funded experiments to 14 european synchrotrons and free electron lasers, including ANKA. the transnational Access program offers travel and subsistence for users of member states and associated countries from outside Germany. the program will last until May 2015. Since the HoRIZoN2020 of the european Community has changed emphasis, a follow-up project of a sim-ilar kind as a union between synchrotrons will not be applied for. the ANKA user office welcomes applications for support through the CAlIpSo initiative until May 2015. Afterwards our users are requested to look into eC projects centered on major societal challenges (QualityNano, talisman, euminafab, Bio-struct-X, etc.) and request support through their transnational access schemes. .

KNMF Laboratory for Synchrotron CharacterisationANKA is engaged in the KNMF activities via its laboratories for Microfab-rication and Synchrotron Characterisation and thus provides a dedicated user service for the Nanoscience and Microtechnology user communities. Beamtime is accessible via the proposal portals of the KNMF (in particular in combination with other KNMF technologies) and of ANKA, and beamtime allocation is based on a peer-review process.

In 2013, the pool of ANKA beamlines accessible via the KNMF proposal portal included infrared/tHz spectroscopy and ellipsometry (IR1 beamline), polycrystalline/powder X-ray diffraction (pDIFF beamline), and X-ray absorp-tion spectroscopy (XAS beamline). Furthermore, the commissioning of the IR2 beamline (infrared/tHz microspectroscopy) was completed and user op-eration commenced. In addition the Institute for Solid-State physics (IFp) at KIt owns and operates the soft x-ray analytics facility WeRA at ANKA, a facility designed for combinatory studies of the electronic and magnetic structure and microstructure, which have particular promise for strongly correlated, thin-film, and/or nanoscale materials. user communities can access WeRA via peer review through the ANKA and KNMF portals and also through the eu programme QNano.

the portfolio of beamlines available through the KNMF will, in the future, be complemented by the X-SpeC beamline which will cover a broad energy range (approx. 80 eV to 15 keV), bringing together soft and hard X-rays in one beamline, and combining them with cutting-edge spectroscopy techniques. these methods will extend KNMF’s spectroscopy portfolio with capabilities such as hard X-ray photoelectron spectroscopy (HAXpeS) and resonant inelastic soft X-ray scattering (soft RIXS).

2013 ANKA-KNMF User Meetingthe 2013 users’ meeting took place on the 26th and 27th September in Bruchsal, a village close to the ANKA site. this meeting was the fifth to be organized together with the Karlsruhe Nano Micro Facility (KNMF). the two-day meeting was attended by almost two hundred participants and reviewed the status and technical progress of both facilities and presented user reports from current research. A plenary session to mark ten years of ANKA user operation was organized on the first day of the meeting and the session was closed by professor eberhard umbach, who, in the very week of the user meeting, was retiring as president of KIt.

Figure 5: Participants at the 2013 ANKA-KNMF User Meeting

X-Ray and THz/IRTechnology 6%

14

Accelerator Report

Accelerator Science and technology

Insertion Device Development

Accelerator Report Appendix Lab ReportBeamline ReportUser Operation


Feedback system and timingone example is the introduction of the new two-dimensional bunch-by-bunch (BBB) feedback system (see this Annual Report). this device was quickly commissioned as it was fully compatible with the chosen ANKA control system and communication protocol. Based on the great success and experience of the two-dimensional BBB, the third dimension of beam stability control is planned to be added in the near future. Detailed studies of beam stability and dynamics have led to several state-of-the-art mea-surement stations being developed. For this the machine core distributed timing system was extended so that all timing signals common to the operation of the machine are now available at every diagnostic station. the distributed timing system has a timing resolution and synchronization in the order of picoseconds. Diagnostics and machine physics data can now be easily correlated across all stations. Furthermore, the timing system handles time stamping and post-mortem triggers. With newly installed beam-po-sition monitors, new bunch-by-bunch feedback system, and the planned installation of RF low-level electronics a fully automated post-mortem data capture will allow fast identification of causes for beam loss and ease trou-ble shooting.

New database CassandraMachine operational data is being read out from approximately 25,000 data nodes at a data rate between 1 and 10 Hz for 24 hours each day. to store all this data for over a ten-year period an Apache Cassandra database, an open source distributed database management system was commissioned. this NoSQl database is designed to handle large amounts of data across many servers thus providing high availability and complete scalability with no single point of failure.

Figure 1: Distribution of delivered beam time in 2013 (January-December)

Collaborations/Contributorsaquenos GmbH, Baden-Baden, GermanyCosylab, ljubljana, SloveniaDimtel, Inc, San Jose, uSA

Contributors/Authors N. J. Smale, e. Hertle, e. Huttel, W. Mexner, A.-S. Müller, S. Marsching, I. KriznarSelected PublicationsN. J. Smale, e. Hertle, e. Huttel, W. Mexner, A.-S. Müller (KIt, Karlsruhe), S. Marsching (aquenos GmbH), I. Kriznar (Cosylab), the ANKA control system: on a path to the future, ICAlepCS 2013, San Francisco, California, uSA, MoppC099 (2013).S. Marsching, aquenos GmbH, Scalable archiving with the Cassandra ar-chiver for CSS, ICAlepCS 2013, San Francisco, California, uSA, tuppC004 (2013).

Accelerator Report

Accelerator Science and Technology | Insertion Device Development

Accelerator Science and Technology

Introduction to ANKA storage ring operation and accelerator science and technology

the accelerator team at the ANKA synchrotron radiation facility can report significant progress in the storage ring and machine operation in 2013. Several upgrades were implemented and new, exciting technologies have been developed and implemented for control, diagnostics, and detection of electrons and photons. Research collaborations between ANKA and various KIt-wide institutes with expertise in fields such as high speed detectors and high speed electronics, have resulted in advances in picosecond timescale, broadband, high throughput, high speed data acquisition. this opens new windows for diagnostics of compressed electron packages (so-called bunches) within a storage ring such as ANKA.

Academic education is an integral part of life at ANKA: as part of the accelerator education and training program at KIt a small fraction of the machine development time in 2013 was provided for hands-on tutorials for students. Additionally in 2013 six dissertations were completed within the field of accelerator physics and technology. phD students provide and provided important contributions to the success of the ongoing research projects and were partially supported via funding by the BMBF Verbund-forschung under contract numbers 05K10VKC/05K13VKA, by the Initiative and Networking Fund of the Helmholtz Association under contract number VH-NG-320, and the eC-funded Marie Curie Initial training Network lA3Net.

the year 2013 was also distinguished by the preparations for the new programme-oriented funding period, poF-III, of the Helmholtz Association. one major contribution in tune with the development of new technologies and experimental methods at KIt is the new linac-based test facility Flute (Ferninfrarot linac- und test-experiment / far infrared linac- and test-ex-periment). Flute will be located near the ANKA storage ring and the project is now well advanced.

the following pages of the Annual Report 2013 cover the activities of the accelerator team and provide a few highlights of research and developments and a look into ongoing and future projects.

Overview of the Accelerator Reportthe Accelerator Report in the present ANKA Annual Report 2013 is structured as follows: it begins with the ANKA storage ring operation, upgrades and refurbishment in 2013, and new developments such as the new digital feedback system for bunch-by-bunch (BBB) control. the report also describes new possibilities to capture short detector signals in the picosecond range, for example, detection of picosecond timescale terahertz signals, which was possible by a KIt-wide research collaboration between several institutes. While the former concentrates on providing new technology to measure all radiation signals generated by each bunch in the storage ring ANKA, also non-invasive electro-optical diagnostics to be able to measure the longitudinal bunch length in a single-shot mode was achieved, systematically measured, and analyzed. Further developments within the accelerator team consider a new compact setup for measuring the elec-tron energy via Compton backscattering of laser photons, the investigation and development of insertion devices, and a feasibility study to show potential improvements of ANKA towards a low emittance storage ring, while maintaining the source points for radiation for the beamlines. Finally a look into the future, the setup of a new linear accelerator Flute in a neighboring building at the ANKA synchrotron radiation facility is described. the acceler-ator team at KIt is an integral part of the ongoing accelerator and research development (ARD) in Germany and within the Helmholtz ARD Distributed test Facility (ARDtF).

Selected PublicationAccelerator Report in the ANKA Annual Report 2012

ANKA storage ring operation and upgrades in 2013ANKA is generally operated at an electron kinetic energy of 2.5 GeV with an injected beam current of nominally 200 mA and a lifetime of around 20 hours. In addition, beam is provided in dedicated shifts at 1.3 GeV for tera-hertz (tHz) applications. In these dedicated shifts the magnet optics are set in such a way that the electron packages (so-called bunches) are compressed to short sub-mm sized lengths. the storage ring has also become an inte-gral part of the accelerator education and training program at KIt, offering a small fraction of the machine development time for hands-on tutorials for students. the following sections give an overview of the machine operation in 2013 and a status update of the ANKA five-year large-scale refurbishment and upgrade plan.

Machine operationIn 2013 the storage ring was in operation for a total of 4181 hours. of this time 57% was provided to user operation at 2.5 GeV and 9% for special user operation at 1.3 GeV with short bunches. A further 4% of the time has been spent with injection and 12% for start-up after shutdowns or weekends. the accelerator development and consolidation program utilized 18% of the running time. the distribution of beam time is illustrated in Fig. 1. of the 110 days scheduled for regular user operation 13 days were lost; 6 of these days were due to power cuts to the KIt site. Several more days were lost due to consequently damaged power supplies. the total availability, taking into account delivered to scheduled beam time, was 96%.

Refurbishment and upgradesIn order to avoid days lost from rare types of events such as major power cuts, several procedures have been put in place to aid the quick recovery of the machine operation. Most notable of these is the implementation of detailed alarm software, which allows a quick identification of devices that have been disturbed, even if still operational. Furthermore, as part of the large-scale ANKA machine upgrade plan, analogue power supplies are being replaced by switched-mode power supplies. these power supplies are more robust against line voltage fluctuation, reduce the overall power consumption while being more efficient, and have advanced self-health analysis on-device soft-ware. the following gives a brief status report and examples of the machine upgrades completed during the time scale of this report.

Selected examples

Control system softwareWith the implementation of a machine tCp/Ip private network in 2012 the replacement of ageing hardware devices, which also dictated the type of con-trol software that can communicate to such devices, has now got thoroughly on the way. Several devices have been replaced such as power supplies, ion pump controllers, etc. these devices have been fully integrated into the new epICS control system software used at ANKA. the combined effect of com-munication over ethernet, new hardware and new control software is leading to an overall considerable improvement in the reliability of the machine.


Accelerator Report


the new digital feedback system for the ANKA storage ring operationA new, digital, and fast bunch-by-bunch (BBB) feedback system has been installed and commissioned at ANKA in october 2013. this system led to an improved accumulated current per injection, a higher overall lifetime of the electron beam, provided a diagnostic tool set for machine development, and new applications for special user operation. Further applications are under study.

IntroductionFilling the ANKA storage ring with electrons encompasses several differ-ent operational stages such as injection, accumulation period, and energy ramp. At ANKA the injection is performed at 0.5 GeV, which is followed by an accumulation period of approximately 30 min. An energy ramp brings the electrons to an kinetic energy of 2.5 GeV, to the final working point during ANKA’s normal user operation. throughout these stages it is high-ly desirable that the electron beam is kept stable at all times. Key beam parameters such as the central RF frequency, the beam phase, the cavity voltage, and the orbit are changing throughout this procedure. the new feedback system was configured to keep the beam stable throughout the whole process by damping the beam’s transverse oscillations during all of these changes, which can finally lead to higher stored beam currents. the electron packages (so-called bunches) making up the beam in the ring can be individually controlled by the new feedback system.

Impact on user operationone of the first achievements was to increase the amounts of filled electron bunches by 33%, which leads to a decreased individual bunch current for the same integrated beam current. With this change the lifetime of the beam increased considerably by 25%. In addition, the average accumulated beam current could be increased from 165 mA to 195 mA. During machine studies even higher beam currents beyond 215 mA were achieved. these improvements suggest possible options to change the duty cycle at ANKA. one option is the accumulation of a current with more than 200 mA, which could lead to a single injection procedure per 24 hours. this would increase the usable beam time and will lead to fewer interruptions of measurements at the beamlines.

Improvements to machine diagnosticsBesides improvements for the normal ANKA user operation, the feedback system also provides sophisticated diagnostic long-term capabilities. It al-lows monitoring important beam parameters constantly such as the trans-verse oscillation frequencies. With this data an in-depth analysis of beam dynamics is now possible. understanding the contributing parameters via this data could lead to a further increased stability and reliability of the ANKA storage ring. In addition, several standard measurements are now automated.A core feature for special user operation is the possibility to excite and ma-nipulate single bunches. one application of the new feedback system is the removal of all bunches but one during the injection process. the feedback system achieves at least the same bunch purity, if compared to the previ-ous method for single bunch injection. Several advantages follow from this new approach, for example, it is feasible to inject multiple isolated bunches within one injection cycle. In addition, the standard ANKA user operation injection setup can also be used for single bunch injections. this reduces drastically the time needed for creating single bunches starting from stan-dard user operation settings in contrast to rarely used single bunch injec-tion settings. Furthermore, a custom filling pattern can be specified with individual bunch currents and the overall bunch currents can be reduced in-between measurements. therefore, it is not necessary to wait for natural losses to occur to measure machine parameters or radiation generation at different beam currents. this dramatically, by orders of magnitude, reduces the amount of time needed for such measurements while it is possible to sample a variety of bunch currents, simultaneously, in one fill.

Figure 1: Lifetime increase due to the new feedback system by 25%. Shown is the lifetime for 130 mA for the months before and after the implementation of the feed-back system

Figure 2: Part of the new feedback system implemented and commissioned in October 2013

Collaborations/ContributorsCenter for Synchrotron Radiation (DeltA), Dortmund, GermanyDimtel, Inc, San Jose, uSAFundingSupported in part by BMBF Verbundforschung under contract number 05K10VKC and 05K13VKA. Contributors/Authorse. Hertle, N. Hiller, e. Huttel, B. Kehrer, A.-S. Müller, N. J. Smale, M. Höner, D. teytelmanSelected Publicatione. Hertle, N. Hiller, e. Huttel, B. Kehrer, A.-.Müller, N. J. Smale (KIt, Karl-sruhe), M. Höner (DeltA, Dortmund), D. teytelman (Dimtel, San Jose), First results of the new bunch-by-bunch feedback system at ANKA, IpAC 2014 Dresden, Germany, tupRI074,1739-1741 (2014)

KAPTUREHigh speed, high throughput broadband data acquisition using fast terahertz detectors and a dedicated electronics

In so-called low-alpha mode ANKA is operated to compress the electron packages (so-called bunches) to very small bunch lengths for which mi-cro-bunching instabilities can occur. Micro-bunching leads to spontaneous changes in the emitted coherent synchrotron radiation (CSR) intensity. these changes can be observed as very high bursts in emitted terahertz (tHz) sig-nals for single-bunch mode as well as in multi-bunch mode in the ANKA storage ring. For the investigation of multi-bunch effects on the longitudi-nal dynamics of the electrons in the storage ring two fundamental diag-nostic instruments are mandatory: tHz detectors to resolve single bunches and dedicated acquisition hardware to monitor all signals turn-by-turn. the KAptuRe (KArlsruhe pulse taking and ultrafast Readout electronics) system, a joint development between several institutes at KIt, in combination with ultra-fast cryogenic and room temperature detectors can fulfill this task.

KAPTUREthe KAptuRe system developed at KIt opens up a new possibility to mon-itor all bunches in a synchrotron storage ring over an unlimited number of turns. the system prototype was successfully commissioned and tested in a real measurement environment in 2013. KAptuRe is used at ANKA to fol-low the turn-by-turn bursting behavior of the generated tHz radiation. this novel diagnostic tool is used at ANKA for the investigation of longitudinal density fluctuations of electron bunches, to explore the fundamental phys-ical mechanisms of their generation and thus on the long term to improve the stability of the emitted CSR. the main components are depicted in Fig. 1. the picosecond pulse from a fast tHz detector is amplified by a low noise amplifier (lNA) and then split into four equal signals by a sideband power divider with an analog bandwidth of up to 100 GHz. the pulse is then sampled by four analog-to-digital converters (ADCs) on the KAptuRe board. each sampling point can be adjusted in 3 ps steps with sub-ps ac-curacy. using four sampling points it is possible to derive the initial pulse width, the peaking time, and the peak height. the revolution time at ANKA is 368 ns with electron bunches spaced in 2 ns intervals. this naturally leads to samples of 184 buckets, which are read out, ordered and evaluated at every revolution by the high through-put read-out board. the data is sent to a computer via the high-speed serial computer expansion bus standard (pCIe, peripheral component interconnect express).KAptuRe can be operated in various modes. Instead of splitting one detec-tor signal and using the four sampling channels to derive the pulse proper-ties, it is also possible to use up to four detectors simultaneously, while each detector is connected directly to one sampling channel. the latter allows to evaluate the performance and characteristics of different detectors while

detecting the same tHz signal, or to gain information of the detected tHz radiation by using, for example, detectors, which are sensitive in different spectral regions. Figure 2 shows the signal of two comparable Schottky diodes each connected to a single sampling channel. Figure 3 shows the bursting behavior in low-alpha mode at the ANKA storage ring. Analysis of the data can give new insights into the physics of inter- and intra-bunch interactions.

Figure 1: View inside the KAPTURE system

Figure 2: Simultaneous measurement of bursting instabilities with two Schottky de-tectors


Accelerator Report


Figure 3: Turn-by-turn and bunch-by-bunch signal of a fast Schottky diode detector recorded by the KAPTURE system (left). Four trains consisting of approx. 33 bunches can be recognised. The behavior is shown for approx-imately 140 thousands consecutive turns. The intensity is color coded. The corresponding bucket current is shown in blue and the mean THz signal in red (right).

Collaborations/ContributorslAS - laboratory for Application of Synchrotron radiationIpS - Institute for photon science and Synchrotron radiationIpe - Institute for Data processing and electronicsIMS - Institute of Micro- und Nanoelectronic Systems Funding Supported in part by Initiative and Networking Fund of the Helmholtz Asso-ciation under contract number VH-NG-320 and in part by BMBF Verbund-forschung under contract numbers 05K10VKC/05K13VKA/05K2010. Contributors/Authors M. Brosi, J. Steinmann, V. Judin, M. Caselle, M. Balzer, S. Cilingaryan, N. Hiller, M. Hofherr, B. Kehrer, A. Kopmann, K. ll’in, S. Marsching, A. Men-shikov, M. J. Nasse, J. Raasch, A. Scheuring, M. Schuh, M. Schwarz, N. J. Smale, p. thoma, S. Wünsch, M. Siegel, M. Weber, A.-S. Müller Selected Publication(s)A.-S. Müller, M. Balzer, M. Caselle, N. Hiller, M. Hofherr, K. S. ll’in, V. Ju-din, B. Kehrer, S. Marsching, S. Naknaimueang, M. J. Nasse, J. Raasch, A. Scheuring, M. Schuh, M. Schwarz, M. Siegel, N. J. Smale, p. thoma, M. Weber, S. Wünsch, Studies of bunch-bunch interactions in the ANKA stor-age ring with coherent synchrotron radiation using an ultra-fast terahertz detection system, IpAC 2013V. Judin, A.-S. Müller, M. Schwarz, Bursting patterns of coherent synchro-tron radiation in the ANKA storage ring, IpAC 2013M. Caselle, M. Balzer, S. Cilingaryan, M. Hofherr, V. Judin, A. Kopmann, K. ll’in, A. Menshikov, A.-S. Müller, N. J. Smale, p. thoma, S. Wünsch, M. Sie-gel, M. Weber, ultra-fast data acquisition system for coherent synchrotron radiation based on superconducting terahertz detectors, IpAC 2013p. thoma, V. Judin, At the limits: how to detect relativistic electrons?, optik & photonik 1/2013, pp. 58-61 (2013)

EOSSingle-shot electro-optical measurements of the longitudinal bunch profiles at ANKA and for Flute

Part 1: Electro-optical near-field setup reveals longitudinal bunch sub-structures during low-alpha operation at ANKAANKA is the first storage ring in the world with a near-field single-shot elec-tro-optical (eo) bunch profile monitor, allowing the acquisition of single-shot longitudinal bunch profiles with sub-picosecond resolution (down to 390 fs granularity). Bunch lengths of down to 1.5 ps (rms) can be measured. the setup is capable of measuring bunch charges as low as 30 pC. Measurements for different bunch compression settings have revealed the expected dynamic sub-structures on the bunch profiles and strong bunch deformations for high bunch charges.

Introduction and motivationDuring ANKA’s low-alpha operation, the bunch length is drastically reduced to sub-mm dimensions and temporally down to a few picoseconds (rms) along the electron orbit, which enables the generation of coherent synchrotron radi-ation (CSR) in the terahertz (tHz) frequency range. In a storage ring, for certain machine conditions such as high currents and settings to strongly compress electron bunches, a bursting behavior of the emitted CSR can be observed. these bursts of radiation can be caused by dynamic changes of the tempo-ral shape of the electron bunches. the longitudinal profile, which reveals the electron distribution at a certain position along the orbit, is a key parameter that also determines the spectral characteristics of the emitted CSR. these dy-namic changes of the longitudinal bunch profile, the so-called micro-bunch-ing, have been predicted by theory. A non-trivial task in performing single-shot and, especially, non-invasive electron beam measurements is to maintain sub-ps accuracy during these measurements. this sub-ps accuracy is essential and mandatory. this was achieved and, consequently, micro-bunching at a storage ring was observed.

Methodthe eo measurement principle employed is based on the technique of spectral decoding (eoSD) seen in Fig.1. Ideally a laser pulse is linearly chirped, which means that spectral frequencies or the respective wavelengths correlate linearly to a temporal position in the laser pulse. Wavelengths or spectral colors are uniquely coded to specific points in time along the laser pulse. In the exper-iment a chirped laser pulse passes through an eo active crystal. the strong electric near-field of the electron bunch, which travels near the eo crystal in parallel to the light pulse, changes the birefringence of the crystal material. the modulation of the crystal’s birefringence leads to an imprint of the longitudinal electron bunch near-field profile on the chirped laser pulse. the temporal mod-ulation, corresponding also to spectral modulation of the laser pulse, modifies the chirp and can be decoded and analyzed in a single-shot spectrometer.

Figure 1 : Working principle of electro-optical spectral decoding (EOSD)

Results

A compact eo monitor was installed in late 2012 inside the ANKA storage ring (see ANKA Annual Report 2012). Measurements in early 2013 have, for the first time at a storage ring, revealed the predicted sub-structures on the longitudinal electron bunch profiles during the micro-bunching instabil-ity in low-alpha operation. Following these first results, detailed systematic studies of single-shot measurements have been performed, which were compared to streak camera measurements obtained in parallel. examples of results are presented in Fig. 2: (a) shows averaged bunch profiles measured with a streak camera, which cannot resolve the anticipated bunch sub-struc-tures due to the required long averaging time, (b-d) show single-shot bunch profiles recorded with the eoSD setup. the profiles in (b) have been record-ed for the same machine conditions as in (a) for a fully compressed beam at a bunch charge of 420 pC. In contrast, the profiles in (c) were recorded for considerably longer bunches, but with the same bunch charge, and - as ex-pected - the sub-structures diminish. Again changing the compression, the profiles in (d) show heavily compressed bunches at a relatively high bunch charge of 650 pC. Here a strong bunch deformation and some sub-struc-tures are visible. the method can be further improved by increasing the resolution and acquisition rate. Damping of the wake-fields will enable the operation of the setup beyond the current single-bunch operation.

Figure 2: Comparison for different machine parameters: (a) averaged bunch profiles measured with streak camera and (b-d) measured with electro-optical spectral decod-ing (EOSD) showing single-shot bunch profiles

Part 2: Electro-optical bunch length monitors for FLUTE: layout and simulationsthe bunches in the new accelerator Flute, currently under construction at KIt next to the ANKA hall, will be significantly shorter than at ANKA with typical bunch lengths in the range of only 5 to 300 fs. therefore, simula-tions of the expected eo signals influenced by various parameters were per-formed at different positions along Flute to determine the requirements and the layout of the eo monitors. the current eo sampling technique, and the electro-optical crystals employed, reaches a resolution limit at 40 fs for very short bunches. In addition, at low electron energies the signal broadens due to the opening angle of the Coulomb field. Improving the resolution could be possible by using alternative materials and redesigning the eo setup using the emitted coherent transition radiation (CtR).

Introduction and motivationKarlsruhe Institute of technology is currently constructing the linac-based light source Flute (Ferninfrarot linac-und test-experiment). It is a dedicated accelerator R&D facility with the main goals being to cover a large charge range and achieving very short electron pulses to generate tHz radiation with high peak fields. the final electron energy would be up to 42 MeV. Flute will be able to operate with a wide range of electron bunch charges and lengths. For further details see the contribution about Flute in this ANKA Annual Report. the wide range of bunch lengths and bunch charges provided by Flute requires a sophisticated single-shot system for online bunch-length diagnostics. An eoSD system for bunch length diagnostics has a variety of parameters, which play a key role in the performance of the system and need to be adapted to the beam parameters. Several numerical simulations were performed to determine these optimum parameters.

Figure 3: Control and data acquisition station of the electro-optical spectral decoding system, enabling systematic studies of single-shot bunch length profiles

ResultsFlute is planned to operate in different charge regimes: a low charge mode at 1 pC, a medium charge mode at 100 pC, and a high charge mode with up to 3 nC. For each of the modes, a maximum bunch compression is de-sired. Beam dynamics simulations with the particle tracking code AStRA (a space charge tracking algorithm) allow the prediction of the transverse and longitudinal beam parameters along Flute. the electrical field strength of a corresponding bunch charge was calculated by using AStRA simulation data. this was followed by simulating the interaction of a laser field with the electric field inside the eo crystal due to the electron bunch passing by. this leads to a modulated laser pulse with temporal information from the electron bunch. A list of parameters of the detection system was varied to find the optimal settings for bunch length measurements for every desired charge regime, for example as a function of crystal thickness, crystal posi-tion in respect to the electron beam, or laser pulse length. the optimum parameters of the detection system for a corresponding bunch charge and position along the machine are shown in table 1, which also includes esti-mated signals (rms bunch length) from such a detection system. For further details see the selected publications.


Accelerator Report


Table 1

Calculation for positions after the gun at 7 MeV gun at 7 MeV chicane at 42 MeV

chicane at 42 MeV 1 100 3000 1 100 3000 1 100 3000

Input sz / fs 520 1200 2500 450 1080 2300 1 67 200

Reconstructed sz / fs 690 1500 3700 448 1060 2270 70 95 235

Deviation / % +20 +20 +50 -0.5 -2 -0.3 unresolved +45 +15

optimum crystal thickness / mm 5 5 5 5 5 5 5 1 0.1

optimum laser pulse length (FWHM) / ps 6.14 6.14 6.14 6.14 6.14 12.28 0.768 0.768 0.768

r0 / mm 2.8 5.6 12.5 0.8 1.2 4.8 0.6 1.6 2.4

Collaborations/Contributorspaul Scherrer Institute (pSI), SwitzerlandDeutsche elektronen-Synchrotron DeSY, Germany

FundingSupported in part by BMBF Verbundforschung under contract number 05K10VKC and 05K13VKA, in part by lA³Net, a Marie Curie Initial training Network (ItN) scheme, and the Initiative and Networking Fund of the Helm-holtz Association under contract number VH-NG-320. Contributors/Authors N. Hiller, A. Borysenko, e. Hertle, e. Huttel, B. Kehrer, V. Judin, S. Marsching, A.-S. Müller, M.J. Nasse, A. plech, R. Rossmanith, R. Ruprecht, p. Schön-feldt, M. Schuh, M. Schwarz, N.J. Smale, J.l. Steinmann, p. Wesolowski, p. peier, V. Schlott, B. Steffen

Selected PublicationsB. Kehrer, A. Borysenko, e. Hertle, N. Hiller, V. Judin, S. Marsching, A.-S. Müller, M.J. Nasse, M. Schuh, Numerical Wakefield Calculations for elec-tro-optical Measurements, MopMe015, IpAC2013N. Hiller, A. Borysenko, e. Hertle, e. Huttel, V. Judin, B. Kehrer, S. Marsching, A.-S. Müller, M.J. Nasse, A. plech, M. Schuh, N.J. Smale (KIt) p. peier, V. Schlott (pSI), B. Steffen (DeSY), electro-optical Bunch length Measurements at the ANKA Storage Ring, MopMe014, IpAC2013N. Hiller, A. Borysenko, e. Hertle, V. Judin, B. Kehrer, S. Marsching, A.-S. Müller, M.J. Nasse, M. Schuh, p. Schönfeldt, N.J. Smale, J.l. Steinmann (KIt) p. peier, B. Steffen (DeSY), V. Schlott [pSI), Status of Single-shot eoSD Mea-surement at ANKA, WeBoBB02, IpAC 2014A. Borysenko, e. Hertle, N. Hiller, V. Judin, B. Kehrer, S. Marsching, A.-S. Müller, M.J. Nasse, R. Rossmanith, R. Ruprecht, M. Schuh, M. Schwarz, p. Wesolowski (KIt), B. Steffen (DeSY), electro-optical Bunch length Monitor for Flute: layout and Simulations, tHpMe123, IpAC2014

ComptonDesign of a compact setup to measure the beam energy by detection of Compton backscattered photons at ANKA

one of the most important parameters of accelerators is their beam energy. So far the method of resonant depolarization has been used to accurately determine the kinetic energy of 2.5 GeV at the ANKA electron storage ring. However this method is cumbersome for lower energies and a good alterna-tive is the detection of Compton backscattered photons which are generated by laser light when photons are scattered off the relativistic electron beam. A compact setup is proposed. the feasibility at the ANKA storage ring has been studied.

IntroductionCompton backscattering (CBS), sometimes also referred to as laser-Compton scattering or inverse Compton scattering, describes the process of scattering of (laser) photons by relativistic electrons. this method does not require a polar-ized electron beam, in contrast to commonly used beam energy measurements such as the method of resonant depolarization. therefore, it can be more ver-satile for continuously monitoring the beam energy. especially at lower energies than 2.5 GeV, the accumulation time for a polarized electron beam is long and impractical for resonant depolarization measurements. the CBS project aims at developing and realizing, for the first time, a transverse configuration instead of a traditionally used head-on collision between laser photons and electrons. this improvement could realize a compact and relatively low-cost setup. It also provides a supplementary beam diagnostic instrument at ANKA, for example, to obtain the precise energy. Subsequently, the precise momentum compaction factor at low-alpha operation could be derived. the transversely configured setup has several advantages: it is very compact and can therefore also be used at rings with restricted space, and the transverse configuration reduces the cut-off energy of the spectrum of backscattered photons by a factor of two. this enlarges the capability of energy measurements compared to traditional head-on collisions and makes measurements, especially detector calibration, considerably easier, because available calibration sources have limited upper energies. the transverse configuration can in principle also be converted into a versatile laser wire diagnostics tool.

Transversely configured CBS setup at ANKAFigure 1 shows an illustration of the transverse CBS setup for energy measure-ments currently under construction at ANKA. the interaction point is located in one long straight section. the gamma photons generated by CBS propagate in a narrow cone along the direction of the electron beam. the photons with an energy near the spectrum cut-off energy are concentrated on the propa-gation axis. A collimator is used in front of the high purity Germanium (HpGe) spectrometer to collect these photons and reduce the background level. It is planned to use a laser, which emits in the mid-infrared range. For this purpose a continuous wave monochromatic Co2 laser with a photon energy of 0.117 eV will be used to ensure that the spectrum cut-off energy is within the detectable range of the commercially available HpGe spectrometers (up to ~10 MeV). the laser can be tightly focused to match the vertical size of the electron beam and therefore maximize the signal rate.

Figure 1: Compact energy measurement setup for detection of Compton backscat-tered photons at ANKA

Signal-to-noise ratio

one challenge of the transverse CBS method is the much lower interaction time between laser photons and electrons, in contrast to the head-on collision scheme where electrons and photon anti-propagate over a longer time span. therefore, a feasibility study has been carried out comparing a simulation of CBS photons with an actual background measurement for the low-alpha mode at 1.3 GeV. the background was measured at the long straight section of the IMAGe beamline (Fig. 2). the HpGe detector (model Canberra GX3018) had an energy resolution of 1.80 keV (FWHM) at 1.33 MeV and an active volume of 139 cm3 (diameter 58 mm, length 52.5 mm). the full energy peak efficiency for 1.5 MeV photons is estimated to be at least several percent. using At (Accelerator toolbox for MAtlAB®) simulations showed a vertical size of the electron beam in low-alpha mode of 96 µm rms. the spectrum of CBS photons reaching the detector during 20 minutes of acquisition time was simulated by using CAIN 2.35 (stand-alone FoRtRAN Monte-Carlo code for the interaction involving high energy electrons, positrons, and photons). It was assumed that it is possible to focus 10 W of laser power to a region of 100 µm rms, which ideally overlaps with the 96 µm rms electron beam at the interaction point, while also considering a typical 40 mA electron beam current. Assuming a 5% full energy peak efficiency (Fepe) a photon density of 4200 counts/keV is found at the edge, and 2800 counts/keV for 16 mm2 and 4 mm2-sized collimators, respectively. Both are sufficient counts to reduce the statistic relative uncertainty of determining the spectrum cut-off energy to a few parts in10-5.Both the CBS photon and the background radiation level (mainly from gas Bremsstrahlung) are proportional to the electron beam current and the detec-tion time. therefore, a signal-to-noise ratio of around 2.5 can be estimated.

Slit size/collimator area / mm2 16 4

Background (measured) / (photons/mA/s) 0.779 0.478

Signal / (photons/mA/s)(simulated at 5% Fepe)

1.98 1.32

Table 1: Average Photon Count Rate

Figure 2: Background measurement at the IMAGE beamline

Collaborations/ContributorsR. Klein, MlS, BerlinC. Wilhelm, S. Kaminski, KSM (KIt)

FundingSupported in part by lA³Net, a Marie Curie Initial training Network (ItN) scheme.

Contributors/Authors C. Chang, D. Batchelor, e. Hertle, e. Huttel, V. Judin, A.-S. Müller, M. J. Nasse, M. Schuh, J. l. Steinmann, S. Bauer, N.J. Smale, M. Süpfle, M. Ha-gelstein, A. Volker, t. Fischböck

Selected Publication(s)C. Chang, D. Batchelor, e. Hertle, e. Huttel, V. Judin, A.-S. Müller, M. J. Nasse, M. Schuh, J. l. Steinmann, Design of a compact setup to measure beam energy by detection of Compton backscattered photons at ANKA, proceedings of IpAC2014, Dresden, Germany, tHpMe112, 3494 (2014).


Collaborations/ContributorsBudker Institute for Nuclear physics, Novosibirsk, Russia

Contributors/Authors A. papash, A-S. Mueller, e. B. levichev, p. A. piminov, S. V. Sinyatkin, K. Zolotarev Selected Publication(s)A. I. papash, A.-S. Müller (KIt), e. B. levichev, p. A. piminov, S. V. Sinyatkin, K. Zolotarev (BINp SB RAS), An ultra-low emittance Model for the ANKA Synchrotron Radiation Source Including Non-linear effects, IpAC2014, Mo-pRo064, 228-230 (2014).

FLUTEa new versatile linac-based test facility for intense terahertz and far-infrared pulses

A new compact versatile linear accelerator named Flute (Ferninfrarot linac- und test-experiment / far infrared linac- and test-experiment) was designed at KIt in collaboration with DeSY and pSI. It will be used to generate strong (several 100 MV/m), ultra-short (< 300 fs) terahertz pulses (up to 25 tHz) for numerous photon science experiments and a variety of accelerator stud-ies. Future research includes pump-probe experiments as well as systematic biomedical studies. the planned projects in accelerator research range from comparing different coherent tHz radiation generation schemes to com-pressing electron bunches and studying beam stability. the construction of the machine started in 2013

IntroductionIn recent years there has been a growing worldwide demand for light puls-es on ultra-short time-scales for the analysis of samples in the materials and life sciences, in chemical kinetics and dynamics, biology, and medicine. Accelerator-based sources can use magnet optics to generate the desired ultra-short light pulses through compression of electron packages (so-called bunches) to a micrometer scale, which leads to coherent light pulses of a few femtoseconds. the development of such a new breed of sources with ultra-short time scales requires fundamental research in technology, mate-rial science, ultra-fast diagnostics and electronics, and theory for a better understanding of the underlying physics.the possibility to generate strong, intense electromagnetic pulses will en-able the exploration of non-linear effects in materials and matter, to perform non-linear spectroscopy in the terahertz frequency domain and in the far-in-frared spectral range, augmenting the variety of terahertz applications per-formed in the linear regime over the last decade. the availability of ultra-short pulses will further stimulate the development of novel technology, such as ultra-fast detectors, new detection schemes and measurement methods be-yond the recent tremendous progress seen in this frequency range.

Motivation for FLUTEFlute is designed to serve as a compact test bench for diagnostics and instru-mentation of very short electron bunches. It will also be used to study space charge and radiation-mediated effects on the electron density, which can re-sult in instabilities. the knowledge gained in such experiments, to diagnose and ultimately control ultra-short electron bunches as well as to examine the field of parameters, will lead to a stable operation with ultra-short bunches. Flute will generate short and strong coherent tHz pulses, which will be uti-lized in pump-probe experiments and various scientific applications.

Principle design of FLUTE and function of its componentsFlute as a linac-based accelerator will consist of three major parts. the first part is the radio frequency (RF)-photo-injector, which was provided by CeRN. It consists of a cathode made from pure copper. Alternatively, it is coated with materials like cesium telluride (Cs2te). the cathode is illuminated by a strong

ultraviolet (uV) laser pulse to release an electron cloud. then, the cloud is accelerated in an RF cavity structure to a kinetic energy of 7 MeV. After an electron beam diagnostic section, the electrons are further accelerated along a 5 m linear accelerator (provided by pSI) to about 41 MeV. In order to com-press the electron cloud to a short bunch, the electrons pass through a special magnetic optics unit consisting of four dipole magnets, the magnetic bunch compressor. the electron bunch exits the bunch compressor with a longitudi-nal root mean square (rms) length well below 90 µm, which corresponds to 300 fs. this requirement is of paramount importance, because this spatially and temporally short electron bunch can now act as a source of coherent tHz radiation covering a wavelength range from 3 mm to 30 µm.

the two main parameters controlling the power of the tHz pulse are the bunch length and the bunch charge. Ideally, maximizing the number of charges and, simultaneously, compressing them in the smallest possible vol-ume, will generate the strongest tHz pulses. However, non-linear effects impose limits on compressing many charges in a small volume. one aim of Flute is to explore and expand these limits by experimentally covering a wide range of bunch charges and bunch lengths ranging from 1 fs at 1 pC to 270 fs at 3 nC. At the design phase these effects were already investigated using numerical simulation (see selected publication 3).

Besides fundamental studies of short pulse generation, the Flute team will also progress to provide stable and reproducible tHz pulses needed for ad-vanced user experiments, which exploit the strong (several 100 MV/m), ul-tra-short (< 300 fs), and broad band (up to 25 tHz) coherent tHz radiation emitted by the electron bunches.Further details and references can be found in the selected publications 1 and 2.

Building and hardware: major milestones reached in 2013

• Refurbishment of the experimental hall for Flute and the heavy radiation protection door were finished. the refurbishment of basement, control room, and measurement room was started.

• Conceptual Design Report (CDR) was finalized and presented to the MAC (Machine Advisory Committee) and SAC (Scientific Advisory Committee), which supported the Flute work plan.

• experimental results of the first successful test of the electron gun at the synchrotron elSA (Bonn) were evaluated.

Simulation and numerical studiesthe aim of Flute is also to investigate theoretically and by simulations how non-linear electron beam dynamics can help to isolate effects, which limit the bunch length and, therefore, the emitted tHz light pulse length. the two main factors contributing are space charge and self-interaction. the latter is the interaction of the electron bunch with its own radiation field, mainly in the last part of the bunch compressor. Space charge effects are smaller at lower electron energy, but dominate the beam dynamics inside the electron gun. Self-interaction limits the performance for high bunch charges above 1 nC and are computationally demanding. However, it was shown that faster algorithms do not yield the same results for the param-eters of Flute (see selected publication 3). For low bunch charges such as 1 pC a different compression scheme was investigated by simulation (see selected publication 5).

Accelerator Report


Low EmittanceFeasibility study: a low emittance ring model based on the ANKA geometry

A new beam optic based on the existing ANKA ring geometry but with twice the number of bending magnets has been investigated in the frame-work of the feasibility studies for compact low emittance synchrotron light sources. the concept would allow us to reduce the natural emittance of the original ANKA double bend achromat lattice from 45 nm∙rad down to 6 nm∙rad while preserving sufficient dynamic range for stable beam cir-culation. Also the high efficiency top-up injection of a 2.5 GeV e-beam and 250-300 mA steady beam current stored in a ring would benefit user experiments.

Introductionthe low emittance (le) ring under study is inscribed into the present ANKA synchrotron geometry in order to preserve existing beam lines. the main objectives of such an upgrade are to

• reduce the emittance of the electron beam down to ~6 nm∙rad,• ensure that the ring dynamic aperture is sufficient for the high efficiency

beam injection (Ax ≈ ±10 mm),• provide a large momentum acceptance (MA ≥ ±2%) to improve the

beam life time,• allow low loss top up injection at 2.5 GeV,• provide a steady e-beam current at the level of 250 to 300 mA.

either a full energy booster synchrotron or a linear accelerator could serve as injectors for such a lattice.

either a full energy booster synchrotron or a linear accelerator could serve as injectors for such a lattice.

Calculation of a minimum emittance cell with “split bend”Comprehensive studies and computer simulations have been done in order to find and optimize a new lattice structure. theoretical minimum emit-tance (tMe) cells with “split bend” (twice the number of bending magnets) and a quadrupole lens in-between (Fig. 1) were used to reduce the natural horizontal emittance as well as to compensate natural chromatic aberra-tions by pairs of non-interleaved sextupole lenses separated by a phase advance close to π. the quadrupole in-between split bends allows com-pensation of the influence of chromatic sextupole pairs located on both sides of the low emittance (le) cell. Also the horizontal betatron function βx and dispersion D are large at the end points of the split cell in order to reduce the required sextupole strength. At the same time both, βx and D, are minimized in the middle of each bend in order to reduce the emittance. Different lattice geometries with gradually reduced emittance and dynamic aperture were investigated.

the horizontal aperture is more important for injection and the cell was adjusted for minimum natural emittance. A tMe of about 8.6 nm∙rad, large dynamic aperture Ax = ±18 mm and momentum acceptance MA = ±6% are available. Slight detuning from the μx = π condition and cell adjusting for minimum emittance leads to a reduction of the tMe to 6.2 nm∙rad, but in expense of a smaller dynamic aperture Ax = ±9 mm and momentum acceptance MA = ±4%.the lowest stable lattice provides a tMe = 2.5 nm∙rad, but small dynamic aperture DA = ±1 mm and MA = ±0.5%. By introducing additional families of sextupoles inside the quadrupoles where βx–functions and dispersion D are still large the dynamic aperture was opened from ±1 mm to ±5 mm, but it is still far below required conditions of stable ring operation.

Figure 1: Low emittance latttice based on the modified TME cell with split bend. Quadrupole between splitted bends allows to adjust phase advance between chromatic sextupoles.

Example of LE ANKA latticeFor further detailed investigations the “split optics” described above was cho-sen with a moderate emittance and the largest DA. the negative gradient Gb = -9.5 t/m was introduced in the dipole magnets to further reduce the natural emittance. Due to the strong focusing in an ultra-compact lattice composed of split bends, the maximum quadrupole gradient reaches 70 t/m to 90 t/m and the maximum sextupole gradient grows to 1500 to 3300 t/m2. Nevertheless, the required field in quadrupoles and sextupoles is reasonable, because of the aperture of focusing elements is reduced from present 70 mm down to 25 mm. Achromat conditions are provided in all four short and four long straight sec-tions to ensure the operation of insertion devices (ID). the geometrical location of the elements of the original and split lattices are compared in Fig. 2.

the source points of synchrotron radiation (SR) and radiation directions from straight sections are the same as in the present ANKA ring. there is no need to modify the location or direction of beam lines associated with insertion devic-es (ID) and experimental hutches. We achieve compensation of second order aberrations and increase the momentum acceptance by a factor of two with respect to the present ANKA lattice. For further details see the selected publi-cation below.

Figure 2: Location of main elements in the original and split magnet LE ANKA cell


Caption 1:FLUTE bunker during (left) and after refurbishment (right). Main accelerator module on a temporary girder (front) and modulator (blue racks).

Caption 2:Longitudinal phase space of a 3 nC bunch at the entrance and the exit of the bunch compressor, which consists of 4 dipole magnets (yellow boxes). At the beginning, the longitudinal phase space shows a linear relationship between electron position and electron momentum. The rms bunch length is above 1 ps. After the bunch compressor the rms bunch length is reduced to about 270 fs, but a clear correlation in phase space is lost due to non-linear interactions. Moreover, different algorithms (1D and 3D) of the simulation program CSRtrack yield different results (see selected publication 3 and 4).

Collaborations/Contributorspaul Scherrer Institute (pSI), SwitzerlandDeutsche elektronen-Synchrotron DeSY, GermanyHelmholtz-Zentrum Dresden-Rossendorf (HZDR), Germany Contributors/Authors M. Schuh, M. Schwarz, M. J. Nasse, R. Ruprecht, S. Naknaimueang, A. plech, S. Marsching, Y.-l. Mathis, R. Rossmanith, M. Schreck, M. Weber, p. Wesolowski, e. Huttel, M. Schmelling, A.-S. Müller Selected Publications1 - M.J. Nasse, M. Schuh, S. Naknaimueang, M. Schwarz, A. plech, Y.-l. Mathis, R. Rossmanith, p. Wesolowski, e. Huttel, M. Schmelling, A.-S. Müller, Flute: A versatile linac-based tHz source, Rev. Sci. Instrum. 84, 022705 (2013).2 - M. J. Nasse, e. Huttel, S. Marsching, A.-S. Müller, S. Naknaimueang, R. Rossmanith, R. Ruprecht, M. Schuh, M. Schwarz, M. Schreck, p. Wesolowski (KIt) R. Assmann, M. Felber, K. Flöttmann, M. Hoffmann, H. Schlarb (DeSY), H. Braun, R. Ganter, l. Stingelin (pSI), Flute: A versatile linac-based tHz source generating ultra-short pulses, WepWA010, proc. IpAC 2013, Shang-hai (China).3 - S. Naknaimueang, e. Huttel, S. Marsching, A.-S. Müller, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schuh, M. Schwarz, M. Weber, p. Wesolowski, Simulating the bunch structure in the tHz source Flute, WepWA008, proc. IpAC 2013, Shanghai (China).4 - S. Naknaimueang, V. Judin, S. Marsching, A.-S. Müller, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schuh, M. Schwarz, M. Weber, p. Wesolowski (KIt), W. Hillert, M. Schedler (universität Bonn), Design Studies for Flute, A linac-based Source of terahertz Radiation, WepSo44 , pro-ceedings of Fel2013, New York, NY, uSA5 - M. Schuh, e. Huttel, S. Marsching, A.-S. Müller, S. Naknaimueang, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schwarz, M. Weber, p. Wesolowski (KIt), R. W. Assmann, K. Flöttmann, H. Schlarb (DeSY), RF com-pression studies for Flute, WepWA009, proc. IpAC 2013, Shanghai (China).

Accelerator Report



2. Main achievements of 30 cm long 20 mm period length undulator mockup coilsIn collaboration with the company BNG, undulator mockup coils with 20 mm period length and 30 cm long (see Fig. 3) have been designed, manu-factured and tested.All changes applied to the short mockups have been applied here. In ad-dition, the staggering has been eliminated by winding each next groove one after the other. Moreover, correction coils for the first and second fieldintegral have been included in the coils.

Figure 3: Undulator mockup coils with 20 mm period length and 30 cm long

the mechanical accuracies reached at room temperature for the two undu-lator halves measured along the coils in the middle and at ± 10 mm, shown in Fig. 4, are very promising.

Figure 4: Mechanical accuracies reached at room temperature for the two undulator halves measured along the coils in the middle and at ± 10 mm in the good field region [7]

the test in liquid helium made in CASpeR I showed that the coils reached 400 A without quench, being the nominal current 380 A. Considering an operating temperature of the magnet of 4.2 K, as for the short mockups a margin of about 2 K is obtained. the spectral performance calculated with SpeCtRA [8] obtained using the measured field of the mockup is encouraging. In Fig. 5 it is compared with the spectral performance calculated using the ideal magnetic field for SCu20 long as the mockup and the ideal magnetic field for a cryogenic permanent magnet undulator with 20 mm period length made of the best material available prFeB (CpMu20) [9].

Figure 5: Calculated spectral performance with SPECTRA [8] using the ideal magnetic field for SCU20 long as the mockup (thin blue line), the measured magnetic field in CASPER I of the SCU20 mockup (light blue line), and the ideal magnetic field for a cryogenic permanent magnet undulator with 20 mm period length made of the best material available PrFeB (CPMU20) [9]. The thick lines are guides for the eye of the tuning curves for the ideal fields [7].

3. First results from a cold vacuum chamber for diagnostics installed at the Diamond light SourceWith the aim of measuring the beam heat load on a cold bore, needed to specify the cooling power for the cryogenic design of superconducting IDs, and in order to gain a deeper understanding in the beam heat load mechanisms, a cold vacuum chamber for diagnostics (ColDDIAG) was built [10]. We are offering its installation in different synchrotron light sources with different energies and beam characteristics. After successful factory acceptance test [11], ColDDIAG was installed in the storage ring at the Diamond light Source (DlS) in November 2011 [12]. Due to a mechanical failure of the thermal transition of the cold beam tube, the cryostat had to be removed after one week of operation. After optimizing the design of the liner thermal transition, ColDDIAG was successfully installed a second time in the DlS in August and has been taking data till August 2013, when it has been removed to make space for a new insertion device [13].In order to determine the beam heat load to the cold liner a calibration of the temperature sensors is necessary. this is done using the heaters installed on the liner and the heaters installed at the upstream and downstream flanges connecting the 50 K shield through the thermal transitions to the cold part of the liner.With the equipped instrumentation, which includes temperature sensors, pressure gauges, mass spectrometers, as well as retarding field analyzers, it is possible to measure together with the beam heat load, the total pres-sure, the gas content, as well as the flux of electrons and/or ions hitting the chamber walls.No significant difference is observed between the measurements per-formed keeping the liner (cooling connection) at a constant temperature of 20 K and letting the liner (cooling connection) increase in temperature by beam heating. A significant discrepancy is observed from the beam heat load values predicted by heating due to geometrical and resistive wall im-pedance [14]. A further indication that the beam heat load is not due to resistive wall heating is the highly non uniform beam heat load distribution observed on the liner. As the liner is made from a single high purity copper block even small temperature gradients must be caused by large differences in the

Insertion Device Development At ANKA we pursue a research and development program to develop su-perconducting (sc) insertion devices (IDs). of fundamental importance for the realization of this program are: i) a close collaboration with our indus-trial partner Babcock Noell GmbH (BNG), and ii) the instrumentation devel-oped and under development to perform R&D. this includes improvements and quality management of the magnetic field properties and understand-ing of the beam heat load mechanisms to a cold bore.

the main activities of the last year have been:

1Design, manufacturing and tests in a lHe bath setup (CASpeR I [1], ChAracterisation Setup for phase error Reduction) of short single mockup undulator coils with 15 mm and 20 mm period length in collaboration with BNG.

2Design, manufacturing and tests in a lHe bath of 30 cm long 20 mm period length undulator mockup coils in collaboration with BNG.

3 First results from of a cold vacuum chamber for diagnostics in-stalled at the Diamond light Source (DlS)

1. test of short mockups for optimization of superconducting undulator coilsWith the aim of developing a SCu with 20 mm period length for the NANo beamline at ANKA, and a SCu with 15 mm period length for low emittance light sources to be tested at ANKA, two short mockups ( ~ 0.15 m, see Fig. 1) have been designed, manufactured and tested to qualify the wire and different winding schemes.the lessons learned from the development of the 1.5 m long coils for the SCu15DeMo to be tested at ANKA have been applied [2]:

• the thin rectangular wire with a cross section of 0.54 x 0.34 mm (includ-ing insulation), chosen to reach high precision in the winding height, is replaced by a thicker wire.

• the cobalt-iron yoke, chosen for its higher magnetization at saturation, but difficult to be procured and hard to be machined, is now substituted with low carbon steel.

• the plates made of one pole and one groove each, and used as building blocks for the long coils, will be replaced by blocks ≈ 0.15 m long.

• the coils are wound with a single strand by winding always in the same direction in every second groove from the beginning to the end of the coil, and coming back filling up the rest of the grooves. In order to allow space for the jump from one groove wound in one direction and the one next to it wound in the opposite direction, staggering on the side of the coil opposite to the beam is unavoidable. the staggering on the side of the coil opposite to the beam has been minimized to avoid a possible unwanted increase of the first and second field integrals, and a reduction of the on axis field quality. With the aim of eliminating the staggering we have changed in the next coils the winding scheme. this is done by winding each next groove one after the other, which has been successfully demonstrated experimentally on other short mockups.

• the choice of a racetrack shape has been made to reduce the magnetic field multipole components.

Figure 1: Short ( ~ 0.15 m) single undulator mockups with 15 mm (left) and 20 mm (right) period length

the load lines of the two mockups as well as the wire current needed to reach the specified field are reported in Fig. 2. the load lines have been calculated using FeMM [4]. the crossing point of the load line and the cur-rent needed to reach the specified field indicates the operating point of the magnet. the maximum current values reached by the two mockups during training in a liquid helium bath are shown in Fig. 2. In Fig. 2 it is also dis-played the critical current of the wire at 4.2 K provided by the supplier and confirmed by measurements performed at the Institute of technical physics (KIt) [5], as well as the critical current of the wire rescaled at the tempera-ture [6] at which it crosses the operating point. Considering an operating temperature of the magnet of 4.2 K both mockups show a temperature margin of about 2 K.

the two mockups reached a very high precision in the pole height devia-tion: twice better (< 19 μm) and four times better (< 9 μm) than the value specified (< 40 μm) for the 1.5 m long undulator coils, for mockup SCu20 and SCu15 respectively.

Figure 2: Load line (dots), wire critical current at different temperatures (dotted line at 4.2 K and dash-dotted line at T > 4.2 K), current goal value (continuous line), and maximum current reached in the liquid helium bath test (dashed line) of the SCU15 (top) and of the SCU20 mockup (down) [3].

Sara Casalbuoni: [email protected]

Accelerator Report


Appendix Lab ReportBeamline ReportUser Operation

μm

μm

μm


heating power. Figure 6 shows the temperature distribution for the sensors placed along the liner during a user run for 686 bunches and 300 mA after reaching thermal equilibrium. While the temperatures during the calibra-tion, for the same heating power, are within ±0.2 K, the values with beam range from 15.2 K to 18.6 K.

Figure 6: Temperature distribution on the cold liner section during user run with 686 bunches for a beam current of 300 mA and top-up operation [13]

the pressure measured in the upstream pumping section has a linear de-pendence on the beam current, in contrast to the pressure measured with the other gauges. this linear behaviour is typical for photodesorption. to shade ColDDIAG from the direct synchrotron radiation created by the up-stream bending magnet, a taper is installed between the upstream pump-ing station and the cryostat. the non-linear pressure increase after the taper demonstrates that the shading is sufficient and no synchrotron radiation is hitting the liner of ColDDIAG. Synchrotron radiation can therefore be excluded as the dominant beam heat load source in ColDDIAG. However, reflected synchrotron radiation might fill the vacuum chamber without be-ing the dominating mechanism of molecule desorption.the residual gas measured in all three sections exhibits an analogue compo-sition dominated by hydrogen.In each of the three liner sections a retarding field analyser (RFA) is installed to investigate the charged particles hitting the chamber walls. Measure-ments show that most of the particles hitting the wall have a negative charge [12]. Figure 7 shows the energy spectrum from the three RFAs lo-cated upstream, downstream and in the cold section of ColDDIAG for 686 bunches and 300 mA beam current. the measurements show that most electrons hitting the RFAs have energies below 10 eV. A rough estimation of the heating power created by electron bombardment can be obtained by assuming that all electrons hitting the cold RFA have a peak energy of 3.5 eV. using a relatively simple model the heating power p is given by p = ΔW Ṅ, where Ṅ is the number of electrons per second hitting the cold liner and ΔW is the transferred energy. Considering the above parameters, the resulting heat load is less than 1 mW. However, the measured energy spec-trum and flux might only show a fraction of the actual number of electrons hitting the wall, because the location of the RFAs could be unfortunate and the maximum detectable energy is limited to 250 eV. Moreover, the small acceptance angle of the RFA for particles with high energies traveling with a velocity component in beam direction can also reduce the amount of detected electrons.

Authors: S. Casalbuoni, S. Gerstl, N. Glamann, A. Grau, t. Holubek,Ch. Meuter, D. Saez de, Jauregui, R. VouttaKIt - ANKA, Synchrotron Radiation Facility, Karlsruhe, Germany

Figure 7: Energy spectrum from the three RFAs located upstream (us), downstream (ds) and in the cold section of COLDDIAG for 686 bunches and 300 mA beam current [13].Experimental and theoretical work is ongoing, with the aim of explaining the very high measured beam heat load compared with existing theories.

References [1] e. Mashkina, A. Grau, C. Boffo, M. Borlein, t. Baumbach, S. Casalbuoni, M. Hagelstein, R. Rossmanith, e. Steffens, W. Walter, Ieee trans. App. Su-percond. 18-2, 1637–1640 (2008).[2] S. Casalbuoni, t. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, J. Steinmann, W. Walter, Ieee trans. on Appl. Super-cond., Vol. 21-3,1760-1763 (2011).[3] S. Casalbuoni, S. Gerstl, N. Glamann, A. Grau, t. Holubek,D. Saez de Jauregui, C. Boffo, M. turenne, and W. Walter, Ieee trans. on Appl. Supercond. , Vol. 24- 3, 4101905 (2014).[4] Finite element Method Magnetics by David Meeker, http://www.femm.info/wiki/Homepage[5] M. Kläser and th. Schneider, private communication.[6] l. Bottura, Ieee trans. Appl. Supercon., vol. 10, pp. 1054-1057, 2000.[7] S. Casalbuoni, S. Gerstl, N. Glamann, A. Grau, t. Holubek, Ch. Meuter, D. Saez de Jauregui, C. Boffo, th. Gerhard, M. turenne, W. Walter, Super-conducting undulator Workshop, Didcot, uK (2014) https://eventbooking.stfc.ac.uk/uploads/superconducting_undulator/casalbuoniscusws2014.pdf[8] t. tanaka and H. Kitamura, J. Synchrotron Rad. 8, 1221 (2001).[9] th. Schmidt, private communication.[10] S. Casalbuoni, t. Baumbach, S. Gerstl , A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, G. Sikler, V. Baglin, R.Cimino, M. Commisso, B. Spataro, A. Mostacci, M. Cox, J. Schouten, e. Wallèn, R. Weigel, J. Clarke, D. Scott, t. Bradshaw, I. Shinton, R. Jones, Ieeetrans. on Appl. Supercond. 21-3, 2300-2303 (2011).[11] S. Gerstl, t. Baumbach, S. Casalbuoni, A. Grau, M. Hagelstein, t. Holubek, D. Saez de Jauregui, V. Baglin, C. Boffo, G. Sikler, t. Bradshaw, R. Cimino, M. Commisso, A. Mostacci, B. Spataro, J. Clarke, R. Jones, D. Scott, M. Cox, J. Schouten, I. Shinton, e. Wallèn, R. Weigel, proceedings of IpAC11, San Sebastian, Spain 2011.[12] S. Gerstl, t. Baumbach, S. Casalbuoni, A. Grau, M. Hagelstein, D. Saez de Jauregui, t. Holubek, R. Bartolini, M. Cox, J. Schouten, R. Walker, M. Migliorati, B. Spataro, I. Shinton, proceedings of IpAC12, New orleans, lou-isiana, 2012.[13] S. Gerstl, S. Casalbuoni, A. Grau, D. Saez de Jauregui, t. Holubek, R. Voutta, R. Bartolini, M. p. Cox, e. C. longhi, G. Rehm, J. C. Schouten, R. Walker, R. Walker, M. Migliorati, B. Spataro, proceedings of IpAC13, Shang-hai, China, 2013.[14] S. Casalbuoni , M. Migliorati, A. Mostacci, l. palumbo, B. Spataro, JINSt 7 p11008 (2012).

Sara Casalbuoni: [email protected]

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Appendix Lab ReportBeamline ReportUser Operation


Beamline Report

Beamline Report

Spectroscopy XAS Sul-X IR1 IR2 WeRA INe uV-CD12

Scattering and ImageNANo SCD pDIFFMpI Fluotopo-toMoIMAGe

MicrofabricationlIGA I, II, III

Appendix Lab ReportAccelerator ReportUser Operation


XASMultipurpose high throughput XAS beamline

the XAS beamline spans the energy range from 2.4 to 27 keV. this covers the K-edges from S to Cd, and up to the l-edge of u. the double crys-tal monochromator design allows exchanging the two parallel mounted Si(111) and Si(311) crystal pairs within minutes. there are two principal modes of detection: transmission and fluorescence measurements. the flu-orescence radiation emitted by the sample as a function of photon energy is recorded using different energy dispersive detector. Additional to stan-dard eXAFS the XAS beamline offers grazing incident XAFS (GI-XAFS) and Q-XAFS. While the standard XAFS-mode is suited for measurement longer than 30 min, the Q-XAFS mode enables scan times of 30 sec. even with this mode it is possible to read out the complete fluorescence spectrum for each incoming photon energy due to the XIA-XMap electronic (1 year stable user operation). this will enable a multi-peak fitting of the fluorescence spectra throughout the spectrum and, thus, a higher precision of the resulting data. typical beam size is 8 mm (hor) x 1 mm (ver) (range 1 x 1 mm2 to 20 x 1 mm2).the XAS beamline offers different types of sample stages: While the high throughput sample stage offers fast sample exchange at standard condi-tions, a closed cycle He-cryostat can be used for measurements down to 15 K. A goniometer can be used for the integration of large set-up’s (75 kg) and GI-XAS measurements. In future a sample stage based on cooling with liquid N2 will offer faster sample exchange with cryostat.

Developments in 2013

A new heavy load experimental table (6 degree of freedom) was installed in summer shutdown 2013 to be able to handle experiments with heavier und more complex sample cells. even with the 6 degree of freedom, the table surface is now 8 cm lower as before (beam height over table 53 cm). In addition to these two advantages, the re-alignment of the experimental set-up after changed positions of the electron beam can be done within 1h. the detector systems are now installed on a multi detector holder, which enables fast changes between 5 element Ge-detector, one element vortex detector and a 6 element SDD with a 100 mm2 per element. this detector offers even higher throughput with an extraordinary energy resolution be-low 210 eV at 260 ns peaking time. the radical new monolithic design has the advantage of nearly no dead space in between the detector pixel. A liquid sample cell was developed in cooperation with Sul. the advanced design of the cell provides very small changes of the volume due to very low vibration of the pump and very stiff windows. A holder for up to 18 sample is available for installation on Huber tower or Hexapod.to further enhance the availability of the beamline, the control system noti-fies the user if for any reason a Q-XAFS or eXAFS scan is not ended in time.

planned upgrades

to enable faster changes of the set-up a special clamp system will be in-stalled late summer. In the mid term future it is planned to develop a new cryostat system and to extend the low energy set-up to be able to handle small in-situ set-ups.

user operation

the XAS beamline is heavily overbooked and the maximum possible user operation time is mainly determined by personnel limitations. A power outage in 2013 led to serious damage to the DCM. We were able to repair the equipment successfully on site, but lost only three weeks of user operation.

Hot topics are battery science, catalysis, thin layers and environmental science. the fraction of complex in-situ experiments is constantly increasing. A reasonable maintenance time of less than 10% is used to keep the beamline at a high quality level. Four days of beamtime were used to show the capabilities of the beamline for radiography but such complex experiments can be done only in cooperation with the beamline scientist.

Figure 1: 6 element SDD (100mm2)

Figure 2: New sample holders for small samples and pellets

Spectroscopy Stefan Mangold : [email protected]

Beamline Report Appendix Lab ReportAccelerator ReportUser Operation

XAS | SUL-X | IR1 | IR2 | WERA | INE | UV-CD12 | NANO | SCD | PDIFF | MPI | FLUO | TOPO-TOMO | IMAGE | LIGA I, II, III


SUL-Xthe Sul X-ray beamline enables investigation of samples – without remount-ing them – sequentially with X-ray fluorescence spectroscopy (XRF), X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD). It uses a wiggler as radiation source, focuses the beam with two mirrors to a slit that de-fines a new source with adjustable size. A Kirkpatrick-Baez mirror system is subsequently used to de-magnify the new source to the sample position. All detectors except the SDD detector operate under vacuum to reach K absorption edges of e.g., p, S and Cl. the CCD detector for XRD is also vac-uum compatible to avoid dismounting during vacuum operation. Besides bulk analysis microfocus XRF, XAS and XRD, grazing incidence XAFS (GI-XAFS), total e-yield XAFS or fast continuous measuring XAFS (Q-XAFS) are offered to users, with beam-size variable from approximately 1 x 1 mm2 to 50 x 40 μm2. Q-scans allow XANeS measurements in typically 1-3 min. total e-yield measurements are restricted to conductive samples. Since 2007 the beamline is operating almost 100% in user operation and needs now time for major upgrades.

overviewthe main components of the experimental station are:

• Vacuum chamber (Fig. Sul 3a) with sample holder (diffractometer with linear stages) and detectors for operation under high vacuum (HV). Vac-uum is required for measurements at low energies. A pre-vacuum pump (screw pump with 650 m3/h) is installed at the roof of the experimental hutch and a turbo-molecular pump (tMp) is available to reach a vacuum better than 10-4 mbar in a reasonable time of about 15 to 20 min.

• Diffractometer (Huber, fig. Sul 3b) with horizontal 2-theta and omega circle (360°), chi cradle (10°, vertical)), phi circle (360°, horizontal), hori-zontal movements x (100 mm) and y (40 mm), vertical movements z1 (90 mm) and z2 (15 mm) as sample holder for sample with 100 mm size and less than 3 kg weight

• CCD detector (photonic science XDR-VHR 2) mounted on the horizontal goniometer (2 theta), active window 124.8 mm vertical, 83.2 mm hori-zontal with pixel size on taper 31.2 µm x 31.2 µm

• Ionization chambers (ADC, type Custom IC-500-100) modified for oper-ation under vacuum with 13 µm Kapton windows, usable with N2, Ar, Ar(20%)-N2(80%) mixture between 50 and 1000 mbar, using Keithley 428 current amplifiers

• 7 element Si(li) Fluorescence detector (Gresham, now SGX Sensortech (MA) ltd), active area per element 30 mm2, energy resolution 360eV for 500 nsec, 220eV for 2 µsec, 144eV for 12 µsec, using XIA Xmap electronics

• optical microscope (thalheim Spezial optik tSo, Camera AVt Merlin F145C2), for in vacuum operation, resolution about 2 µm, with transmit-ted, reflected and leD ring light sources

• Additional linear stages for reference foils and primary beam stop Available methods include microfocus / grazing X-ray absorption spec-troscopy (XAS) in transmission and fluorescence geometry, also with total e- yield (teY), microfocus X-ray fluorescence spectroscopy (XRF) and X-ray powder diffraction (XRD).

Developments in 2013Because no conventional cryogenic sample holder fits to our sample stage a specific device for cooling samples down to -100°C was constructed and a prototype has been built. Applications are reducing of irradiation effects on radiation sensitive samples and to investigate cryogenic mineral phases or phase transformations at low temperatures for example.

A compact theta-2theta goniometer in vertical geometry for small samples is in the process of production. It will enable for example measurements of X-ray absorption spectra in different crystallographic orientations of single

crystals. It can be equipped optional with a photodiode or avalanche pho-todiode as detector.

In the mid-term it is planned to replace the seven element Si(li) detector with a multi element Silicon Drift Diode (SDD) detector sustaining higher count rates and therefore being more capable of detecting trace elements.

A project for a mirror system for efficient suppression of higher harmonics for X-ray absorption spectroscopy below 3 keV has been submitted.

user Activities in 2013During 2013 finally 17 proposals have received beamtime (note that the number of proposals here is for the calendar year whereas the figures in the table refer to calls and represent the accepted proposals). the majority of beamtime at the Sul-X beamline has been requested by and granted to users from the environmental research field (about 59% of proposals). Among those were three proposals that combined environmental science with material science from the Celitement group and the mineralogical fac-ulty of the university of Halle who were using the hydrothermal reaction chamber recently developed by the Celitement group to track mineral fluid reactions to improve a novel cement type. the other user applications came from Material Science and Nano and Micro technology (each about 18 %) and a minor fractions was from life science (1 proposal).

other projects from environmental science comprise mainly speciation of element in different parts of our environment like Se in plants, Zn an As in soils, As in aerosols, Ni, Zn and u in clay minerals. topics in Material Science and Nano and Micro technology were for example: Investigation of phosphorous doping of Silicon nano-crystals (SiNC) for third generation photovoltaic devices, development of lead-free ferroelectric materials, de-termination of oxidation state and coordination number of eu in epitaxial europium silicide (euxSi1-x) films and nano-islands as part of investigations to downscaling of CMoS devices, and picosecond resolved X-ray scatter-ing in low alpha mode to solve questions of ultrafast structural dynamics of condensed matter systems, such as photo-excited molecules, nanoscale dynamics or phonon dynamics in crystalline substances. Research in life sci-ence focused on sulfur speciation in human prostate cancer tissues.

Approximately 10% of the total beamtime has been used for industrial customers and about 10% for in-house research and feasibility test of user projects. Fifteen percent of the beamtime was needed for quality assurance and maintenance, a fraction which is increasing from year to year due to the aging of beamline components.

A feasibility test of DAFS spectroscopy has been performed but is not yet in a state to be offered for users.to improve the lateral resolution and to enable parallel detection of X-ray fluorescence spectra across an area of interest at the Sul-X beamline the X-ray color camera (SlCam) of the Institute for Scientific Instruments GmbH has been tested with its demagnification capillary optics. evaluation is on-going.

Whether the above hydrothermal reaction chamber will lead to a new re-search field at the beamline will depend on the personnel situation in the above mentioned institutions and on its applicability to topics of users who are doing research in the accessible pressure and temperature range (up to 16 bar water pressure and 200 °C).

New, key in-house research activities at the beamline during the last calls involve the analyses of thin films for hard coatings with eXAFS spectroscopy and XRD and transmission full field X-ray absorption spectroscopy.

Spectroscopy

three examples of research projects in 2013 are summarized in the follow-ing short descriptions. the reader is referred to the publications list for more information:

(1) Cobalt Binding in the Photosynthetic Bacterium Rhodobacter (R.) Sphaeroides by X-ray Absorption Spectroscopy

QuestionChemical fate of bioaccumulated Co on bacterium R. sphaeroides

Experimental ApproachCo K XANES and EXAFS on R. sphaeroides samples containing whole cells and cell-free fractions obtained from cultures exposed to 5 mM Co2+ solu-tions

Results• octahedral coordination for Co, oxygen- ligand atoms in first shell.• In soluble cell portion Co binds to carboxylate.• on photosynthetic membrane Co also binds to sulfolipids in large quan-

tity, a typical response mechanism of R. S. to abiotic stress.

eXAFS signals (left) and Ft (right) of R. sphaeroides grown in 5 mM CoCl2 solution: Measured (dots), calculated with (dotted lines) and without (full lines) MS paths

Co binding sites: Co coordi-nated to four water molecules and (a) two sulfonic groups or (b) two carboxylic groups.

Reference(s)Belviso B., Italiano F., Caliandro R., Carrozzini B., Costanza A., trotta M. (2013) Cobalt binding in the photosynthetic bacterium R. sphaeroides by X-ray absorption spectroscopy. BioMetals, 26, 5, 693-703

(2) In-situ XRD Measurements Under Hydrothermal Conditions

QuestionDevelopment of environmentally friendly building materials on the basis of α-Ca2[HSio4](oH): Celitement® and “belite” cements.

Experimental Approach• InsituX-raydiffraction:16keV,2θ = 3 - 30° (d = 14 - 1.5 Å)• Reactioncell:200°C,16barsaturatedsteampressure,pH=13

Setup at the Sul-X beam-line

Start diffraction pattern end (after about 8 h) diffraction pattern

Hydrothermal reaction cell

ResultsDissolution kinetics of starting material, transformation, identification and kinetics of formation of calcium-silicate-hydrate reaction products• Dissolution of Ca(oH)2

• Formation of nanocrystalline calcium-silicate-hydrate• Multistage formation of α-Ca2[HSio4](oH)

Figure 1: XRD reflection intensity as a function of time



Ralph Steininger: [email protected] Jörg Göttlicher: [email protected]


(3) Spatially resolved XAS and XRD study of sputter-deposited hard coatings with composition gradient

Multi-element hard-coating materials based on transition metals, such as Cr-Al-N, are widely used in industry. their mechanical properties including hardness and friction depend on the composition and microstructure of the coating. Many samples are required to find the optimum coating for a certain application. one powerful technique for reducing the number of experiments is based on the so-called combinatorial approach for thin film deposition, exploiting the deposition gradient resulting e.g. from codeposi-tion of several materials from a segmented sputter target (Figure 1). With increasing Al content, Cr-Al-N undergoes a transition from fcc to hcp, which influences significantly the microstructure and the hardness of the system. Most promising for applications is an fcc structure with high Al content. Far from the transition region, the crystalline structure can be easily determined by XRD, while close to the transition region, several co-existing phases with small domains only detectable by eXAFS might form. therefore, a combined, spacially resolved XAS and XRD study of a Cr-Al-N coating deposited from a segmented target was performed at the Sul-X beamline. the composition gradient was verified using X-ray fluorescence mapping, which required also the vacuum option of the beamline. (Figure 2).

Interestingly, the microstructure (including texture, strain, and grain size) is also influenced by the deposition geometry (Figure 3.). In the frame of a KIt inhouse collaboration project between the IAM-AWp, the IpS and ANKA, both the detailed aspects of the composition-dependent microstructure of Cr-Al-N and related materials and the influence of the codeposition process itself are studied in detail.

Figure 1: Magnetron sputtering using the seg-mented sputter target

Figure 2: X-ray fluorescence mapping of Cr and Al over the large substrate

Figure 3: X-ray diffraction pattern on selected positions

(220)

Spectroscopy

Beamline publications 2013 • Belviso B., Italiano F., Caliandro R., Carrozzini B., Costanza A., trotta M.

(2013) Cobalt binding in the photosynthetic bacterium R. sphaeroides by X-ray absorption spectroscopy. BioMetals, 26, 5, 693-703

• Bolanz R.M., Wierzbicka-Wieczorek M., Caplovicová M., uhlík p., Göttli-cher J., Steininger R. Majzlan J. (2013) Structural Incorporation of As5+ into Hematite. envirnonmental Science and technology, 47, 9140-9147

• Czapla J., Kwiatek W.M., lekki J., Dulińska-litewka J., Steininger R., Göt-tlicher J. (2013) Chemical species of sulfur in prostate cancer cells studied by XANeS spectroscopy. Radiat. phys. Chem., 93, 154-159

• Czapla J., Kwiatek W.M., lekki J., Kisiel A., Steininger R., Goettlicher J. (2013) eXAFS studies of prostate cancer cell lines. Journal of physics: Conference Series, 430, 012040

• Fischer M., thomas D.N., Krell A., Nehrke G., Goettlicher J., Norman l., Meiners K.M., Riaux-Gobin C., Dieckmann G. S. (2013) Quantification of ikaite in Antarctic sea ice, Antarctic Science, 25, 421-432

• Gamaletsos p., Godelitsas A., Dotsika e., tzamos e., Göttlicher J., Filippi-dis A. (2013) Geological Sources of As in the environment of Greece: A Review, in: the Handbook of environmental Chemistry (Springer 2013) doi: 0.1007/698_2013_230

• Goettlicher J., Kotelnikov A., Suk N., Kovalski A., Vitova t., Steininger R. (2013) Sulfur K X-ray absorption near edge structure spectroscopy on the photochrome sodalite variety hackmanites, Z. Kristallogr., 228, 157–171

• Hiller e., petrák M., tóth R., lalinská-Voleková B., Jurkovič l., Kučerová G., Radková A., Šottník p., Vozár J. (2013) Geochemical and mineralogi-cal characterization of a neutral, low-sulfide/high-carbonate tailings im-poundment, Markušovce, eastern Slovakia, environ Sci pollut Res., DoI 10.1007/s11356-013-1581-5

• Issenmann D., Ibrahimkutty S. , Steininger R., Göttlicher J , Baumbach t., Hiller N., Müller A-S., plech A. (2013) ultrafast laser pump x-ray probe experiments by means of asynchronous sampling, J. phys.:Conf. Ser. 425, 092007

• Kilias S.p., Nomikou p., papanikolaou D., polymenakou p. N., Godelitsas A., Argyraki A., Carey S., Gamaletsos p., Mertzimekis t.J., Stathopoulou e., Goettlicher J., Steininger R., Betzelou K., livanos I., Christakis C., Croff Bell K., Scoullos M. (2013) New insights into hydrothermal vent process-es in the unique shallow-submarine arc-volcano, Kolumbo (Santorini), Greece, SCIeNtIFIC RepoRtS 3 : 2421

• Mangold S., Steininger R., dos Santos Rolo t., Göttlicher J. (2013) Full field spectroscopic imaging at the ANKA-XAS- and -Sul-X-Beamlines. Journal of physics: Conference Series. 430 (2013)

• Mangold S., Steininger R., Spangenberg t. (2013) High throughput data acquisition at the XAS and Sul-X beamline at ANKA. Journal of physics: Conference Series, 430 (2013) 012022

• Noked o., Melchior A., Shuker R., livneh t., Steininger R., Kennedy B.J., Sterer e. (2013) pressure-induced amorphization of la1/3tao3 .J. Solid State Chem., 202, 38–42

• Veselská V., Majzlan J., Hiller e., petková K., Jurkovic l., Ďurža o., Vole-ková-lalinská B., (2013) Geochemical characterization of arsenic-rich coal-combustion ashes buried under agricultural soils and the release of arsenic. Applied Geochemistry, 33, 153–164

• Vitova t., Denecke M.A., Göttlicher J., Jorissen K., Kas J.J., Kvashnina K., prüßmann t., Rehr J.J., Rothe J. (2013) Actinide and lanthanide spe-ciation with high-energy resolution X-ray techniques. Journal of physics: Conference Series, 430, 012117

• Winkel l. H. e., Casentini B., Bardelli F., Voegelin A., Nikolaidis N. p., Charlet l. (2013) Speciation of arsenic in Greek travertines: Co-precipi-tation of arsenate with calcite. Geochimica et Cosmochimica Acta, 106 (2013) 99–110

• Ziegler S., Dolch K., Geiger K., Krause S., Asskamp M., eusterhues K., Kriews M., Wilhelms-Dick D., Goettlicher J., Majzlan J., Gescher J. (2013) oxygen-dependent niche formation of a pyrite-dependent acidophilic consortium built by archaea and bacteria, the ISMe Journal, 7, 1725–1737



Ralph Steininger: [email protected] Jörg Göttlicher: [email protected]


Figure 3: The experimental setup of the IMS group is in the foreground, behind it is the IR1 diagnostic port

Developments in 2013the ellipsometry station at IR1 has now been in continuous operation for 13 years. the Bruker 66v/s FtIR spectrophotometer at this station was discon-tinued by the manufacturer some years ago and will become increasingly difficult to service and maintain in the coming years. Discussions of the situation with MpI-FKF Stuttgart led to the decision to replace the spectro-photometer with Bruker’s new flagship research instrument, the Vertex 80v, within the next few years. Good progress was made with the BMBF-funded project to install a new experimental station for spectroscopy under extreme conditions at IR1. the project kick-off meeting took place at ANKA on 30th october 2013, attended by the Augsburg and Bayreuth teams as well as representatives of the ANKA directors and relevant departments. At this and subsequent meetings, the options for the layout of the station within the IR1 hutch as well as for the required ancillary working areas were dis-cussed, and optimal solutions were agreed. In addition, the Augsburg team presented their initial design for the custom IR microscope for review, and concepts for the coupling of the instrument to the synchrotron beam were discussed. the FtIR spectrophotometer for the new station was ordered towards the end of the year.

user Activities 2013Infrared spectroscopy is characterized by an especially broad range of appli-cations, thus the ANKA-IR user community includes researchers from many other fields including geology, materials research, surface science, micro-technology, nanosciences and biological sciences.In 2013 a total of 7 in house, external and long term projects were hosted at the IR1 beamline, comprising 22 blocks of beamtime. As in the previous years the IR1 beamline was primarily used by the groups of Christian Bern-hard (university of Fribourg) and Alexander Boris (Max planck Institute for Solid State Research). the IR1 beamline was also used regularly for in-house projects by the tHz group (lAS, KIt), who exploit the beamline’s extraction optics and diagnostic port for ultrafast studies of the electron beam tem-poral structure in low α mode. our regular users at IR1 also included the groups of Michael Siegel (IMS, KIt) who develops ultra fast tHz detectors which are then characterized with the coherent IR/tHz synchrotron beam, and of petra Hellwig (university of Strasbourg) for studies of structure and dynamics during protein-protein interactions.

Spectroscopy

Beamline Report

IR1 Beamline for Infrared/tHz spectroscopy and ellipsometry the IR1 beamline at ANKA is primarily used for research work in the area of solid state physics. Its experimental station for IR/tHz ellipsometry, operated jointly by the Max planck Institute for Solid State Research in Stuttgart and the university of Fribourg in Switzerland, is mainly dedicated to investigations of the mechanism of high temperature superconductivity. the new experimental station for for studies of solids at extreme temperature and pressure, currently under construction in a BMBF-funded collaboration with the universities of Augsburg and Bayreuth, will be used for example for characterization of ex-otic electronic and structural states of matter under extreme conditions and for tuning the ground state of strongly interacting low-dimensional electron systems. In addition, the FtIR vacuum spectrometers at the heart of both ex-perimental stations can be used independently for IR/tHz spectroscopy in any field of science.

Figure 1: The ellipsometric assembly at IR1. Key: (IFS) = Bruker IFS 66v/S FTIR spectro-photometer, (P) = polarizer , (A) = analyzer, (D) = liquid He cooled bolometer detector

overviewIn 2013 the IR1 beamline provided 58 days of 107 available days for user operation. In addition, 19 days of special user operation beamtime in low α mode were provided. 10 days were spent for maintenance, development and pilot experiments.

the methods IR spectroscopy in transmission, reflection, attenuated total reflectance and IR ellipsometry are implemented at the IR1 beamline by the ellipsometer (supplied by MpI-FKF, Stuttgart) that is coupled to an FtIR spec-trometer (Bruker IFS 66v/S) covering a spectral range from 4 to 10,000 cm-1 (0.5 meV to 1.24 eV, 2.5 mm to 1 μm) with a resolution down to 0.1 cm-1. It is equipped with high-sensitivity detectors (liquid-He cooled bolometers, liquid N2 cooled MCt (HgCdte) and InSb detectors, and Si or Ge diodes) and appropriate beamsplitters (Mylar films, multilayer, KBr and quartz). the instruments are evacuated or N2 purged to avoid water and Co2 absorp-tion bands. the ellipsometer operates under vacuum and is provided with an optimized bolometer detector and a liquid He cryostat.

Figure 2: The THz group‘s experimental setup for electron beam time structure studies in operation at the IR1 diagnostic port

the new experimental station for studies of matter under extreme con-ditions will consist of a state-of-the-art vacuum FtIR spectrophotometer (Bruker Vertex 80v) coupled to a custom long working distance microscope that is currently under construction in the laboratory of prof. Christine Kuntscher at the university of Augsburg. the microscope is designed to accommodate a diamond anvil cell in a liquid He cryostat. Static pressures of over 800 Gpa will be generated in a double-stage diamond anvil cell based on nanopolycrystalline diamond, developed in the laboratory of the other partner in this BMBF-funded project, prof. Natalia Dubrovinskaia of the university of Bayreuth. this far exceeds the highest pressures available at synchrotron infrared beamlines to date and will be used for example for studies of the structural, electronic, vibrational and optical properties of elemental solids such as hydrogen and boron at pressures high enough to close their band gaps.

Figure 4: Christine Kuntscher at the IR1 beamline with her experimental station for infrared spectroscopy at extreme pressures and temperatures



David Moss: [email protected] Mathis: [email protected]

Biliana Gasharova: [email protected] Süpfle: [email protected]


user Activities in 2013New equipment has been commissioned, for example a rotational posi-tioner of the company SmarAct for polarized microscopy measurements; a heating stage FtIR600 of the company linkam for in situ experiments up to 600°C.

In fall the microscopy station has been opened to pilot experiments of ex-perienced users: • We continued our contributions to the award winning Celitement®

project. Continuous cutting-edge fundamental research helps the under-standing and thus the sustained success of novel materials design. one example is the in situ study of the phase transformations upon heating of α-Ca2[HSio4](oH), which is one very promising precursor for the devel-opment of novel energy and Co2 efficient cements. this pilot experiment was combined with the commissioning of a linkam FtIR600 heating stage, which is now in operation and available to our general users.

• the users groups around Frank Neubrech (university of Stuttgart) and Christian Huck (university of Heidelberg) performed pilot experiments at the IR2 microscopy station on metal nanowires. performing SeIRS (surface-enhanced infrared spectroscopy) with organic probe molecules on nanowires of varying materials and geometry, they gain insight in the dependence of vibrational signal enhancement on internal damping, as well as scattering and absorption characteristics of nanostructures.

Figure 5: Christian Huck (University Heidelberg) at the IR microscopy station measuring resonances of gold nanowires in the mid-IR

User Operation Accelerator Report Beamline Report Lab Report Applications Appendix

2012 ANKA ANNUAL REPORT | 32

In the design of the IR2 beamline there has been a special focus on reduction of ground vibrations. The infrared beam is transported by mirrors, and due to the long optical path length the mirror vibrations add up directly to the synchrotron beam fluctuations. Especially the water cooling of the primary extraction mirror introduces additional oscillations that can be seen as intensity fluctuations at the experimental stations. Therefore a fast feedback system similar to the one at the ALS infrared beamline has been installed. In a first step the characteristic fluctuation frequencies of the IR2 beamline have been measured. In the future they will be damped by a piezo driven mirror system that stabilizes the beam to ensure constant measurement conditions at the IR2 experimental stations.

Since Bruker Optics no longer supports their older IR spectromers such as the IFS66v/S currently at IR2, a new Vertex80v FTIR spectrometer was purchased. Its coupling to the beamline and IR microscope will require re-design of the station

and compatibility tests. In order not to further delay the opening of the IR2 microscopy station, its installation and commissioning will follow at a later date.

Progress has also been made with the second experimental station at IR 2, the infrared nanoscope (Fig. 5). The purpose of this unique instrument is to provide broadband infrared spectroscopy and imaging at a lateral resolution orders of magnitude better than the diffraction-limited resolution provided by conventional optics. This is achieved by exploiting the field enhancement effect at an AFM tip as it contacts the surface of the sample: the infrared light reflected at the tip position is extracted from the general reflected signal by locking onto the AFM tapping frequency, giving a lateral resolution determined effectively by the size of the AFM tip. The experimental station, based around a commercial AFM from WITec, was developed by our partners from the Martina Havenith group (University of Bochum) within the framework of a BMBF Verbundsforschung project. In 2012 the coupling through the FTIR Vertex80v has been realized (Fig. 6) and the coupling of the IR synchrotron beam into the nanoscope is currently under design.

User operationIn 2012 the IR microscopy station has been in regular use with its built-in thermal light source, in particular for the IR group’s continuing contributions to the award winning Celitement® project. An innovative reaction cell for hydrothermal synthesis was designed and commissioned in collaboration with the Building Materials group of ITC (KIT). It allows for complementary in-situ investigation of reaction kinetics at both the IR microscope as well as at the SUL-X beamline. The IR microscope has been further used in a number of KIT-internal collaborations within the framework of the BioInterfaces program and for projects of some external users.

After the successful commissioning of the IR microscope with synchrotron light in August 2013 the station has been opened for external users. The first external user groups and in-house projects for work with IR synchrotron light are scheduled for September 2013.

v

IntroductionWhen ANKA opened for the general user community in March 2003, the IR beamline with its IR microspectroscopy station immediately became ANKA’s most heavily oversubscribed beamline with over 400% overdemand. Within 5 years, the decision had been taken to move the IR miccroscope to a new infrared beamline in order to provide more beamtime by no longer having to share the beam with the vacuum ellipsometry station. This also provided the opportunity to make a number of improvements to the design of the beamline in order to enhance performance even further. This ambitious project required an extended period of time until satisfactory solutions could be found for all the technical issues. It is therefore with great pleasure that we report that IR2 is now open for users.

The lateral resolution achievable with conventional synchrotron IR microscopy is restricted by classical optical diffraction limit, which is an increasingly significant limitation into the long wavelength range. A novel near-field approach is being implemented at IR2’s second experimental station, in which lock-in detection of field-enhanced scattering from a tapping AFM tip will provide broad-band IR spectroscopy with a lateral resolution two orders of magnitude better than the optical diffraction limit.

Construction progressFurther issues that have delayed the opening of this new IR microspectroscopy beamline have been identified and solved. The unacceptable temperature increase upon irradiation with synchrotron light of the actively cooled surface of the extraction mirror was traced to an error in the contractor’s design for the water cooler. After several improvement attempts a new cooler has been designed, assembled (Fig. 1) and installed at IR2 (Fig. 2) in the January 2013 shutdown. Finally, bake out and conditioning with synchrotron beam (Fig. 3) confirmed that the beamline is now working as designed. Consequently a basic commissioning with synchrotron light could be conducted. Test experiments at the IR2 diagnostic port (Fig. 4) and with the IR microscope showed that the introduction of the window changer further downstream, just one of the improvements compared to the design of IR1, indeed leads to increased flux.

IR2 Beamline for IR/THz Micro and Nano Spectroscopy


WERA | U V-CD 12 | I R1 | I R2 | X AS | F LUO | SUL-X | INE | L IGA | S CD | I MAGE | T OPO-TOMO | S CD | P DIFF | N ANO | M PI-MF

Spectroscopy

David Moss: [email protected] Yves-Laurent Mathis: [email protected]

Biliana Gasharova: [email protected] Michael Süpfle: [email protected]

Beamline: +49 (0)721 608 26613

CONTACT

Figure 4: The experimental setup of the THz group with two bolometer detectors, behind it is the IR2 diagnostic port.

Figure 2: The holder containing the extraction mirror M1 is installed at IR2 after re-designing of the water cooling system.

............................................Information

The IR2 beamline is ANKA’s second infrared beamline, constructed primarily in order to provide more beamtime at the experimental station for IR/THz microspectrosopy due to the consistently high demand for this techique amongst ANKA’s users. In a subsequent development, BMBF funding obtained by the University of Bochum was used to establish an additional experimental station for near-field IR/THz nanospectroscopy which is currently under construction.

Figure 1: Assembling the new water cooler of the extraction mirror M1 of the IR2 beamline.

Figure 3: The IR2 synchrotron light in the visible range, projected on a sheet of paper 4 m from the diagnostic port.

Figure 6: The IR nanoscope under construction at IR2.

Figure 5: IR2 beamline experimental stations: on the right-hand side in the foreground is the IR microscopy station with a Bruker IFS66v/S spectrometer coupled to an IRScope II infrared microscope equipped with single element and imaging detectors, and on the left-hand side the new IR nanoscopy stati-on with the WITec AFM (in the acoustic isolation box) and Bruker Vertex 80v FTIR spectrometer. In the background are the fast feedback system, window changer and diagnostic port.

Figure 6: IR2 beamline experimental stations: on the right-hand sight in the foreground is the IR microscopy station with a Bruker IFS 66v/S spectrophotometer coupled to an IRscope II infrared microscope equipped with single element and imaging detectors.On the left-hand side the new IR nanoscopy station with the WITec AFM (in the acous-tic isolation box) and Bruker Vertex 80v FTIR spectrometer. In the background are the fast feedback system, window changer and diagnostic port.

IR2 Beamline for IR/tHz Micro and Nano Spec-troscopy

the IR2 beamline is ANKA’s second infrared beamline, constructed primarily in order to provide more beamtime at the experimental station for IR/tHz microspectrosopy due to the consistently high demand for this techique amongst ANKA’s users. In a subsequent development, BMBF funding obtained by the university of Bochum was used to establish an additional experimental station for near-field IR/tHz nanospectroscopy which is currently under construction.

overviewthe experimental stations are based on FtIR spectrophotometers (Bruker Vertex80v and IFS 66v/S), covering a spectral range from 4 to 10,000 cm-1 with a spectral resolution down to 0.1 cm-1, and equipped with high-sensitivity detectors and appropriate beamsplitters for all spectral rang-es. the vacuum spectrophotometer is complemented by a Bruker IRscope II infrared microscope with single-element and imaging detectors, including a liquid He cooled bolometer for the far IR spectral range down to 100 cm-1.

A selection of microscope objectives is available for measurements in trans-mission, reflection, grazing incidence, and AtR sampling geometry. the microscopy station exploits the brilliance advantage of synchrotron light to offer infrared/tHz microspectroscopy at measurement spot sizes down to the diffraction limit.

Developments in 2013Further issues that have delayed the opening of this new IR microspectroscopy beamline have been identified and resolved. the temperature increase upon irradiation with synchrotron light of the actively cooled surface of the extraction mirror was traced to an error in the contractor’s design for the water cooler. A new cooler has been designed, assembled (Fig. 1) and installed at IR2 (Fig. 2) in the January 2013 shutdown.









v







Spectroscopy



Beamline: +49 (0)721 608 26613

CONTACT



............................................Information






Figure 1: Assembling the new water cooler of the extraction mirror M1 of the IR2 beamline









v







Spectroscopy



Beamline: +49 (0)721 608 26613

CONTACT



............................................Information






Figure 2: The holder containing the extraction mirror M1 is installed at IR2 after re-de-signing of the water cooling system

Finally, bake out and conditioning with synchrotron beam (Fig. 3) confirmed that the beamline is now working as designed.









v







Spectroscopy



Beamline: +49 (0)721 608 26613

CONTACT



............................................Information






Figure 3: The IR2 synchrotron light in the visible range, projected on a sheet of paper 4m from the diagnostic port

Consequently a basic commissioning with synchrotron light could be con-ducted. test experiments at the IR2 diagnostic port (Fig. 4) and with the IR microscope showed that the introduction of the window changer further downstream, just one of the improvements compared to the design of IR1, indeed leads to increased flux.









v







Spectroscopy



Beamline: +49 (0)721 608 26613

CONTACT



............................................Information






Figure 4: The experimental setup of the THz group with bolometer detectors, behind it is the IR2 diagnostic port

Spectroscopy David Moss: [email protected] Mathis: [email protected]

Biliana Gasharova: [email protected] Süpfle: [email protected]




WERASoft x-ray analytics facility With a bending magnet as the source, IFp’s soft x-ray analytics facility WeRA covers photon energies from 100 to 1500 eV with a resolution e/Δe up to 104. linear and circular polarization can quickly be selected and switched. exper-imental stations for photoemission electron microsopy (peeM), for soft x-ray absorption (NeXAFS) and photoemission (peS, ARpeS), and for soft x-ray mag-netic dichroism (XMCD) are in operation. the latter is provided by the Max-planck Institute for Intelligent Systems (MpI-IS), Stuttgart, in the framework of a long-term cooperation. the stations are connected in ultrahigh vacuum to preparation chambers such as for pulsed-laser deposition (plD), for thin-film and surface preparation, and for carbon-based and other nanomateri-als. Auxiliary in-situ analysis by methods like leeD and RHeeD is available.

the spectroscopic techniques provide a multi-faceted and detailed picture of the electronic and magnetic structure, covering aspects like band or orbital character and occupancy, charge, orbital, or magnetic order, spin and orbital magnetic moments; they address diverse energy scales and various degrees of bulk and surface sensitivity; they can be made specific to elements, to lat-tice sites, or even to valences of a single element; and imaging of topograph-ic, chemical, or magnetic contrast as well as spectromicroscopy (μ-NeXAFS, μ-peS, μ-ARpeS, μ-XMCD) provides laterally resolved information. the setup is designed for combining all these spectroscopic and preparation techniques in order to obtain further insight.Recently, MpI-IS has upgraded the XMCD station by a fast-ramp magnet pro-viding high magnetic fields up to 7 t. Radiation from an undulator will be avail-able at WeRA; all methods will benefit greatly from the increased photon flux and flux density at the sample.

Spectroscopy Stefan Schuppler: [email protected] peter Nagel: +49 (0)721 608 26560

Michael Merz: [email protected]




upgrades in 2013In 2013 a multi-analyzer crystal (MAC) spectrometer for high (energy) resolution X-ray emission spectroscopy (HRXeS) has been installed at the INe-Beam line (Fig. 3). the spectrometer assembly comprises a mobile and a stationary positioning unit. the five analyzer crystal positioning stages possess four degrees of freedom each. the crystal stages are mounted on a common granite block, which is installed on a mobile rack, hosting power supplies and motion controllers for all 23 spectrometer axes. the station-ary detector positioning unit comprises three degrees of freedom (a long and a short linear stage and a rotation stage), which allow the detector to be moved along the Rowland circle. the MAC spectrometer has been commissioned and exhaustively tested in various pilot experiments at the INe-Beamline in 2013. Due to flux limitations at the INe-Beamline, the HRX-eS spectrometer is foreseen to be moved as the future core component to the neighboring ACt experimental station upon finishing setup and com-missioning of the new CAt-ACt high energy / high flux X-ray spectroscopy beamline at ANKA in 2015.

user Activities 2013INe in house projects in 2013 included various investigations of the structur-al incorporation of actinides and chemical homologues in colloids and sec-ondary mineral phases, aqueous speciation of actinides in highly saline solu-tions, the redox chemistry of Np(VI)/Np(VII), th(IV) solubility in the presence of fulvic acid and the pH dependency of Am(III) complexation with acetate.

For the first time ever at a synchrotron radiation experimental station, a highly active glass sample derived from a hot industrial vitrification process of HAWC (Highly Active Waste Concentrate) generated during nuclear fuel reprocessing, a glass fragment sampled during hot operation of the Karl-sruhe vitrification plant VeK in 2009/10, was investigated at the INe-Beam-line in 2013. Direct determination of actinide and fission product speciation in a highly active nuclear material was shown to be feasible at ANKA.

A dedicated experimental setup developed for in-situ measurements at high temperatures (up to 2000 K) under air or a controlled reducing or oxidizing atmosphere was successfully tested by a research group around p. Martin and F. lebreton from CeA at Cadarache and Marcoule, France. to perform pilot experiments with u-bearing materials in 2013, the furnace chamber - acting as first sample containment - was placed into a sealed plexiglas box providing the necessary second containment. Both containments are equipped with Kapton windows permeable for incident, transmitted and fluorescence X-rays. A silica window on top of the assembly allows to mea-sure temperatures using a pyrometer.

A group around A. olson and S. Kozimor from los Alamos National lab, uSA, has exploited the low-e capabilities for measurements on radioactive samples at INe-Beamline in 2013 for systematic studies of covalency effects in actinide complexes from the point of view of phosphorous, sulfur and chlorine ligands.

Figure 3: (left) 3D CAD model and (right) photo of the MAC spectrometer during initial mechanical performance tests

Beamline publications 2013• “2,6-Bis(5,6-dipropyl-1,2,4-triazin-3-yl)-pyridine: Structures of An(III) and

ln(III) 1:3 complexes and selectivity“, N. l. Banik, M. A. Denecke, A. Geist, G. Modolo, p. J. panak, J. Rothe, Inorganic Chemistry Communications 29 (2013) 172–174

• “Characterization of u(VI)-phases in corroded cement products by mi-cro(μ)-spectroscopic methods”, J. Rothe, B. Brendebach, C. Bube, K. Dardenne, M. A. Denecke, B. Kienzler, V. Metz, t. prüßmann, K. Rick-ers-Appel, D. Schild, e. Soballa, t. Vitova, Journal of physics: Conference Series 430 (2013) 012114

• “Study of uranium oxidation states in geological material”, I. pidchenko, S. Salminen-paatero, J. Rothe, J. Suksi, Journal of environmental Radioac-tivity 124 (2013) 1-6

• “Structure and spectroscopy of hydrated neptunyl(VI) nitrate complexes”, p. lindqvist-Reis, Ch. Apostolidis, o. Walter, R. Marsac, N. l. Banik, M. Y. Skripkin, J. Rothe, A. Morgenstern, Dalton trans. 42 (2013) 15275 – 15279

• “exploring the solution behavior of f-element coordination compounds: a case study on some trivalent rare earth and plutonium complexes”, M. W. löble, p. oña-Burgos, I. Fernández, C. Apostolidis, A. Morgenstern, o. Walter, F. Bruchertseifer, p. Kaden, t. Vitova, J. Rothe, K. Dardenne, N. l. Banik, A. Geist, M. A. Denecke, F. Breher, Chem. Sci. 4 (2013) 3717-3724

• “Synthesis and characterization of thorium, uranium and cerium oxide nanoparticles”, N. Batuk, D. V. Szabó, M. A. Denecke, t. Vitova and S. N. Kalmykov, Radiochim. Acta 101 (2013) 233–239

• “lead uptake in diverse plant families: a study applying X-ray Absorption Near edge spectroscopy”, G. lisa Bovenkamp, A. prange, W. Schumach-er, A. Smith, K. Ham, and J. Hormes, environ. Sci. technol., (2013) DoI: 10.1021/es302408m

• “XANeS characterization of uo2/Mo(pd) thin films as models for ε-parti-cles in spent nuclear fuel”, M. A. Denecke, t. petersmann, R. Marsac, K. Dardenne, t. Vitova, t. prüßmann, M. Borchert, u. Bösenberg, G. Falken-berg and G. Wellenreuther”, Journal of physics: Conference Series 430 (2013) 012113

• “the incorporation of europium into apatite: a new explanation”, K. S. Holliday, K. Dardenne, C. Walther, t. Stumpf, Radiochim. Acta 101, 267-272 (2013)

• “preparation and Characterization of Fe-, Co-, and Ni-containing Mg-Al-layered Double Hydroxides”, H. Curtius, G. Kaiser, K. Rozov, A. Neumann, K. Dardenne, D. Bosbach, Clays and Clay minerals 61 (2013), 424-439

• “Coupling XRD, eXAFS, and C-13 NMR to Study the effect of the Carbon Stoichiometry on the local Structure of uC1 +/- x”, u. C. Nunez, l. Martel, D. prieur, e. l. Honorato, R. eloirdi, I. Farnan, t. Vitova, J. Somers, Inorg. Chem. 52 (2013), 11669-11676

• “Study of uranium oxidation states in geological material”, I. pidchenko , S. Salminen-paatero , J. Rothe , J. Suksi, Journal of environmental Radio-activity 124 (2013) 141-146

• “local and electronic Structure of Americium-Bearing puo2”, D. prieur, u. Carvajal-Nunez, t. Vitova, and J. Somers, eur. J. Inorg. Chem. 2013, 1518–1524

• “Accommodation of multivalent cations in fluorite-type solid solutions: Case of Am-bearing uo2”, D. prieur, p. Martin, F. lebreton, t. Delahaye, D. Banerjee, A. C. Scheinost, A. Jankowiak, J. Nucl. Mat. 434 (2013) 7–16

• “Comparative investigation of N donor ligand-lanthanide complexes from the metal and ligand point of view”, t. prüßmann, M. A. Denecke, A. Geist, J. Rothe, p. lindqvist-Reis, M. löble, F. Breher, D. R. Batchelor, C. Apostolidis, o. Walter, W. Caliebe, K. Kvashnina, K. Jorissen, J. J. Kas, J. J. Rehr, t. Vitova, J. phys: Confer. Ser. 430 (2013) 012115

• “Actinide and lanthanide speciation with high-energy resolution X-ray techniques”, t. Vitova, M. A. Denecke, J. Göttlicher, K. Jorissen, J. J. Kas, K. Kvashnina, t. prüßmann, J. J. Rehr and J. Rothe, Journal of physics: Conference Series 430 (2013) 012117

• “Actinide Colloids and particles of environmental Concern”, C. Walther and M. A. Denecke, Chem. Rev. 2013, 113, 995−1015

INE Beamline for Actinide and Radionuclide Science

the INe-Beamline at ANKA is dedicated to actinide and radionuclide re-search with emphasis on X-ray spectroscopy techniques. Radionuclides up to 106 times the european exemption limit and up to 200 mg of fissile iso-topes 235u and 239pu each can be handled at the beamline, applying a safe but flexible containment concept. the synchrotron based activities at the INe-Beamline are embedded in INe’s in-house research, thereby allowing a combination of analytical and instrumental methods, notably laser tech-niques and microscopic methods. Ancillary facilities for radioactive sample preparation are provided at INe controlled area laboratories.

overviewthe INe-Beamline at ANKA provides dedicated instrumentation for X-ray spectroscopic characterization of actinide samples and other radioactive materials. R&D work at the beamline focuses on various aspects of nuclear waste disposal within INe’s mission to provide the scientific basis for as-sessing long-term safety of a nuclear waste repository in a deep geological formation. the INe-Beamline is accessible for the actinide and radiochem-istry community through the ANKA pRC proposal system and the eu Fp7 large Infrastructure Initiative tAlISMAN. experiments with activities up to 106 times the european exemption limit are feasible within a flexible con-tainment concept. the close proximity of the INe-Beamline to INe’s con-trolled area labs offers infrastructure unique in europe for the spectroscopic and microscopic characterization of actinide samples. the modular beam-line design enables to adapt sample environments and detection schemes to various scientific questions. the well-established bulk XAFS techniques in transmission and total fluorescence yield detection mode (Fig. 1) have been augmented by more advanced methods using a micro-focused beam, including (confocal) XAFS / XRF detection (Fig. 2) and a combination of (µ-)XAS and (µ-)XRD. Additional instrumentation for high resolution X-ray emission (HRXeS) spectroscopy has been installed and successfully tested.

Research efforts at the INe-Beamline at ANKA are mainly driven by the Karl-sruhe based institutes KIt-INe and JRC-Itu, user groups from CeA (F), Man-chester university (GB), los Alamos National lab (uSA) and various national (Heidelberg, Mainz, Hannover) and international universities. Furthermore, the INe-Beamline serves as education and training center for young scien-tists, providing and maintaining nuclear competence.

Figure 1: Standard setup for XAFS measurements of bulk samples

AvailabilityIn 2013 a total of 32 in house and external projects were hosted at the INe-Beamline. the time available for INe internal research amounted to ~32% of all available shifts (38 days). Fifteen days were spent for maintenance, de-velopment and pilot experiments. As in the previous years, the majority of beamtime shifts in 2013 was given to external projects with (43 days) and without (9 days) pRC or tAlISMAN evaluation (i.e., through direct coopera-tion with KIt-INe). In 2013 external user groups from a total of 11 German and International research institutions (europe, uSA, Russia) visited ANKA to conduct experiments at the INe-Beamline. As in previous years, a significant percentage of in-house and pRC beamtime was used by Master and phD students to perform experiments in the framework of their theses (a total of 8 projects, corresponding to ~30% of all available shifts).the degree of over-booking – being on average at a factor of 3 during the past three calls – re-cently reached a factor of 6 at ANKA call 23 (April 2014 – September 2014).

Instrumentation and Special FeaturesEnergy range: 2.1 keV - 25 keV (p to pd K-edges, actinides up to the Cf l3-edge) Flux: ~2×1010 photons / sec at Zr K- / pu l3-edges using Ge(422) crystalsSource: 1.5 t bending magnet (eC = 6 keV)

Optics: lemonnier-type fixed exit DCM, exchangeable crystal pairs: Si(111), Si(311), Ge(422); Rh coated silicon mirrors (collimating 1st and focussing 2nd mirror) for a ~500 μm × 500 μm beam spot at sample position; addi-tional micro-focus options with poly-capillary half lenses (~25μm focus) for µ-XAS/XRF or single-bounce capillary (~35μm focus) for µ-XRD, SeSo X-ray beam position monitor

Sample positioning: various sample holders for radioactive or air sensitive samples; high precision HuBeR sample positioning system, goniometer cra-dles and auxiliary slits for both standard XAFS and surface sensitive grazing incidence techniques; pI hexapod for positioning of secondary focusing op-tics; pI heavy load hexapod for positioning of heavy sample environments

Class 3B sample pre-alignment diode laser

Detectors: ionization chambers for nominally high energies (transmission mode); ionization chambers for nominally low energies (oken ltd.); XRD-setup using image plates; 5 pixel leGe solid state fluorescence de-tector (Canberra); silicon drift detector (Vortex 60-eX); silicon drift detector (KeteK AXAS-M); digital fluorescence detector read-out (XIA-DXp)

experimental hutch operated as temporary controlled area with sepa-rate ventilation system; access control via personal lock; equipment for contamination monitoring; video surveillance of lock room and samples

Figure 2: (left) polycapillary setup for µ-XAFS/XRF measurements at the INE-Beamline – the Vortex silicon drift detector (SDD) is depicted with a secondary capillary mounted for confocal measurements (VLM: visible light microscope); (right) reconstructed 3D U distribution in contaminated sludge sample from a decantation basin at a former U reprocessing facility (scales in µm).

Spectroscopy Jörg Rothe: [email protected] prüßmann: [email protected]




Spectroscopy

Beamline Report

UV-CD12 Vacuum-uV circular dichroism spectroscopy beamlineuV-CD12 is a high-flux bending magnet beamline with an endstation for steady-state synchrotron radiation circular dichroism (SRCD) spectroscopy, which is predominantly used for structural biology work. It provides focused monochromatic circularly polarized light in the VuV to Near-uV spectral range. SRCD is a biophysical technique for (secondary and tertiary) structure analysis of proteins, nucleic acids, carbohydrates and other biomaterials as well as for small chiral organic molecules. uV-CD12 is owned and operated by KIt´s Institute of Biological Interfaces (IBG-2) as a CRG beamline.

overview• Availability: In 2013 the beamline provided 72 days of user operation

compared to the 107 days available in total from the machine. A bro-ken vacuum feedthrough at the grating motor of the monochromator chamber led to bad vacuum and downtime due to a labour-intensive repair. user operation had to be cancelled from June to August 2013 but beamtime for external users was fully compensated later from IBG-2´s internal contingent.

• Instruments: modular SRCD spectropolarimeter with toroidal grating• Methods: experimental endstation for steady-state measurements of liquid

samples (protein solutions) with peltier element temperature controller for thermal scans, experimental endstation for oriented circular dichroism (oCD) of solid samples (oriented peptide/lipid membranes)

Developments in 2013Recently, a second experimental station was installed at the beamline based on IBG-2´s long-term expertise in structural characterization of bio-mole-cules in anisotropic lipid environment. A newly developed modular sample chamber with a rotatable cell holder, a water thermostat and a tempera-ture/humidity sensor control system for automated oriented CD (oCD) has been built up (see Figure 1 A/B). oCD using synchrotron-radiation is a valu-able method for getting a global view on secondary structure, alignment and aggregation behaviour of folded peptides in oriented lipid membranes, i.e. hydrated lipid bilayers that are macroscopically oriented with respect to the light beam. the new experimental station allows for SR-oCD measure-ments of solid biological samples (mimics of cell membranes), which are difficult to measure in CD spectroscopy due to the possible occurrence of linear dichroism and birefringence artifacts. these have to be precluded by recording and averaging spectra at 8 different rotation angles around the beam axis. the new SR-oCD station is the only station worldwide with au-tomated data acquisition and provides improved spectral data quality and sensitivity especially for unsaturated and long-chain lipid environments at wavelengths < 200 nm compared to conventional oCD, which has been utilized at IBG-2 for nearly ten years. SR-oCD allows speeding up the screening of experimental conditions under which interesting and function-ally relevant changes in peptide structure and alignment occur. It allows elucidating structure / function relationships of , e.g.,antimicrobial peptides that lyse bacterial cell membranes (potential new antibiotics), cell-penetrat-ing peptides that may translocate cargo through cell membranes without destroying them, or hydrophobic membrane proteins that are involved in cell-signaling (which are studied at IBG-2 within the frame of KIt´s BioInt-erfaces program). Besides the importance of SR-oCD for in-house projects, there is also a clearly observable demand of external users for this tech-nique, which is reflected in the fact that 70% of the proposals submitted in 2013 were asking for access to this technique.

user Activities 2013• In 2013 10 proposals were granted beamtime via ANKA´s peer review

application procedure corresponding to 21 beamtime days (30% of available uo days). the overbooking in terms of days of beamtime applied for versus days available was 135%. By restricting the amount of beamtime assigned to some projects by the pRC it was possible to accommodate all projects. A 20% beamtime contingent in each Call is granted to u.K. users according to the contract with the Science & technology Facilities Council (StFC, Daresbury laboratory, u.K.). u.K. users had 22 beamtime days (20% of the theoretically possible 107 days) which corresponds to almost 30% of the uo days that were available at uV-CD12 last year (due to the repair of the vacuum leakage). 19 days were used for IBG-2 in-house research and 10 days were necessary for beamline maintenance and tests / optimization of the newly developed oCD endstation.

• the main activities on the beamline in 2013 have been concerned with life science applications and uV-CD12 has attracted external users both from Germany (Kaiserslautern, Marburg) as well as from international universities (u.K., Brazil, Finland, and turkey). Among these, petri Kursula and his group from DeSY Hamburg/university of oulu combine the “clas-sical” protein crystallography methods with SRCD and nicely demon-strate the gain in information content obtained with this approach. they received beamtime for conformational studies of myelin-related proteins (MBp, p2 and CNpase) or peptide fragments derived from these proteins. Myelin proteins interact intimately with the lipid bilayer and play crucial roles in the assembly, function, and stability of the myelin sheath which surrounds the axons of nerves and enables rapid transduction of axonal impulses. the SRCD results obtained reveal conformational changes of these proteins and peptides in membrane-mimicking environments and give novel insights into the mechanisms of membrane binding and stack-ing. three British user groups - among these high-ranking SRCD experts prof. B.A. Wallace and Dr. R. Janes from the university of london – were coming repeatedly to uV-CD12 for measurements of, e.g., voltage-gated sodium channels, the heart muscle protein α-tropomyosin or stathrins. the beamline has also attracted researchers from Brazil who study, e.g., the folding of antimicrobial peptides like plantaricin in different bacterial model membranes to understand the mechanism of action of this natural food preservative.

• IBG-2´s in-house research was mostly focusing on analyzing the second-ary structure and aggregation behavior of different membrane-active peptides (KIGAKI, Sb056, tp10, SAp) and their mutants in aqueous, mi-cellar or lipidic environments.

Figure 1: (A) Photograph of the experimental end-station for steady-state SRCD mea-surements and the new in-house built sample chamber with the lid opened. (B) Mod-ules for liquid-state SRCD with Peltier elements for thermostating / thermal scans and SR-OCD (solid samples) with a water-thermostated OCD cell mounted on a rotation stage; modules can be mounted alternately in the sample chamber.

Authors: Julio Cesar pissuti Damalio, Jose luiz lopes, patricia Kumagaiuniversity of Sao paulo, Sao Carlos Institute of physics, Sao Carlos, Sao paulo, Brazil

Beamline publications 2013

• J. l. S. lopes, D. orcia, A. p. u. Araujo, R. DeMarco, and B. A. Wallace, (2013), Folding Factors and partners for the Intrinsically Disordered pro-tein Micro-exon Gene 14 (MeG-14), Biophys. J. 104, 2512 – 2520.

• N. D´Avanzo, e. C. McCusker, A. M. powl, A. J. Miles, C. G. Nichols, B. A. Wallace, (2013), Differential lipid Dependence of the Function of Bacte-rial Sodium Channels, ploS oNe 8(4), e61216.

• M. Myllykoski, A. Raasakka, M. lehtimäki, H. Han, I. Kursula, and p. Kur-sula (2013), Crystallographic Analysis of the Reaction Cycle of 2´,3´-Cyclic Nucleotide 3´-phosphodiesterase, a unique Member of the 2H phosphoe-sterase Family, J. Mol. Biol. 425, 4307-4322.

• G. Muruganandam, J. Bürck, A.S. ulrich, I. Kursula, and p. Kursula (2013), lipid Membrane Association of Myelin proteins and peptide Segments studied by oriented and Synchrotron Radiation Circular Dichroism Spec-troscopy, J. phys. Chem. B 117, 14983 – 14993.

• p. Anand, Structure based design of protein linkers for Zinc finger Nucle-ases, phD thesis (INt), Karlsruher Institut für technologie, 2013.

• J. Bürck, “uV-CD12 @ ANKA: Beamline, experimental Facilities and Ap-plications”, Invited talk at u.K.-Brazil Workshop: enabling Novel and High-impact Studies with Synchrotron Radiation Circular Dichroism Spec-troscopy, Birkbeck College, university of london, 8-9 May 2013.

A B

SR-LCD

SR-OCD



Jochen Bürck: [email protected] Siegmar Roth: [email protected]

Bianca posselt: [email protected]


NANOHigh-resolution x-ray diffraction, surface and interface X-ray scattering investigation beamlinethe NANo beamline currently houses two experimental stations, NANo1 and NANo2. NANo1 is dedicated to in-situ high resolution X-ray diffrac-tion and surface scattering methods for the study of the growth and the processing of thin films multilayers and nanostructures. NANo2 is presently being used for the commissioning and the methodical development of hard X-ray full field transmission microscopy.

overviewX-ray diffraction probes the spatial arrangement of atoms in a crystal lattice. It is sensitive not only to chemical composition and lattice parameter, but also to the strain and the strain distribution, lattice defects, dislocations, the shape, the size and the distribution of surface nanostructures. With the advent of synchro-tron radiation the range of applications has been extended from bulk crystals to thin films and multilayers, epitaxial superlattices, nanostructures, nanocrystal-line materials and even to magnetic structures and multilayers.

High resolution X-ray diffraction methods While High Resolution Symmetric X-Ray Diffraction (HR-SXRD) is well suited to the out of plane determination of crystalline parameters and to the determina-tion of pure screw dislocation densities, [see eg. S. lazarev et al.,J. Appl. Cryst. 46 120-127 2013] High Resolution Asymmetric X-Ray Diffraction (HR-ASXRD) is applicable to the determination of composition and strain relaxation. It also enables us to separate the effects of tilt and correlation length.

Grazing incidence diffraction methods By using Grazing Incidence Diffraction GID with a crystal analyzer, we can ob-tain depth-resolved X-ray data, which demands a high flux. this allows the determination of in-plane crystalline parameters and additionally enables an accurate determination of pure edge dislocations.

Full field transmission microscopy and spectroscopic imagingA Carl Zeiss full field transmission X-ray Microscope (Carl-Zeiss-tXM) is operational at the second experimental station NANo2. the tXM has three operational modes: absorption contrast, phase contrast and scan-ning mode. the spectroscopic imaging is realized by combining full field transmission X-ray Microscopy (tXM) and X-ray Absorption Near edge Structure spectroscopy (XANeS) techniques to follow both the chemical phase transformation and the microstructural evolution of electrode ma-terials upon operation within an electrochemical cell.

Instrumentationthe instrumentation at NANo1 was specified to allow the in-situ characteriza-tion using synchrotron radiation. We aim for investigating changes in structural parameters such as lattice parameters, chemical composition, layer thickness, surface and interface roughness, inter-diffusion, crystal lattice quality/homo-geneity, strain distribution, nanostructure geometry (size/shape/correlations) during the growth process of individual monolayers as function of the temperature, the deposition time, the pressure and the flow rate of material. the second experimental station NANo2 is currently used for hard X-ray microscopy and spectroscopic imaging.

Special featuresthe optics of the beamline offer versatile choice of functionalities. three operation modes are available at the beamline: monochromatic, pink and white beam. the flux density at the sample can be increased at the expense of the angular resolution by using the beam with the mirrors vertically and horizontally to 80 µm V x 200 µm H. the heart of the first experimental station NANo1 is a heavy duty diffractometer with three different config-urations which has been coupled to a variety of environmental chambers

like Molecular Beam epitaxy (MBe) to study the growth of GaAs Nanowires, pulsed laser Deposition for performing time resolved diffraction and detecting the critical thickness for the domain formation in Ba0.5Sr0.5tio3 grown on Mgo.

Availability Although in 2013 the beamline was not open for general user operation initial realistic experiments could be performed together with in-house research staff and collaboration partners in connection with the commissioning of the hard X-ray full field microscope. In 2013, the in-situ plD was delivered and integrat-ed into the beamline and first time resolved X-ray diffraction experiment during the growth of Ba0.5Sr0.5tio3 on Mgo was successfully performed.

Developments 2013the main technical/scientific developments in 2013 were:• Integration of the In-situ pulsed laser Deposition growth at the station

NANo1 for time resolved experiment using high resolution X-ray diffrac-tion methods.

• Integration of the MBe chamber at the diffractometer for the In-situ study of the GaAs Nanowires growth.

• Implementation of 3D-Reciprocal Space Mapping methods with a 2D-de-tector as a rapid tool for investigating the influence of growth parame-ters on defects in semipolar GaN.

• establishment of the spectroscopic imaging methods at the microscope for the in-operando study of electrochemical processes in spinel cathode batteries.

Further developments in the near future will include: • Microfocus beam X-ray diffraction experiment using compound refrac-

tive lenses in collaboration of the institute of Microtechnology IMt at KIt.• establishment of fluorescence investigation of biological samples under

cryogenic conditions.

Figure 1: 1a right, 1a middle corresponds respectively to the design and to the picture of the electrochemical cell dedicated to the in-operando study. 1a left the Li-Battery operational with the electrical connection integrated into the TXM. Layout of acquisi-tion procedure using the mosaic stitching to record the 2D morphological images and to derive the XANES integrated curve for Mn (1b). 1c: schematic presentation of the hard X-ray full field transmission microscope at ANKA used to perform the spectro-scopic imaging measurement at constant magnification. [2]


Figure 2:Right row: 2D Morphology images and the 2D chemical phase mapping of Mn (Mn3+, Mn4+) determined for 5V, down the voltage capacity profile of LiNi0.5Mn1.4O4 spinel cathode.Middle row: 2D Morphology images and the 2D chemical phase mapping of the Man-ganese oxidation states (Mn4+, Mn3+) determined at 4.7 V, 3.5 V and 2.7 V indicating the increase in the Mn3+ content.Left row: Integrated bulk Ni-XANES measured over the field of view 40x32µm and the corresponding fitting using the least-squares linear combination of standard samples derived from the TXM-package [22] at 4.7 V, 3.5 V and 2.7 V. [2]

Figure 3:a) Picture of the In-Situ synchrotron PLD chamber combined into the multipurpose heavy duty diffractometer installed at the Nano beamline located at the synchrotron facility ANKA, Germany. The onset shows the plume forming after ablating the (BST, x=0.5) target during the In-Situ characterization.b) 3D model of the In-Situ PLD chamber incorporated into the diffractometer from the exit windows side of view showing specifically the available horizontal angular range of 55 degrees dedicated to the coplanar X-ray diffraction and the vertical angular range of 70 degrees devoted to the non-coplanar diffraction geometry.c) Picture from the open In-Situ PLD chamber showing the hexapod as a sample ma-nipulator used to align the sample with respect to the incident

Figure 4:a) Selected 2D-reciprocal space maps recorded during the PLD for deposition times of 0, 1, 7, 17 and 105 min.b) The diffraction intensity profiles derived from the 2D-RSMs along the crystal trun-cation rod CTR showing the substrate peak of MgO, (BST, x=0.5) peak 1 shifting con-tinuously by increasing the film thickness recorded during the In-Situ Synchrotron PLD investigation of the reflection 002. The CTR profiles are shifted vertically for better clarity.c) 2D- reciprocal space map RSM of asymmetric reflection 113 after the completion of the PLD growth at t=105 min showing two distinguishable peaks 1 and 2. [1]

Beamline publications 2013• [1] Sondes Bauer, Sergey lazarev, Alan Molinari, Andreas Breitenstein,

philipp leufke, Robert Kruk, Horst Hahn and tilo Baumbach, „the power of in situ pulsed laser deposition synchrotron characterization for the detection of domain formation during growth of Ba0.5Sr0.5tio3

on Mgo“ J. Synchrotron Rad. (2014). 21, 386.• [2] Sondes Bauer, lea De Biasi, Sven Glatthaar, leonel toukam, Holger

Gesswein, tilo Baumbach, “ In operando study of novel high volt-age spinel cathode material liNi0.5Mn1.5o4 using two dimensional full-field spectroscopic imaging of Ni and Mn within 40 nm resolution” in preparation.

• [3] Sondes Bauer, Sergey lazarev, Martin Bauer, tobias Meisch, Marian Caliebe, Vaclav Holy, Ferdinand Scholz, and tilo Baumbach, “3D reciprocal space mapping with a 2D-detector as a low latency tool for investigating the influence of growth parameters on defects in semipolar GaN to be submitted



Sondes Bauer: [email protected]


Beamline publications 2013 • C. Schenk, F. Henke, A. Schnepf, “[Ge12{FeCp(Co)2}8{FeCp(Co)}2]: A

Ge12 Core Resembles the Arrangement of the High-pressure Modifica-tion Germanium (II)”, Angewandte Chemie International edition 52 (6) 1834–1838 (2013)

• J. Majzlan, H. Schlicht, M. Wierzbicka-Wieczorek, G. Giester, H. pöll-mann, B. Brömme, S. Doyle, G. Buth, C. Bender Koch, “A contribution to the crystal chemistry of the voltaite group: solid solutions, Mössbauer and infrared spectra, and anomalous anisotropy“, Mineralogy and petrol-ogy 107 221-233 (2013)

• S. Saouane, G. Buth, F. p. A. Fabbiani, “Crystal structure and packing en-ergy calculations of (+)-6-aminopenicillanic acid”, Acta Crystallographica Section C: Crystal Structure Communications 69 1238-1242 (2013)

• D. Issenmann, N. Wehmeier, S. eon, H. Bracht, G. Buth, S. D. Ibrahimkut-ty, A. plech, “Determination of nanoscale heat conductivity by time-re-solved x-ray scattering”, thin Solid Films 541 28-31 (2013)

• G. Buth, e. Huttel, S. Mangold, R. Steininger, D. Batchelor, S. Doyle, R. Simon, “experimental test of Data Analysis Methods from Staggered pair X-ray Beam position Monitors at Bending Magnet Beamlines” Journal of physics: Conference Series 425 042004 (2013)

• A. M. Ako, B. Burger, Y. lan, V. Mereacre, R. Clérac, G. Buth, S. Go-mez-Coca, e. Ruiz, C. e. Anson, A. K. powell, “Magnetic Interactions Mediated by Diamagnetic Cations in [Mn18M](M = Sr2+,Y3+,Cd2+, and lu3+) Coordination Clusters Inorganic Chemistry” 52 5764-5774 (2013)

• G. Abbas, Y. lan, V. Mereacre, G. Buth, M. t. Sougrati, F. Grandjean, G. J. long, C. e. Anson, A. K. powell, “Synthesis, Magnetism, and 57Fe Möss-bauer Spectroscopic Study of a Family of [ln3Fe7] Coordination Clusters (ln = Gd, tb, and er)”, Inorganic Chemistry 52 11767-11777 (2013)

• t. Zarganes-tzitzikas, C. G. Neochoritis, J. Stephanidou-Stephanatou, C. A. tsoleridis, G. Buth, G. e. Kostakis, “Azodicarboxylates: valuable reagents for the multicomponent synthesis of novel 1,3,4-thiadiazoles and imidazo[2,1-b][1,3,4]thiadiazoles”, tetrahedron 69 (24) 5008–5015 (2013)

• S. lazarev, S. Bauer, K. Forghani, M. Barchuka, F. Scholz, t. Baumbach, “High resolution synchrotron X-ray studies of phase separation phenom-ena and the scaling law for the threading dislocation densities reduction in high quality AlGaN heterostructure”, Journal of Crystal Growth 370 51–56 (2013)

• S. lazarev, S. Bauer, t. Meisch, M. Bauer, I. tischer, M. Barchuk, K. thon-ke, V. Holy, F. Scholz, t. Baumbach, “three-dimensional reciprocal space mapping of diffuse scattering for the study of stacking faults in semipolar (1122) GaN layers grown from the sidewall of an r-patterned sapphire substrate”, Journal of Applied Crystallography 46 5 1425-1433 (2013)

• B. Krause, B. Miljevic, t. Aschenbrenner, e. piskorska-Hommel, C. tes-sarek, M. Barchuk, G. Buth, R. Donfeu tchana, S. Figge, J. Gutowski, D. Hänschke, J. Kalden, t. laurus, S. lazarev, R. Magalhaes-paniago, K. Se-bald, A. Wolska, D. Hommel, J. Falta, V. Holý, t. Baumbach, “Influence of a low-temperature capping on the crystalline structure and morphology of InGaN quantum dot structures Journal of Alloys and Compounds”, 585 572-579 (2014)

• F. p. A. Fabbiani, G. Buth, D. C. levendis, A. J. Cruz-Cabeza, “pharma-ceutical hydrates under ambient conditions from high-pressure seeds: a case study of GABA monohydrate”, Chemical Communications 50 1817-1819 (2014)

• S. Bergantin, M. Moret, G. Buth, F. p. A. Fabbiani, “pressure-Induced Conformational Change in organic Semiconductors: triggering a Revers-ible phase transition in Rubrene”, the Journal of physical Chemistry C 118 (25) 13476–13483 (2014)

SCDSingle Crystal Diffraction Beamlinethe ANKA-SCD beamline is an instrument for the structure determination of small or weakly diffracting crystals and for ex-situ characterization of surfaces and interfaces with X-ray scattering methods.

overviewAt the ANKA-SCD beamline the structure of complex, crystallized mole-cules can be revealed by means of Single Crystal X-ray Diffractometry. this technique yields the atomic coordinates within the unit cell of a single crystal. Due to the high incoming photon flux, ANKA-SCD is often used for the structure determination of small or weakly diffracting crystals. two single-crystal diffractometers are available for this purpose that can be used alternatively, one equipped with a large (Ø 340 mm) but comparatively slow image plate detector and one with a small but relatively fast CCD detector.In addition, diffraction studies on surfaces and interfaces, such as semicon-ductor interfaces, also nanostructured surfaces and interfaces, are feasible. A 6+2 - circle diffractometer that we received as a permanent loan from the lAS at KIt Campus South is available for this task. It features X-ray diffrac-tion methods such as Reciprocal Space Mapping, X-Ray Reflectometry and Grazing Incidence Diffraction.

Developments in 2013the 6 - circle diffractometer from the lAS has continuously been upgraded to serve its purposes in surface, interface and thin film characterization. the new 2 – circle analyzer with high-resolution crystal rotation stage and the motorized instrument base have been described in the previous report. A low-noise, high dynamic range single-photon-counting position sensitive detector (Mythen 1K) had already been added to the instrument before. In 2013 the developmental activities focused on the implementation of SAXS and GISAXS methods. A Roper Scientific / princeton QuadRo CCD detector that will be shared between the Fluo and SCD beamlines has been ob-tained from the NANo beamline as a permanent loan. the detector system comprises a 4K * 4K CCD chip and a 2.7:1 demagnifying fiber optics taper with a Ø 165 mm Beryllium entrance window. Accessories for this detector have been purchased and assembled on a dolly for easy transport between the beamlines. the accessories comprise a power supply for the detector electronics, an AC200-A10 (thermo electron leD GmbH) water thermostat for the peltier cooling, and a Nettop pC for the data readout via FireWire interface. unfortunately no proprietary 64bit drivers for the QuadRo CCD were available from princeton at the time of ordering, so the 64bit Nettop pC was set up with a 32bit operating system (openSuSe 12.3). the drivers for addressing the CCD are interfaced by tANGo. the spec macros on the control computer for the 6+2 – circle diffractometer have been extended, so that now the Mythen 1K pSD and the princeton CCD can be used in-terchangeably or in parallel. A manually adjustable beam stop was placed before the entrance window of the CCD detector and a 0.5 mm thick tan-talum foil was introduced into the attenuator box as an experimental beam shutter. As a preliminary setup the QuadRo CCD was mounted in a fixed frame made of “item™” aluminium profiles (see figure 1). A pilot user ex-periment was conducted in December 2013. the influence of antimicrobial peptides on the morphology of phospholipid bilayers was investigated with Grazing Incidence Small Angle Scattering (main proposer: Stefan Grage, IBG II). the samples were kept in a specially designed humid air environ-ment during the experiments. the results of the pilot experiment are de-scribed in a separate user report.the aim for the near future is to provide a variable sample to detector dis-tance for SAXS and GISAXS studies, to be able to match the instrumental resolution to the structural properties of the samples. the space behind the 6+2 – circle diffractometer is occupied by the table carrying the Bruker and Stoe diffractometers for single crystal structure determination at present. the table has now been equipped with wheels allowing to move it to the side by approximately 300 mm, vacating space for flight tubes and the

QuadRo CCD detector hanging down from a rail. Motorized horizontal and vertical displacements by one detector window radius will be provided.

user Activities in 2013 Apart from the already mentioned GISAXS study on the influence of an-timicrobial peptides on the morphology of phospholipid bilayers, pRC re-viewed beamtime at ANKA-SCD was dedicated to the determination of structures from a variety of systems, such as large paramagnetic aggregates of transition-metal and lanthanide cations, novel binary tin subhalides and metalloid tin cluster compounds, oligonuclear spin transition complexes, semiconduclor cluster molecules, novel catalysts, and displacive and or-der-disorder phase transitions of pb-lawsonite. layer and interface quality of multilayered films for thermoelectric materials have been assessed with X-ray reflectivity and high-resolution diffraction.A significant amount of in-house beamtime went into studies of AlGaN epilayers grown on Sapphire with coplanar and non-coplanar diffraction and of InGaAs/GaAs quantum dots grown on a patterned substrate. Fur-thermore the structures of Rare earth and Re silicide films and nanoislands on Si substrates have been studied with X-ray diffraction and reflectometry.

Figre 1: Test setup for SAXS / GISAXS at the 6+2 - circle diffractometer

Gernoth Buth: [email protected]





PDIFFX-ray powder diffraction beamlinethe pDIFF beamline is dedicated to diffraction experiments on bulk poly-crystalline materials under in-situ conditions and for high-resolution powder diffraction, residual stress and texture measurements. In certain cases it is also suited to scattering studies on thin-films and epitaxial layers.

overviewthere are two diffractometer setups available at the beamline. the origi-nal 4-circle Kappa-diffractometer is now mainly used for texture, crystallize size analyses and stress measurements (sin2ψ method) on either using the analyser or the Soller collimator (0-dimensional detectors with point-for-point scanning), or in special cases with the CCD detector. the heavy-duty 3-circle diffractometer is normally equipped with both the CCD detector and the INel 90° line detector. this instrument is almost exclusively used for in-situ time-resolved experiments. usage of the two setups is divided approximately 50:50.

of the 107 days of operation supplied by the machine in 2013 the beamline was available for users a total of 81 days, with 68 days being allocated to external (pRC-reviewed) proposals and 13 days to in-house research. the remaining 26 days are accounted for by machine failure, beamline reconfig-uration for users, beamline maintenance and reduced staff support. In total 21 projects received beamtime – 18 of these via the pRC-review process and three in-house projects. of the 18 peer-reviewed proposals nine of these came from KIt institutes (north & south campuses) and nine from external institutes.

Developments in 2013the major effort in 2012-2013 has been to improve the facilities for in-situ experiments being done on the large (heavy-duty) powder diffractometer. this has centered on three main aspects:

• installation of an XYZ-stage for the positioning of various sample chambers (both from ANKA and from external users)

• installation of a motorized linear stage for the princeton CCD detector• development of spec macros for automated in-situ measurements (sample

changing, beam monitoring, detector control, temperature control).

Major improvements in the tANGo-driver for the princeton CCD camera have meant that this detector is really now in a useable state. Many groups are now using this detector exclusively for their experiments (with a time resolution of around 1-2 seconds).

Figure 1: Figure 1: The new motorized linear stage for the CCD camera (upper left) on the heavy-duty diffractometer. The distance between CCD and sample is adjust-able between approx. 100mm and 900mm.

on the small diffractometer a compact XYZ-stage has been installed (which due to the space limitations was always a problem). An additional high-resolution Soller-collimator is also now available: this gives a factor 10-20 increase in intensity compared to the high-resolution crystal analyzer, with about a factor of 5 decrease in angular resolution.

Figure 2: New sample holders for small samples and pellets

Additionally a motorized beam-stop for the CCD camera, with an integrated pIN-diode for measurement of the direct beam intensity, has been installed.

user ActivitiesA significant fraction of the beamtime in 2013 was dedicated to in-situ materials investigations. Groups from KIt-IAM, KIt-INt and the university of Kiel are involved in the characterization of battery materials - both chem-ical-structural, phase, and microstructural aspects during charge/discharge cycling and aging. In-situ tensile deformation studies of metallic alloys - both in thin film form and as bulk (wire) materials have been performed by groups from KIt-IAM and the MpI-eisenforschung, and first experiments on catalytic materials have been made by Grunwaldt et al. (KIt-ICtpC). In addition, first proof-of-principle in-situ experiments using high-power la-ser radiation for surface modification of steels (Gibmeier, KIt-IAM) were performed at the beamline with sub-second time resolution using a cus-tom-built chamber.

Figure 3: Setup for high-power laser experiments on PDIFF. The vacuum chamber is shown without its lid. Four Mythen modules in the backscattering region record the diffraction signal (only 2 can be seen in the photo).

High-resolution measurements (using the crystal analyzer) have included structural analysis of phase transformations in pyrrhotites as well as the investigation of laue crystal lenses for high-energy X-ray focusing.

Beamline publications 2013• p. J. Bereciartua, F. J. Zuñiga, J. M. perez-Mato, V. petříček, e. Vila, A. Cas-

tro, J. Rodríguez-Carvajal, S. Doyle: Superspace Description of the System Bi2(n+2)Mon o6(n+1) (n=3, 4, 5 and 6), Aperiodic Crystals (2013) pp 149-155

• l. Hartmann, D. Djurado,I. Florea, J-F. legrand, A. Fiore, p. Reiss, S. Doyle, A. Vorobiev, S. pouget,F. Chandezon, o. ersen, and M. Brinkmann: large-Scale Simultaneous orientation of CdSe Nanorods and Regioregu-lar poly(3-hexylthiophene) by Mechanical Rubbing, Macromolecules 46, (2013) 6177.

• B. Krause, S. Darma, M. Kaufholz, S. Mangold, S. Doyle, S. ulrich, H. leiste, M. Stüber t. Baumbach: Composition-dependent structure of polycrystalline magnetron-sputtered V–Al–C–N hard coatings studied by XRD, XpS, XANeS and eXAFS, J. Appl. Cryst. (2013). 46, 1064–1075.

• M. Schroeder, S. Glatthaar, H. Geßwein, V. Winkler, M. Bruns, t. Scherer, V. Sai Kiran Chakravadhanula, J. R. Binder: post-doping via spray-drying: a novel sol–gel process for the batch synthesis of doped liNi0.5Mn1.5o4

spinel material, J Mater Sci (2013) 48:3404–3414. • K.C. Sekhar, S. levichev, Koppole Kamakshi, S. Doyle, A. Chahboun,

M.J.M. Gomes: effect of rapid thermal annealing on texture and proper-ties of pulsed laser deposited zinc oxide thin films, Materials letters 98 (2013) 149–152.

• pavel Seredin, Vladimir Kashkarov, Anatoliy lukin, Yury Ippolitov, Robert Julian and Stephen Doyle: local study of fissure caries by Fourier trans-form infrared microscopy and X-ray diffraction using synchrotron radia-tion, J. Synchr. Rad., 20 (2013) 705–710,

• Weisenburger, A. Jianu, S. Doyle, M. Bruns, R. Fetzer, A. Heinzel, M. Del-Giacco, W. An, G. Müller :oxide scales formed on Fe–Cr–Al-based model alloys exposed to oxygen containing molten lead, Journal of Nuclear Ma-terials 437 (2013) 282–292.



Scattering and Imaging Stephen Doyle: [email protected]


MPIMultipurpose high-throughput XAS beamline

the MpI Beamline is a beamline for the in-situ investigation of structural and magnetic properties of nano-scaled systems, e.g. surfaces, interfaces, nanoparticles, thin films and multilayers, under industrially and environ-mentally relevant conditions such as high temperature/gas pressures, ex-ternal mechanical forces, aggressive gas atmospheres or strong electric or magnetic fields.

overviewthe available X-ray technologies are X-ray diffraction and reflectivity, crystal truncation rod scattering, grazing incidence diffraction, and (thin film) pow-der diffraction. It is owned and operated by a consortium of Max-planck-In-stitutes.

Developments 2013In 2013 we performed first in-situ GISAXS experiments on euSi2 nano-islands.

A future significant upgrade of the beamline is planned. this will ensure reliable operation by changing all motor power supplies and controllers to ANKA’s standard Middex controllers as well as installing the standard ANKA Beam line safety system pVSS. In 2014, the detector arm will be modified to eliminate possible collisions and a 12 foil absorber changer will replace the 4 foil one. Also in 2014, a new small closed cycle refrigerator for the small Huber eulerian cradle will provide cooling down to 10K.

user Activities 2013the users’ experiments done were from the following core areas:

• Structure of rare earth transition-metal oxide single crystals, thin films and multilayers

• Structure of cobalt- and ironoxides as well as Heusler alloys• In-plane structure of bi-layer Graphen• Ex-situ studies of semiconductor nanostructures• oxidation of metallic alloys• In-situ growth of metallic alloy films• In-situ stress measurements and fault structures in metallic alloy thin films• In-situ reactive changes of the surface structure and morphology of

intermetallic phases

Beamline publications 2013

• A. Frano, e. Benckiser, Y. lu, M. Wu, M Castro-Colin, M. Reehuis, A. V. Boris, e. Detemple, W Sigle, p. v. Aken, G Cristiani, G.logvenov, H.-u. Habermeier, p. Wochner, B. Keimer, V. Hinkov: “layer Selective Control of the lattice Structure in oxide Superlattices, Advanced Materials” (2013), dx.doi.org/10.1002/adma.201303483.

• u. Hejral, A. Vlad, p. Nolte, and A. Stierle: “In Situ oxidation Study of pt Nanoparticles on Mgo(001)”, J. phys. Chem. C (2013) dx.doi.org/10.1021/jp404698k. [MpI]

• M.K.A. Koker, J. Schaab,N.Zotov, e.J. Mittemeijer: “X-ray diffraction study of the reverse

• martensitic transformation in Niti shape memory thin films”, thin Solid Films 545 (2013) 71–80. [MpI]

• S. J. B. Kurz, C. ensslen, u. Welzel, A. leineweber and e. J. Mittemeijer: “the thermal stability of Ni–Mo and Ni–W thin films: Solute segregation and planar faults”, Scripta Mater. 69 (2013) 65–68. [MpI]

• V. Vonk, N. Khorshidi, A. Stierle, H. Dosch: “Atomic structure and com-position of the yttriastabilized zirconia (111) surface”, Surface Science 612 (2013) 69–76. [MpI]

• D. Franz, S. Runte, C. Busse, S. Schumacher, t. Gerber, t. Michely, M. Mantilla, V. Kilic, J. Zegenhagen, A. Stierle: Atomic Structure and Crys-talline order of Graphene-Supported Ir Nanoparticle lattices, phys. Rev. lett. 110 (2013) 065503

• J. lohmiller, A. Kobler, R. Spolenak, p. A. Gruber: the effect of solute segregation on strain localization in nanocrystalline thin films: Dislocation glide vs. grain-boundary mediated plasticity, Appl. phys. lett. 102 (2013) 241916

• A. pareek, G. N. Ankah, S. Cherevko, p. ebbinghaus, K. J. J. Mayrhofer, A. erbe, F. u. Renner: effect of thiol self-assembled monolayers and plasma polymer films on dealloying of Cu–Au alloys, RSC Advances 3 (2013) 6586-6595

peter Wochner: [email protected]




FLUOX-ray fluorescence spectroscopy beamlinethe Fluo beamline is situated at a bending magnet port. It is equipped with a double multilayer monochromator, providing high photon flux at moderate energy resolution, and is predominantly used for X-ray fluorescence measurements and mappings with spatial resolution in the micrometer range. With Confocal X-ray Fluorescence and X-ray Fluorescence tomog-raphy, depth-resolved measurements are possible, allowing access to three-dimensional mappings of major, minor, and trace elements in a sample.

overviewIn 2013 the beamline provided 59 days of peer reviewed user operation. even though the machine failure rate in 2013 was high, with 26 days which were partially or totally lost, the impact on peer reviewed user time could be restricted to 5 days. three experimental projects used the princeton QuadRo powder diffraction camera which is in shared use with SCD beamline.

Developments 2013the main siginificant developments at the beamline in 2013 were:• the digital signal processor for the energy dispersive detector was re-

placed by the faster XIA-Mercury system which provides besides higher resolution and improved throughput the possibility of breakless recording of spectra which is important for scanning in continuous motion.

• the sample positioner was exchanged by a more robustly designed set-up equipped with linear motors for fast and vibration free operation. (Newport ) A sophisticated motor controller (Newport XpS) allows for continuous scanning and mapping on efficient trajectories by providing suitable triggering modes.

A total of 15 beamtime days was used in 2013 for commissioning the new equipment.

Currently large solid angle geometries are being tested in order to speed up data acquisition by reducing pixel dwell time..

user Activities 2013In 2013 the Fluo beamline was used for 13 projects consisting of 59 days of external (57) and internal (2) user operation and 12 days of in-house research. the main areas of user experiments were biology and medicine, nuclear energy related environmental research, mineral resources and archeometry. the beamline is also used for the characterization of X-ray optics for beam focusing and imaging, also including set-ups for X-ray microscopy.

Beamline publications 2013 • Al-ebraheem, A., Geraki, K., leek, R., Harris, A. l., & Farquharson, M. J.

(2013). the use of bio-metal concentrations correlated with clinical prog-nostic factors to assess human breast tissues. X-Ray Spectrometry, 42(4), 330–336. doi:10.1002/xrs.2463

• Nazmov, V., Mohr, J., & Simon, R. (2013). Mosaic-like micropillar array for hard x-ray focusing—one-dimensional version. Journal of Micro-mechanics and Microengineering, 23(9), 095015. doi:10.1088/0960-1317/23/9/095015

• pemmer, B., Roschger, A., Wastl, A., Hofstaetter, J. G., Wobrauschek, p., Simon, R., … Streli, C. (2013). Spatial distribution of the trace elements zinc, strontium and lead in human bone tissue. Bone, 57(1), 184–93. doi:10.1016/j.bone.2013.07.038

• Reiche, I., Müller, K., Albéric, M., Scharf, o., Wähning, A., Bjeoumik-hov, A., … Simon, R. (2013). Discovering vanished paints and natural-ly formed gold nanoparticles on 2800 years old phoenician ivories us-ing SR-FF-microXRF with the color X-ray camera. Analytical Chemistry, 85(12), 5857–66. doi:10.1021/ac4006167

• Roschger, A., Hofstaetter, J. G., pemmer, B., Zoeger, N., Wobrauschek, p., Falkenberg, G., … Streli, C. (2013). Differential accumulation of lead and zinc in double-tidemarks of articular cartilage. osteoarthritis and Cartilage / oARS, osteoarthritis Research Society. doi:10.1016/j.joca.2013.06.029



Rolf Simon: [email protected]


Figure 1: New Grating Interferometry Setup

Figure 2: Results from high throughput X-ray tomography; a: Beetle forewing that served as template for a research pavilion at the University of Stuttgart; b: polygon mesh of a fossil braconid wasp of an undescribed genus from Baltic amber; c: Seg-mented mesh of a fossil clown beetle (Onthophilus intermedius) from fissure filling; d: rendering of the scull of a common newt (Lissotriton vulgaris).

Beamline publications 2013 • P. Vrśanský, T. van de Kamp, D. Azar, A. Prokin, L. Vidlička, P. Vagovič, “Cock-

roaches probably Cleaned up after Dinosaurs”, ploS oNe 8, e80560, 2013

• t. van de Kamp, A. ershov, t. dos Santos Rolo, A. Riedel, t.Baumbach, „Insect Imaging at the ANKA Synchrotron Radiation Facility”, entomolo-gie heute 25, 147-160, 2013

• p. Vagovic, D. Korytár, A. Cecilia, e. Hamann, l. Švéda, D. pelliccia, J. Härtwig, Z. Zápražný, p. oberta, I. Dolbnya, K. Shawney, u. Fleschig, M. Fiederle, t. Baumbach, “High-resolution high-efficiency X-ray imaging system based on the in-line Bragg magnifier and the Medipix detector”, J. Synchrotron Rad. 20, 153-159, 2013

• B. K. tanner, J. Wittge, p. Vagovic, t. Baumbach, D. Allen, p. J. McNally, R. Bytheway, D. Jacques, M. C. Fossati, D. K. Bowen, J. Garagorri, M. R. elizalde, A. N. Danilewsky, “X-ray diffraction imaging for predictive metrology of crack propagation in 450-mm diameter silicon wafers”, powder Diffraction 28, 95-99, 2013

• t. Koenig, e. Hamann, S. procz, R. Ballabriga, A. Cecilia, M. Zuber, X. llopart, M. Campbell, A. Fauler, t. Baumbach, M. Fiederle, “Charge Sum-ming in Spectroscopic X-Ray Detectors with High-Z Sensors”, Ieee trans-actions on Nuclear Science 60, 4713-4718, 2013

• e. Hamann, A. Cecilia, A. Zwerger, A. Fauler, o. tolbanov, A. tyazhev, G. Shelkov, H. Graafsma, t. Baumbach, M. Fiederle, “Characterization of photon counting pixel detectors based on semi-insulating GaAs sensor material”, J. phys.: Conf. Ser. 425, 062015, 2013

• A. Danilewsky, J. Wittge, K. Kiefl, D. Allen, p. McNally, J. Garagorri, M. R. elizalde, t. Baumbach, B. K. tanner, „Crack propagation and fracture in silicon wafers under thermal stress”, J. Appl. Cryst. 46, 849-855, 2013

TOPO-TOMOthe topo-toMo beamline is devoted to conventional X-ray topography and micro-imaging both in 2D (radiography) and 3D (tomography). Digital white-beam topography in projection and section topography mode as well as digital white and pink (10-2 energy resolution) beam radiography and microtomography in absorption and phase contrast are available.

overview Available methodsWhite beam X-ray topography: Detailed information on defect distribu-tions in crystals can be provided by synchrotron X-ray topography in which an intense, highly collimated beam of X-rays is directed onto a crystalline sample in laue or Bragg configuration. this non-destructive analysis tech-nique is mainly used for the study of dislocations, planar defects, stacking faults, growth defects or large precipitates. Also very small local defects like nm-scale voids in Si can be imaged as well as long range strain in electronic devices.

High resolution synchrotron radiography and micro-tomography: High-resolution and phase contrast radiography are used to investigate micro-structured, multi-component material systems, e.g. to detect de-laminations between substrates and glob tops encapsulating wire-bonded devices. Radiographs taken from different projection angles allow obtain-ing three-dimensional information with a spatial resolution down to the sub-micrometer range by means of computed microtomography. the sub-sequent application of 3D image analysis methods can be used for the de-termination of size distributions, orientations or spatial correlations within the tomographic, multi-constituent volume images.

Phase-contrast imaging with a grating interferometer: phase-contrast imaging with a grating interferometer provides determination of the refrac-tive index distribution within a sample even for materials with similar refrac-tive indices. the topo-toMo white beam station enables high phase sen-sitivity and spatial resolution of about 5 μm together with a short exposure time below 1 s. By combining a grating interferometer with computed to-mography the refractive index distribution can be acquired in a 3D volume.

Instrumentationthe topo-toMo beamline is equipped with highly specialized compo-nents, like optical tables, linear and rotary stages, slit systems, a double multilayer monochromator, detector systems and cameras. Detector optics are available both for white and monochromatic beam, ranging from a total magnification of 1x to 50x. Depending on the experimental requirements, the detector can be chosen for high sensitivity (0.7 FpS, 5000 gray levels, 9 µm pixel size) or high speed (5400 FpS, 700 gray levels, 20 µm pixel size).

Special featurestopo-toMo is currently able to perform the fastest tomography in the world. tomograms of dynamic processes can be acquired within 30 millisec-onds with reduced quality and moderate spatial resolution of about 10 µm and tomograms of static conditions take only 130 milliseconds with highest quality and spatial resolution of 2.5 µm.

Availability In 2013 the topo-toMo beamline provided 86 of 107 available days for user operation, which included in-house, external and commercial projects. Additional 16 days haven been used for commissioning and testing of beamline components.Currently only topography beamtime can be offered to external user groups. For tomography experiments, the beamline has got the function as a pre-development station for the new IMAGe-beamline and also serves as an educational beamline as new techniques are being developed within phD-works as inhouse-studies. As there is not yet a routine setup, tomography service cannot be offered to external user groups and tomography measurements can only be done within inhouse-research.

Developments 2013

upgrade of the Grating Interferometry Setup. this setup is a motorized system with opportunities for automation in order to facilitate the usage and to deliver a higher degree of precision (Figure 1). the design is flexible and allows a higher throughput for quality control of the X-ray gratings.

the mechanics of the first slits have been upgraded in order to provide higher precision.

the camera pool has been extended by a new Andor Neo camera, a 5.5 megapixel CMoS camera, providing global and rolling shutter, minimized dark current (vacuum cooled down to -40 °C) and 100 fps full frame in burst mode.

As already started in 2012, the main focus has been put on the reliability of the beamline. existing bugs, mechanical or It-related, have been fixed and tested and spare parts of crucial components have been bought in order to guarantee an operational beamline.

Future upgradesA dedicated small animal scanner for high throughput X-ray micro-tomog-raphy is planned to be installed at the beamline.A source grating is planned to be implemented at the beamline in order to provide better coherence conditions.

user Activities 2013the main activities on the beamline in 2013 have been concerned with life science,material science, nano and micro technologies, quality assurance of optics and detectors (e.g. optics fabricated by KIt-IMt at ANKA-lIGA beamline) and development of X-ray imaging methods.

user experiments (examples):• Quality assurance measurements of X-ray imaging optics, which are de-

velopments of the Institute of Microstructure technology (IMt) at KIt, have been performed. examples for such optics are rolled-type X-ray lenses or X-ray prismatic lenses, which are fabricated by deep X-ray li-thography (at ANKA).

• White beam high throughput tomography of biological samples has been optimized. Research projects included the investigation of changes in the morphology of skull and teeth of newts during metamorphosis, the description of fossil arthropods, examination of pollen distribution on bees and the lightweight architecture of beetle forewings (Figure 2). the latter resulted in the construction of a research pavilion at the university of Stuttgart.

• Dislocations in GaAs by X-Ray diffraction imaging have been studied in-situ by X-ray diffraction imaging. A number of GaAs wafers with well defined artificial defects from indentation have been characterized by in-frared and interference contrast microscopy before and after heat treat-ment. During the heating the dynamics of the dislocations have been ob-served in-situ by X-ray diffraction imaging with a digital indirect detector system at 5 frames per second.

• Investigation of strain-induced structural changes in Si single crystals ex-ploiting the three-dimensional resolution of a pnCCD. the pnCCD as an energy-dispersive detector allows a simultaneous measurement of the positions and energies of laue spots

thorsten Müller: [email protected]





Hard X-ray Microscopy and Quality Assurance X-ray optical compo-nents: the MiQA experimental station, dedicated to hard X-ray Microscopy and Quality Assurance of X-ray optical components, is designed to operate in a wide X-ray energy range of 10 keV to 60 keV implementing comple-mentary imaging contrasts with a resolution range from 500 μm down to 40 nm.

Instrumentation

the beamline is being stepwise commisioned since 2013 with a temporary white beam station placed in the optical hutch (Figure 3) at a distance of 25 m from the source. the station is equipped with highly specialized components, linear and rotary stages, slit systems, detector systems and cameras. Detector optics is available for white beam experiment, ranging from a total magnification of 1x to 3x.

Availability

the temporary white beam station installed at the IMAGe/XMIC beamline has the function of a pre-development station for the final stations that will be installed at the beamline. In addition, the station is used to test techniques that are being developed in the framework of in-house activities.

Developments 2013• Installation and test of the white beam station placed in the optical hutch

at 25 m from the source.• Starting of operation.

Figure 3: White beam temporary station at the Image beamline. The radiation beam shutter is located on the right side of the image. The experimental station is positioned on the left side, after a 12 m long vacuum tube.




IMAGE/XMIC

the IMAGe/XMIC beamline is being constructed in the western straight-sec-tion of the ANKA storage ring. three experimental stations will be estab-lished at the beamline for fulfilling different imaging methods. Station 1 is a full-field transmission X-ray microscope for hard X-rays, locat-ed in the first experimental hutch. Station 2 for fast white-beam computed tomography/laminography, in-cludes coherent imaging by in-line holography, grating interferometry, and 3D micro-diffraction imaging methods. It will be located in the second ex-perimental hutch. Station 3, located in the second experimental hutch, will be a hard X-ray microscope dedicated to non-destructive testing based on different types of deep X-ray lithographical lenses, with an optical resolution down to 20 nm.

overview Available methodsHard X-ray microscopy: the hard X-ray microscopy setup, dedicated to the study of biological samples, will be placed in the experimental Station 1 of the beamline (Figure 1). Currently the microscope is installed and oper-ational at the NANo beamline (Figure 2). the full-field transmission micro-scope is specified for an energy range from 2 keV to 12 keV, based on cap-illary condensers and high resolution zone plates with a spatial resolution of 30 nm. 2D radiography and 3D tomography are possible in absorption contrast as well as Zernike phase contrast. An X-ray fluorescence detector adds the possibility of mapping elemental compositions within the sample. the high penetration depth of hard X-rays allows for imaging of samples up to several tens of µm thickness. the microscope is equipped with a cryogen-ic sample environment for vitrified samples in order to enable imaging of bi-ological samples as close to their natural state as possible. Furthermore, the cryogenic sample environment contributes to minimizing radiation damage. First experiments have been successfully conducted.

Figure 1: Schematic drawing of the IMAGE beamline and the northwest hall exten-sion. The first experimental hutch will host the full-field transmission X-ray microscopy station. The second experimental hutch will host a multi-purpose imaging station for fast tomography, laminography and diffraction imaging, and a hard X-ray microscope dedicated for non-destructive testing based on different types of deep X-ray litho-graphical lenses.

Figure 2: (upper) 3D-illustration of the main functional components of the hard X-ray microscope, and (lower) the microscope installed on the NANO beamline

High resolution synchrotron radiography and micro-tomography: the experimental station dedicated to high resolution synchrotron radiog-raphy and microtomography, so called uFo-CoDe, will cover a variety of scan geometries, contrast mechanisms, and a wide range of temporal reso-lutions in a single setup for highest flexibility, enabling the full potential of the beamline to be exploited. Besides radiography, both tomographic and laminographic scan geometries will be used for 3D imaging, each with the possibility to be operated with various contrast modalities. using white-beam and combined with a flexible transmission detector system optimized for high frame rates these methods will aim for high speed applications, e.g. tomographic imaging in the sub-second regime. High sample through-put will be enabled by an automatic sample exchange system. Monochro-matized X-rays delivered by either the DMM or the DCM will allow for high contrast and high resolution down to the sub-micron range. In addition to absorption contrast, propagation based phase contrast and grating inter-ferometry will give access to complementary sample properties. In addition to transmission based methods, the uFo-CoDe station will implement an operation mode dedicated for diffraction imaging experiments like rocking curve imaging or diffraction tomography. this will be supported by a ded-icated detector system providing flexible detector positioning in the whole hemisphere above the sample, allowing diffracted X-rays far off the primary beam direction to be detected.

Sondes Bauer: [email protected]


Beamline publications 2013• Jensen, t. H.; Bech, M.; Binderup, t.; Böttiger, A.; David, C., Weitkamp,

t., Zanette, I.; Reznikova, e.; Mohr, J.; Rank, F.; Feidenhans’l, R.; Kjaer, A.; Hojgaard, l.; pfeiffer, F.; Imaging of Metastatic lymph Nodes by X-ray phase-Contrast Microtomography; public library of Science oNe, 8(1):e54047 (2013) DoI: 10.1371/journal.pone.0054047

• Rutishauser, S.; Bednarzik, M.; Zanette, I.; Weitkamp, t.; Börner, M.; Mohr, J.; David, C.; Fabrication of two-dimensional hard X-ray diffraction gratings; Microelectronic engineering, 101 (2013), pp 12-16

• DoI:10.1016/j.mee.2012.08.025• ogurreck, M.; Wilde, F.; Herzen, J.; Beckmann, F.; Nazmov, V.; Mohr, J.;

Haibel, A.; Müller, M., Schreyer, A.; the nanotomography endstation at the petRA III Imaging Beamline; Journal of physics: Conference Series 425, 18 (2013) DoI:10.1088/1742-6596/425/18/182002

• Greiner, F.; Quednau, S.; Dassinger, F.; Sarwar, R., Schlaak, H. F.; Guttmann, M.; Meyer, p.; Fabrication techniques for multisacale 3D-MeMS with ver-tical metal micro- and nanowire integration; Journal of Micromechanics and Microengineering 23 (2013), 025018 (12pp) DoI:10.1088/0960-1317/23/2/025018

• Willner, M.; Bech, M.; Herzen, J.; Zanette, I.; Hahn, D.; Kenntner, J.; Mohr, J.; Rack, A.; Weitkamp, t.; pfeiffer, F.; Quantitative phase-contrast computed tomography at 82 keV; optics express 21, 4 (2013), pp. 4155-4166 DoI: 10.1364/oe.21.004155

• Fu, J.; Willner, M.; Chen, l.; tan, R.; Achterhold, K.; Bech, M.; Herzen, J.; Mohr, J.; Schulz, J.; pfeiffer, F.; Helical Differential X-ray phase-Contrast Computed tomography; pRl

• Börner, M.; Fornasier, H.; Hübner, B.; Karbacher, A.; Matthis, B.; Meyer, p.; Mohr, J.; Münch, D.; Straus, C.; Wolf, J.; the potential of Modem X-ray Resists for High Aspect Ratio Microstructure Fabrication - A Comparison; Springer Journal “Microsystem technologies”, sowie als poster auf dem HARMNSt Workshop 2013, Berlin 21.04. - 24.04.2013

• thüring, t.; Hämmerle, S.; Weiss, S.; Nüesch, J.; Meiser, J.; Mohr, J.; David, C.; Stampanoni, M.; Compact hard X-ray grating interferom-etry for table top phase contrast micro Ct; proc. SpIe 8668, Medical Imaging 2013: physics of Medical Imaging, 866813 (March 6, 2013) DoI:10.1117/12.2006865

• Jark, W.; last, A.; Concept for rapid tuning and switching of X-ray ener-gies; SpIe Conference 8778, eooo111, Advances inX-ray Free-electron lassers II: Instrumentation

• Ruiz, M.; Zanette, I.; Rack, A.; Chabior, M.; Scherer, K.; Mohr, J.; Meyer, p.; Weitkampf, t.; pfeiffer, F.; X-ray gratingbased phase-contrast imaging at 126 keV; 22nd International Congress on X-Ray optics and Microanal-ysis, Hamburg 2-6 September 2013

• Nazmov, V.; Kluge, M.; last, A.; Marschall, F.; Mohr, J.; Vogt, H.; tajiri, H.; Ahrens, Voigt, A.; An X-ray refractive mosaic lens with very large aper-ture; ICXoM 22 Konferenz, Hamburg, Deutschland, 02.09. - 6.09.2013

• Jark, W.; last, A.; Márkus, o.; High speed photon energy tuning of X-rays with high duty cycle by use of Clessidra prism arrays; SpIe proceedings zur Konferenz “Advances in X-Ray/euV optics and Components VIII (Conference 8848)” ende August 2013 in San Diego

• Nazmov, V.; Mohr, J., Simon, R.; Mosaic-like micro micropillar array for hard x-ray focusing - one-dimensional version; Journal of Michromechan-ics and Microengineering, 23 (2013), pp. 095015 DoI: 10.1088/0960-1317/23/9/095015

• Vogt, H.; last, J.; Mohr, J.; Marschall, F., Kluge, M.; Nazmov, V.; Metten-dorf, K.-u.; eisenhower, R.; low Cost Rolled Xray prism lenses to Increase photon Flux Density in Diffractometry experiments; proceedings of: Den-ver X-ray Conference 2013, the Westin Westminster, Westminster, Colo-rado, uSA, Aug 5 - 9, 2013

• Meiser, J.; Kunka, D.; Meyer, p.; Koch, F.; Amberger, M.; Schulz, J.; Wal-ter, M.; Mohr, J.; Gitterstrukturen mit hohem Aspektverhältnis für eine neuartige auf phasen- und Dunkelfeldkontrast beruhende Röntgen-bildgebung; proceedings Mikrosystemtechnik Kongress 2013, Aachen, Deutschland, 14.-16. oktober 2013, pp.450 – 452 VDe-Verlags GmbH, ISBN Nr. 978-3-8007-3555-6

• Vogt, H.; last, A.; Mohr, J.; Marschall, F.; Kluge, M.; Nazmov, V.; Metten-dorf, K.-u.; eisenhower, R.; Refraktive Röntgenlinsen zur Intensitätser-höhung im Spot einer Röntgenröhre; proceedings Mikrosystemtechnik Kongress 2013, Aachen, Deutschland, 14.-16. oktober 2013, pp. 453 - 456 VDe-Verlags GmbH, ISBN Nr. 978-3-8007-3555-6

• Kunka, D.; Mohr, J.; Nazmov, V.; Meiser, J.; Meyer, p.; Amberger, M.; Koch, F.; Schulz, J.; Walter, M.; Duttenhofer, t.; Voigt, A.; Ahrens, G.; Grützner, G.; Characterization method for new resist formulations for HAR patterns made by X-ray lithography; Microsystem technologies 2013 DoI:10.1007/s00542-013-2055-x

• Jochen Heneka „Neues lIGA2.X Verfahren zur industriellen Fertigung von hochpräzisen Kunststoff-Mikrobauteilen“, proceeding Mikrosystemtech-nik Kongress 2013 Aachen, ISBN 978-3-8007-3555-6, 306 – 308 as well as KIt presseinformation 091/2013

LIGA I, II, IIIX-ray lithography beamlines

the Institute for Microstructure technology (IMt) operates a cleanroom facility which is equipped with three lIGA beamlines to perform X-ray li-thography at ANKA. each beamline is dedicated to a specific task in the lIGA-process: high resolution X-ray mask making (lItHo 1), deep X-ray li-thography (lItHo 2) and ultra-deep X-ray lithography (lItHo 3; currently under commissioning; see below).

overviewIn 2013 about 20 projects were accepted and carried out within the frame-work the KNMF proposal system. the aim of these projects was to develop and fabricate high aspect ratio microstructure components for applications in fluidics, optics and mechanics, as well as mould inserts for replication. Among these project partners were several international institutions from France, Italy, Canada, Switzerland and england. In addition the beamlines were also used by the company microworks to manufacture precise lIGA structures for industrial use.

Developments 2013Besides the development and characterisation of new resist formulations within several BMBF projects (e.g. RölinGi) a major upgrade will be the upscaling of lItHo3. this will include a double mirror system for multi-pur-pose usage of the beamline and a new scanner unit.

user Activities 2013the majority of user projects still concentrate on the fabrication of high-ly sophisticated micro structures with dimensions down to the nanometer range and extreme aspect ratios (Fluidic Chips, RF MeMS structures, mould-ing tools, X-ray lenses and X-ray grating structures). A new generation of X-ray lIGA mould inserts has been created and investigated within a phD thesis which will be completed in the near future. In collaboration with tRlabs and the university of Saskatchewan (Canada) RF MeMS structures such as metal and polymer antennas have been produced and optimized with several material properties. Compound refractive X-ray optics have been fabricated at the lIGA beamlines with the aim to use them to build up a high energy X-ray microscope at petRA III and ANKA. In this context a new lens type (so called taille-lenses), with varying aperture along the optical axis has been developed which allows higher homogeneity in the field of view of the microscope image. Also lenses with customer defined spot sizes have been successfully realized. the lenses have been characterized at the beamlines ANKA-topo-toto and ANKA-NANo. Further process development will result in improved illumination optics and imaging optics specially designed for use at ANKA respectively petRA III in 2014.

Figure 1: CRL with varying apertures

Figure 2: Image intensity distribution for a) CRL with constant aperture b) “Taille”-CRL. The increase of intensity in the edges could be seen clearly.

Further improvement in the quality of our X-ray gratings for computed to-mography (Ct) has also been achieved, with optimized exposure and pro-cessing conditions in general resulting in grating set-ups which show an increase of the visibility of more than a factor 2 in an x-ray tube configu-ration. By stitching individual grating structures (50 x 50 mm2) together a larger operational area can be achieved. High quality phase contrast and dark field images could be achieved for areas of 50 x 100 mm2 and even 100 x 100 mm².

Figure 3a): Two stitched 50x50mm² gratings to achieve an active area of 50x100mm²

Figure 3b) The challenge of stitching is to achieve well aligned gratings with a correct spacing and a minimized squint.

A more detailed description of the activities can be found in the KNMF Annual Report 2013.

Microfabrication Martin Börner: [email protected] +49 (0)721 608 24437pascal Meyer:[email protected] +49 (0)721 608 23924

Franz Josef pantenburg: [email protected] +49 (0)721 608 22600



Lab Report

Bio lab

KNMF laboratory for Synchrotron Characterisation

Lab Report Appendix Beamline ReportAccelerator ReportUser Operation


(mRNA) levels (Bio-Rad 185-5200Sp2)• SDS-pAGe and Western blot: Separation of proteins, specific identifica-

tion of proteins via antibodies (Bio-Rad 165-8025Mp & 170-3848Mp)• Gel electrophoresis and Imaging system: Separation of DNA and RNA,

visualization of DNA, RNA and proteins (Bio-Rad 170-8195Mp)

For 2014, the plan is to bring all equipment into service, establish the first sample preparation protocols and also prepare the requirements for S1-sta-tus (biosafety level 1), which will the also allow working with certain genet-ically modified organisms.

thomas van de Kamp: [email protected]

BioLabthe ANKA Biolab is dedicated to provide the workspace and necessary equipment to characterize and prepare biological samples for experiments at ANKA. It supports both in-house research and user experiments, mainly in connection to the tomography beamlines topo-toMo and IMAGe.

overviewA key aspect of the laboratory is the sample preparation for cryogenic ex-periments at the ANKA hard X-ray cryo microscope, which is currently com-missioned at the NANo Beamline and will be installed at the IMAGe Beam-line. For this purpose the laboratory is equipped with a high pressure freezer to process small tissue samples. Further, an automated plunge freezing sys-tem for cryo preparation of fluid or extremely thin samples is installed.

For tomographic experiments of larger biological samples, a critical point dryer allows controlled drying of specimens up to a size of several centi-meters.

Figure 1: Fume hood

the samples can be characterized by optical microscopy before and after the X-ray experiments. For this purpose, two microscopes are installed to facilitate (fluorescence) light microscopy and stack photography.

Methods from molecular biology like real-time pCR, SDS-pAGe, Western Blot and gel electrophoresis allow for the hierarchical analysis of radiation dose on the levels of DNA, RNA and proteins and the investigation of mo-lecular mechanisms promoting for example cell migration, cell death and cell growth.

Figure 2: Working space of the BioLab

Furthermore, samples embedded into epoxy resin may be sectioned with an ultramicrotome for histological staining and correlative imaging (e.g. light microscopy and transmission electron microscopy).

Figure 3: PCR cycler, critical point dryer and stereo microscope (from left to right)

Developments in 2013In 2013, the installation of the Biolab was completed and it has been fitted with the equipment for the preparation and characterization of biologicals samples for measurements at the imaging beamlines.

Available techniques are:• Sample preparation for X-ray tomography and Microscopy• plunge freezing: Shock-freezing of samples up to 50 µm thickness; sam-

ples on teM grids (leica eM Gp)• High pressure freezing (operated by ItG): Freezing of tissue samples of

about 100 µm thickness (Wohlwend HpF Compact 02)• Freeze substitution (operated by ItG): embedding of cryo samples (leica

AFS2)• Critical point drying: Gentle drying of larger samples for tomography

or electron microscopy; Sample size up to several centimeters (leica eM CpD 300)

• Microtomy (located at ItG). Cryo sectioning for transmission electron mi-croscopy; sections of about 50 to 100 nm thickness (leica eM uC7 with eM FC7 cryo chamber)

• Correlative Imaging• light microscopy: 5x, 10x, 20x, 40x, 63x objective lenses; multiple (au-

tomated) image acquisition options (z-stack, mosaic) (leica DMI 6000B)• Stereo microscopy: pre- and post-inspection of samples; moderate mag-

nification (0.57-9.2x); Stack photography (leica Z16 Apo)• Molecular Biology• Real-time pCR Cycler: Quantification of DNA and gene expression

Lab Report Appendix Beamline ReportAccelerator ReportUser Operation

Bio Lab | KNMF


KNMF Laboratory for Synchrotron Characterisation Infrared and hard X-ray spectroscopy, X-ray diffraction – IR1, IR2, pDIFF, XAS, and X-SpeC Beamlines

T. Baumbach, S. Doyle, B. Gasharova, C. Heske, B. Krause, S. Mangold, Y.-L. Mathis, D. Moss, A.-S. Müller, and L. Weinhardt,

Karlsruhe Institute of Technology (KIT), ANKA

ANKA, the national German synchrotron radiation facility at KIt, is engaged in the KNMF activities of its laboratories for Microfabrication and Synchro-tron Characterization. ANKA provides dedicated user service for the Nano-science and Microtechnology user communities. Beamtime is accessible via the proposal portals of the KNMF (in particular in combination with other KNMF technologies) and of ANKA, and beamtime allocation is based on a peer-review process.

In 2013, the pool of ANKA beamlines accessible via the KNMF proposal portal included infrared/tHz spectroscopy and ellipsometry (IR1 beamline), polycrystalline/powder X-ray diffraction (pDIFF beamline), and X-ray absorp-tion spectroscopy (XAS beamline). Furthermore, the commissioning of the IR2 beamline (infrared/tHz microspectroscopy) was completed and user op-eration commenced. And, finally, X-SpeC, a future beamline in the soft and hard X-ray regime for X-ray spectroscopy and in-situ studies, was designed and ordered. In the following, the various beamline capabilities and their upgrades in 2013 will be briefly discussed, and a science application of an off-normal sputter deposition study will be presented

the IR1 and IR2 beamlines feature classical synchrotron radiation and edge radiation from a bending magnet and offer infrared/tHz spectroscopy, microspectroscopy, and ellipsometry capabilities. the experimental stations at both beamlines are based on FtIR spectrophotometers (Bruker IFS 66v/S), covering a spectral range from 4 to 10,000 cm-1 with a spectral resolution down to 0.1 cm-1, and equipped with high-sensitivity detectors and appro-priate beamsplitters for all spectral ranges.

the ellipsometry set-up at IR1 is operated by MpI-FKF Stuttgart and the university of Fribourg, Switzerland, runs under vacuum, and features an op-timized bolometer detector and a liquid He cryostat. Coherent tHz emission can be exploited when the ANKA accelerator is operated in low-α mode, resulting in an extremely intense beam in the 5 – 50 cm-1 spectral range.

the ellipsometry set-up at IR1 runs under vacuum and features an optimized bolometer detector and a liquid He cryostat. Coherent tHz emission can be exploited when the ANKA accelerator is operated in low-α mode, resulting in an extremely intense beam in the 5 – 50 cm-1 spectral range.

the newly accessible IR2 experimental station exploits the brilliance advan-tage of synchrotron light to offer infrared/tHz microspectroscopy at mea-surement spot sizes down to the diffraction limit. the vacuum spectropho-tometer is complemented by a Bruker IRscope II infrared microscope with single-element and imaging detectors, including a liquid He cooled bolome-ter for the far IR spectral range down to 100 cm-1. A selection of microscope objectives is available for measurements in transmission, reflection, grazing incidence, and AtR sampling geometry.

the XAS beamline features X-ray absorption spectroscopy (XAS) on a di-pole magnet source. Besides standard XAS measured in transmission (de-tection limit ~5%) and fluorescence (detection limit 1 mmol/l) modes, the

beamline offers a “Quick XAS” mode, allowing scans as fast as 30 seconds. Grazing incidence XAS provides surface sensitivity in the 50 nm range. the XAS beamline spans the energy range from 2.4 to 27 keV, covering the K-edges from S to Cd, and up to the l-edge of u. upgrades performed in 2013 focused on the installation of an experimental table with high load ca-pacity and 6 degrees of freedom. Further ongoing upgrades will allow high-ly reproducible (better than 10 µm) and fast exchange of sample holders.

the PDIFF beamline is primarily used for hard X-ray diffraction investiga-tions of bulk polycrystalline materials under varying in-situ conditions, utiliz-ing various combinations of detectors and sample-environmental chambers. Various transmission and reflection diffraction geometries are possible, and samples in various forms can be measured (capillaries, flat plates, pellets, and thin films). In addition, the beamline offers the possibility of high-res-olution powder diffraction for detailed structural investigations, residual stress and texture measurements, albeit with reduced options for in-situ observations.

In 2013 a wide variety of investigations were performed at the beamline for the elucidation of the relationship between crystal and supramolecular structure and materials functionality. examples from current research proj-ects, with particular focus on micro- and nano-properties, include in-situ studies on the influence of grain size, grain boundaries and stacking faults on the deformation mechanics in thin multilayer films, in-situ observation of strain development in pearlitic steel wires, and the in-situ characterization of phase composition in li-ion battery materials during charge/discharge cy-cling. technical developments at the pDIFF beamline in 2013 have included the installation of a motorized linear stage for the large CCD camera and the commissioning of a setup for repeated cyclic measurement of multiple battery-cells during charging/discharging processes.

the portfolio of beamlines available through the KNMF will, in the future, be complemented by the X-SPEC beamline. X-SpeC will cover a broad energy range (approx. 80 eV to 15 keV), bringing together soft and hard X-rays in one beamline, and combining them with

Fig. 1: Top left: Sputter geometry for off-normal deposition. Top right: Pole figure showing the resulting biaxial texture. Bottom left: Non-contact AFM image of a VN thin film surface, bottom right: in-situ texture measurement.

cutting-edge spectroscopy techniques. these methods will extend KNMF’s spectroscopy portfolio with capabilities such as hard X-ray photoelectron spec-troscopy (HAXpeS) and resonant inelastic soft X-ray scattering (soft RIXS).

Jürgen Mohr: [email protected]

Nanostructure formation mechanisms during sputter depositionAs an example of research conducted within the framework of the KNMF laboratory for Synchrotron Radiation (in combination with other KNMF facilities), we report on a study of the fundamental structure formation mechanisms during sputter deposition. off-normal deposition offers very interesting possibilities to tailor the nanostructure of sputter-deposited thin films. the direction of the incoming flux influences the orientation, size, and porosity of columnar structures formed, e.g., by transition metal car-bides and nitrides. It can also change the crystallite orientation, leading in the extreme case to the formation of biaxial textures. these textures are of special interest since, for many applications, they offer a cheap alternative to single-crystalline material. Both the texture and the shape of the columns allow for the control of the mechanical properties of the coating. For the prediction of these properties, a detailed understanding of the growth process is required. In situ X-ray reflectivity, eXAFS and diffraction measurements at the synchrotron give de-tailed insight into the sputter process [1]. to further deepen the understand-ing and to arrive at a unique interpretation of the results, however, further correlation with complementary measurement approaches is needed. As shown in Fig. 1, additional data for a VN thin film surface was obtained, utilizing the experimental capabilities to derive pole figure measurements and scanning probe microscopy data.

[1] Krause et al., J. Synchr. Rad. 19 (2012) 216.

Soft x-ray spectroscopy and spectromicroscopy – WeRA

P. Nagel, M. Merz, D. Fuchs, Th. Wolf, M.-J. Huang, H. v. Löhneysen, and S. Schuppler Karlsruhe Institute of Technology (KIT), Institut für Festkörperphysik (IFP)

the Institute for Solid-State physics (IFp) at KIt owns and operates the soft x-ray analytics facility WeRA at the synchrotron radiation facility ANKA. WeRA is designed for facilitating combinatory studies of the electronic and magnetic structure and microstructure, which have particular promise for strongly correlated, thin-film, and/or nanoscale materials. this is both at the heart of IFp’s own activities within the HGF programme “Science and tech-nology of Nanosystems” (StN) and those of the external user communities, which can access WeRA via peer review through the ANKA and KNMF por-tals and also through the eu programme QNano.

the soft x-ray analytics facility WeRA takes a fully combinatory and inte-grative approach to studying the microscopic electronic and magnetic structure – (i) by coherently combining important electron spectroscopies (peS, NeXAFS, XMCD; all in a number of variants; XMCD is supplied through a long-term cooperation with the MpI-IS Stuttgart) mutually and also with laterally resolved spectromicroscopy in peeM (μ-NeXAFS, μ-peS, μ-XMCD); (ii) by organically tying in quasi-in-situ sample synthesis in currently 4 prepa-ration chambers, all dedicated to specific techniques including pulsed-laser deposition (plD), and with uHV sample transfer between endstations and chambers; and (iii) also by combining radiation sources: bending magnet for more “standard” experiments and covering the full photon-energy range 100 – 1500 eV; undulator (future) for experiments demanding considerably enhanced sensitivity (higher photon flux / flux density) and ultimately also with full polarization control. the resulting cluster of methods and possibili-ties is unique, and users increasingly appreciate the further insights that this approach and these combinations offer for their experiments.

Within the general thrust of IFp’s activities in StN to understand strong electron-electron correlations and related phenomena in condensed mat-ter, current in-house research at WeRA concentrates on 3d transition-metal (tM) compounds where electron correlation competes with other interac-tions on similar energy scales to create phases with novel properties (and

susceptible to epitaxial strain imposed by and tunable through the growth process), and on iron-based pnictides whose superconducting properties have posed important challenges in condensed-matter physics as well. user projects performed at WeRA cover a large variety of interesting subjects in fundamental and applied science and typically range from microscopic to long-range effects, from molecular order in organic materials to novel magnetic properties, from bulk samples to ultrathin films, and more. the element-specific electronic and magnetic structure of all those materials has been studied by performing electron spectroscopies like NeXAFS, peS, and XMCD and spectromicroscopy (peeM), and also taking advantage of the possibilities for in-situ sample preparation at WeRA. In the following, we briefly touch upon a selection of recent results.

Recently, new aspects of the magnetic exchange mechanism in hole-doped ferromagnetic cobaltates could be clarified with the help of XMCD on ep-itaxially strained la0.7Sr0.3Coo3 films [1]. o K XMCD is directly sensitive to both magnetism and hybridization. An XMCD effect is found only for the energy range of t2g states which thus must participate in the magnetic ex-change. Furthermore, the strong strain dependence of the magnetic anisot-ropy (even with a sign change) indicates a substantial effect of Jahn-teller distortion, which can occur only in Co3+ HS and, thus, corroborates that the magnetic interaction is of the Co3+ HS – Co4+ HS double exchange (De) type. the high sensitivity of tC to the bulk compression, along with the linear cor-relation between tC and the strength of the o2p-Co3d hybridization observed in NeXAFS and XMCD, indicates that the double exchange is, however, spe-cial in that it approaches the limit of strong coupling. this is also evident in and can be explained by the small bandwidth of the t2g-derived states. In other words: a new, strong-coupling, t2g-mediated double exchange appears to be at work here, not the plain-vanilla, medium-coupling eg-based De gen-erally found in other tM systems such as the manganites.

the exchange interaction of the single spin localized at the central ion of Cu-tetraazaporphyrin molecules deposited on magnetite (100) was shown by XMCD to have clear anisotropic character, indicating that in this sys-tem, the Heisenberg model usually used to describe exchange interaction in molecular magnets becomes insufficient. this opens up possibilities for a future control over the spin configuration in single molecular magnets [2]. XpS and NeXAFS helped to understand the depth-dependent molecular orientation when chemically transforming chloroaluminum phthalocyanine, AlClpc, to μ-(oxo)bis(phthalo-cyaninato)aluminum(III), (pcAl)2o, on indium tin oxide [3], indicating also that a controlled environment, in particular the presence of some humidity, is necessary for the reaction to take place. Fur-ther interesting results include certain aspects of the Kondo effect observed in Gd-doped Zno, where XMCD shows the dopant to behave entirely para-magnetic [4], and the absence of an XMCD effect for all elements contained in ferromagnetic In2o3:Cr, suggesting that the magnetism in this system originates from vacancies [4]. Most fruitful has been the cooperation with the Max-planck Institute for Intelligent Systems (MpI-IS) Stuttgart (prof. G. Schütz, pD e. Goering, and coworkers). their excellent XMCD setup at WeRA – fully embedded in the WeRA user facilities available through the standard ANKA and KNMF review system – is made almost peerless worldwide by the high sensitivity and par-ticularly by the new, fast-ramp 7 t magnet.

[1] D. Fuchs et al., phys. Rev. lett. 111, 257203 (2013).[2] J. Klanke et al., phys. Rev. lett. 110, 137202 (2013).[3] F. latteyer et al., Anal. Bioanal. Chem. 405, 4895 (2013).[4] Y. li et al., phys. Rev. B 87, 155151 (2013); J. B. Yi et al. thin Solid Films 531, 481 (2013).

Lab Report

Bio Lab | KNMF

Appendix Beamline ReportAccelerator ReportUser Operation


Appendix ANKA Seminars 2013

publications 2013

Appendix Lab ReportBeamline ReportAccelerator ReportUser Operation


ANKA Seminars 2013

Feasibility study of low emittance storage ring based on ANKA synchrotron light source,evgenij levichev, Budker Institute for Nuclear physics, Novosibirsk, Russia

Overview and current activities at the Sirius Light Source,James Citadini, Instrumentação e Controles especiai, CNpeM/lNlS, Brasil

Enhancement of Arsenic Adsorption during Mineral Transformation from Siderite to Goethite: Mechanism and Application, Huaming Guo, School of Water Resources & environment China university of Geosciences, Beijing, p.R.Ch

Nano-meter resolution X-ray topography (nm-XRT), ping Yang, Singapore Synchrotron light Source (SSlS), National university of Singapore

Commissioning of the third stage of the Novosibirsk free electron laser and achievements in the terahertz optics and photonics,Boris Knyazev, Budker Institute of Nuclear physics SB RAS, Novosibirsk & Novosibirsk State university

Microstructured Frequency Selective Quasi-Optical Components and Devices for MM-wave and Terahertz Applications: Research-and-De-velopment Activities in Novosibirsk,Sergey Kuznetsov, laboratory of Advanced Research on MM-wave and tHz Radiation, Novosibirsk State university (NSu)

How to characterise a beam - without touching it?Carsten p. Welsch, university of liverpool / Cockcroft Institute, uK

Phase retrieval in in-line phase tomography - developments and ap-plications,Max langer, european Synchrotron Radiation Facility, Grenoble Cedex, France

Discontinuous Galerkin Schemes for Kinetic Plasma Models and Po-tential Application to Laser-Plasma Accelerators,James Rossmanith, Iowa State university, uS

Effect of disorder and reduced dimensionality on phonons in iron oxide - ab initio and nuclear inelastic scattering studies,przemysław piekarz, Institute of Nuclear physics in Kraków, polish Academy of Sciences, poland

The I12 High Energy Beamline for Engineering, Material Science and Processing at the Diamond Light Source,Michael Drakopoulos, Diamond light Source, uK

HRPD Beamline P02.1 at Petra III,peter Walter, Deutsches elektronen-Synchrotron (HASYlAB), Germany

X-ray tomography of granular and colloidal materials,Mario Scheel, european Synchrotron Radiation Facility, France 3D-Druck / Rapid Prototyping: Überblick über den Stand der Technik und die Möglichkeiten einer neuen Fertigungstechnologie. Vorführung eines 3D-Druckers, peter Moster, INR, KIt, Germany

Applications of X-ray phase-contrast imaging in diagnostics of emerging X-ray sources and in biomedical imaging,Sergei Gasilov, Department of physics, ludwig Maximilians university, Muenchen, Germany

WAVE - A Computer Code for the Tracking of Electrons Through Magnetic Fields and the Calculation of Spontaneous Synchrotron Radiation,Michael Scheer, Helmholtz-Zentrum Berlin für Materialien und energie

Electronic structure investigation of organic/metal interfaces with soft x-ray photoelectron spectroscopy,Marc Häming, university of Würzburg, experimental physics VII, Germany

Picosecond Photochemistry Studied with X-Ray Absorption Spectroscopy, using an X-Ray Streak Camera,Bernhard Adams, Advanced photon Source, uSA

X-ray Phase Imaging Based on Grating Interferometry,Atsushi Momose, Institute of Multidisciplinary Research for Advanced Materials, tohoku university, Japan

Case studies of polycrystalline and epitaxial metallic thin film growth using real-time optical stress sensor,G. Abadias, université de poitiers-CNRS-eNSMA, Département physique et Mécanique des Matériaux, France

pawel Wesolowski: [email protected]

Appendix

ANKA Seminars 2013 | Publications 2013

Lab ReportBeamline ReportAccelerator ReportUser Operation


Hahn, S. Indris Structural Evolution of Li2Fe1-yMnySiO4 (y = 0, 0.2, 0.5, 1) Cathode Materials for Li-Ion Batteries upon Electrochemical Cycling, J. Phys. Chem. C 117 (2013) 884-893

32. H. Curtius,G. Kaiser, K. Rozov, A. Neumann, K. Dardenne, D. Bos-bach Preparation and Characterization of Fe-, Co-, and Ni-contain-ing Mg-Al-Layered Double Hydroxides, Clays and Clay Minerals 61 (2013) 424-439

33. J. Czapla, W. M. Kwiatek, J. Lekki, J. Dulińska-Litewka, R. Steininger, J. Göttlicher Chemical species of sulfur in prostate can-cer cells studied by XANES spectroscopy, Radiat. Phys. Chem. 93 (2013) 154-159

34. J. Czapla, W. M. Kwiatek, J. Lekki, A. Kisiel, R. Steininger, J. Goet-tlicher EXAFS studies of prostate cancer cell lines, J. Phys.: Conf. Ser. 430 (2013) 012040

35. N. D´Avanzo, E. C. McCusker, A. M. Powl, A. J. Miles, C. G. Nich-ols, B. A. Wallace Differential Lipid Dependence of the Function of Bacterial Sodium Channels, PLoS ONE 8 (2013) e61216

36. A. Danilewsky, J. Wittge, K. Kiefl, D. Allen, P. McNally, J. Garagorri, M. Reyes Elizalde, T. Baumbach, B. K. Tanner Crack propagation and fracture in silicon wafers under thermal stress, J. Appl. Cryst. 46 (2013) 849-855

37. I. Denden, R. Essehli, M. Fattahi Spectrophotometric study of the behaviour of pertechnetate in trifluoromethanesulfonic acid: effect of alpha irradiation on the stability of Tc(VII), J. Radioanal. Nucl. Chem. 296 (2013) 149-155

38. M. A. Denecke, T. Petersmann, R. Marsac, K. Dardenne, T. Vito-va, T. Prüßmann, M. Borchert, U. Bösenberg, G. Falkenberg, G. Wellenreuther XANES characterization of UO2/Mo(Pd) thin films as models for ε-particles in spent nuclear fuel, J. Phys.: Conf. Ser. 430 (2013) 012113

39. O. Deutschmann, J-D. Grunwaldt Abgasnachbehandlung in mo-bilen Systemen: Stand der Technik, Herausforderungen und Pers-pektiven, Chemie Ingenieur Technik 85 (2013) 595-617

40. J. Ebad-Allah, L. Baldassarre, M. Sing, R. Claessen, V. A. M. Bra-bers, C. A. Kuntscher Polaron physics and crossover transition in magnetite probed by pressure-dependent infrared spectroscopy J. Phys.: Condens. Matter 25 (2013) 035602

41. F. P. A. Fabbiani, G. Buth, D. C. Levendis, A. J. Cruz-Cabeza Phar-maceutical hydrates under ambient conditions from high-pressure seeds: a case study of GABA monohydrate, Chem. Commun. DOI: 10.1039/c3cc48466a (2013)

42. M. Fischer, D. N. Thomas, A. Krell, G. Nehrke, J. Goettlicher, L. Norman, K. M. Meiners, C. Riaux-Gobin, G. S. Dieckmann Quan-tification of ikaite in Antarctic sea ice, Antarctic Science 25 (2013) 421-432

43. U. E. A. Fittschen, C. Streli, F. Meirer, M. Alfeld Determination of phosphorus and other elements in atmospheric aerosols using syn-chrotron total-reflection X-ray fluorescence, X-Ray Spectrometry 42 (2013) 368-373

44. D. Franz, S. Runte, C. Busse, S. Schumacher, T. Gerber, T. Michely, M. Mantilla, V. Kilic, J. Zegenhagen, A. Stierle Atomic Structure and Crystalline Order of Graphene-Supported Ir Nanoparticle Lattices, Phys. Rev. Lett. 110 (2013) 065503

45. D. Fuchs, M. Merz, P. Nagel, R. Schneider, S. Schuppler, H. von Löhneysen Double exchange via t2g orbitals and the Jahn-Teller ef-fect in ferromagnetic La0.7Sr0.3CoO3 probed by epitaxial strain, Phys. Rev. Lett. 111 (2013) 257203

46. H. Fukui, M. Simon, V. Nazmov, J. Mohr, K. Evans-Lutterodt, A. Stein Alfred, A. Q. R. Baron Large-aperture refractive lenses for momentum-resolved spectroscopy with hard X-rays J. Synchrotron Rad. 20 (2013) 591-595

47. B. Fulda, A. Voegelin, F. Maurer, I. Christl, R. Kretzschmar Cop-per Redox Transformation and Complexation by Reduced and Ox-idized Soil Humic Acid. 1. X-ray Absorption Spectroscopy Study, Environ. Sci. Technol. 47 (2013) 10903-10911

48. B. Fulda, A. Voegelin, K. Ehlert, R. Kretzschmar Redox transforma-tion, solid phase speciation and solution dynamics of copper during

soil reduction and reoxidation as affected by sulfate availability, Geochimica et Cosmochimica Acta 123 (2013) 385-402

49. L. Gharnati, N. E. Musko, A. D. Jensen, G. M. Kontogeorgis, J.-D. Grunwaldt Fluid phase equilibria during propylene carbonate syn-thesis from propylene oxide in carbon dioxide medium, J. of Super-critical Fluids 82 (2013) 106-115

50. J. Goettlicher, A. Kotelnikov, N. Suk, A. Kovalski, T. Vitova, R. Steininger Sulfur K X-ray absorption near edge structure spectros-copy on the photochrome sodalite variety hackmanite, Z. Kristal-logr. 228 (2013) 157-171

51. C. A. Gorski, L. E. Klupfel, A. Voegelin, M. Sander, T. B. Hofstetter Redox Properties of Structural Fe in Clay Minerals: 3. Relationships between Smectite Redox and Structural Properties, Environ. Sci. Technol. 47 (2013) 13477-13485

52. F. Greiner, S. Quednau, F. Dassinger, R. Sarwar, H. F Schlaak, M. Guttmann, P. Meyer Fabrication techniques for multiscale 3D-MEMS with vertical metal micro- and nanowire integration, J. Micromech. Microeng. 23 (2013) 025018

53. J.-D. Grunwaldt, J. B. Wagner, R. E. Dunin-Borkowski Imaging Catalysts at Work: A Hierarchical Approach from the Macro- to the Meso- and Nano-scale, Chem. Cat. Chem. 5 (2013) 62-80

54. A. Grzechnik, N. Khaidukov, K. Friese Crystal structures and sta-bility of trigonal KLnF4 fluorides (Ln = Y, Ho, Er, Tm, Yb), Dalton Transact. 42 (2013) 441-447

55. T. Günter, M. Casapu, D. Doronkin, S. Mangold, V. Trouillet, T. Augenstein, J.-D. Grunwaldt Potential and Limitations of Natural Chabazite for Selective Catalytic Reduction of NOx with NH3, Che-mie Ingenieur Technik 85 (2013) 632-641

56. M. Hagelstein, T. Liu, S. Mangold, M. Bauer Time-resolved com-bined XAS and UV-Vis applied to the study of the cerium catalysed BZ reaction, J. Phys.: Conf. Ser. 430 (2013) 012123

57. E. Hamann, A. Cecilia, A. Zwerger, A. Fauler, O. Tolbanov, A. Tyazhev, G. Shelkov, H. Graafsma, T. Baumbach, M. Fiederle Char-acterization of photon counting pixel detectors based on semi-insu-lating GaAs sensor material, J. Phys.: Conf. Ser. 425 (2013) 062015

58. L. Hartmann, D. Djurado, I. Florea, J-F. Legrand, A. Fiore, P. Reiss, S. Doyle, A. Vorobiev, S. Pouget, F. Chandezon, O. Ersen, M. Brink-mann Large-Scale Simultaneous Orientation of CdSe Nanorods and Regioregular Poly(3-hexylthiophene) by Mechanical Rubbing, Macromolecules 46 (2013) 6177-6186

59. S. Heidari Bateni, F. Bonfigli, A. Cecilia, T. Baumbach, D. Pelliccia, F. Somma, M. A. Vincenti, R. M. Montereali Optical characterisation of lithium fluoride detectors for broadband X-ray imaging, Nucl. In-str. Meth. Phys. Res. A 720 (2013) 109-112

60. U. Hejral, A. Vlad, P. Nolte, A. Stierle In Situ Oxidation Study of Pt Nanoparticles on MgO(001), J. Phys. Chem. C 117 (2013) 19955-19966

61. L. Helfen, F. Xu, H. Suhonen, P. Cloetens, T. Baumbach Lamino-graphic imaging using synchrotron radiation – challenges and op-portunities, J. Phys.: Conf. Ser. 425 (2013) 192025

62. L. Helfen, F. Xu, H. Suhonen, L. Urbanelli, P. Cloetens, T. Baum-bach Nano-laminography for three-dimensional high-resolution im-aging of flat specimens, J. Instr. 8 (2013) C05006

63. S. Hillenbrand, R. Assmann, A.-S. Müller, O. Jansen, V. Judin, A. Pukhov Study of Laser Wakefield Accelerators as injectors for Syn-chrotron light sources, Nucl. Instr. Meth. Phys. Res. A http://dx.doi.org/10.1016/j.nima.2013.10.081i (2013)

64. E. Hiller, M. Petrák, R. Tóth, B. Lalinská-Voleková, L. Jurkovič, G. Kučerová, A. Radková, P. Šottník, J. Vozár Geochemical and min-eralogical characterization of a neutral, low-sulfide/high-carbonate tailings impoundment, Markušovce, eastern Slovakia, Environ. Sci. Pollut. Res. 20 (2013) 7627-7642

65. A. F. Hofacker, A. Voegelin, R. Kaegi, R. Kretzschmar Mercury Mobilization in a Flooded Soil by Incorporation into Metallic Copper and Metal Sulfide Nanoparticles, Environ. Sci. Technol. 47 (2013) 7739-7746

66. A. F. Hofacker, A. Voegelin, R. Kaegi, F.-A. Weber, R. Kretzschmar

Publications 2013

ISI refereed publications

1. G. Abbas, Y. Lan, V. Mereacre, G. Buth, M. T. Sougrati, F. Grand-jean, G. J. Long, C. E. Anson, A. K. Powell: Synthesis, Magnetism, and 57Fe Mössbauer Spectroscopic Study of a Family of [Ln3Fe7] Coordination Clusters (Ln = Gd, Tb, and Er), Inorg. Chem. 52 (2013) 11767-11777

2. S. Achenbach, D. T. Haluzan, D. M. Klymyshyn, M. Börner, J. Mohr: Large tuning ratio high aspect ratio variable capacitors using lev-eraged bending, Microsyst. Technol. DOI 10.1007/s00542-013-19407(2013)

3. V. Afonso Rodríguez, A. Bernhard, A. Keilmann, P. Peiffer, R. Ross-manith, C. Widmann, T. Baumbach, M. Nicolai, M. C. Kaluza: De-velopment of a Superconducting Transverse-Gradient Undulator for Laser-Wakefield Accelerators, IEEE Transactions on Applied Superconductivity 23 (2013) 4101505

4. A. M. Ako, B. Burger, Y. Lan, V. Mereacre, R. Clerac, G. Buth, S. Gomez-Coca, E. Ruiz, C. E. Anson, A. K. Powell: Magnetic Interac-tions Mediated by Diamagnetic Cations in [Mn18M](M = Sr2+,Y3+,Cd2+, and Lu3+) Coordination Clusters, Inorg. Chem. 52 (2013) 5764-5774

5. S. Aland, S. Boden, A. Hahn, F. Klingbeil, M. Weismann S. Weller: Quantitative comparison of Taylor flow simulations based on sharp-interface and diffuse-interface models, International Journal for Numerical Methods in Fluids 73 (2013) 344-361

6. A. Al-Ebraheem, K. Geraki, R. Leek, A. L Harris, M. J Farquharson: The use of bio-metal concentrations correlated with clinical prog-nostic factors to assess human breast tissues, X-Ray Spectrometry 42 (2013) 330-336

7. N. L. Banik, M. A. Denecke, A. Geist, G. Modolo, P. J. Panak, J. Rothe: 2,6-Bis(5,6-dipropyl-1,2,4-triazin-3-yl)-pyridine: Structures of An(III) and Ln(III) 1:3 complexes and selectivity, Inorg. Chem. 29 (2013) 172-174

8. A. Baniodeh, C. E. Anson, A. K. Powell: Ringing the changes in FeIII/YbIII cyclic coordination clusters Chem. Sci. 4 (2013) 4354-4361

9. M. Bär, J. Klaer, L. Weinhardt, R. G. Wilks, S. Krause, M. Blum, W. Yang, C. Heske, H.-W. Schock Cu2-xS Surface Phases and Their Impact on the Electronic Structure of CuInS2 Thin Films – A Hidden Parameter in Solar Cell Optimization, Advanced Energy Materials 3 ( 2013 ) 777-781

10. M. Bär, J.-P. Theisen, R. G. Wilks, F. Erfurth, R. Felix, D. Gerlach, S. Haas, L. Tati Bismaths, F. Reinert, F. Kronast, T. P. Niesen, J. Palm, S. Visbeck, L. Weinhardt Lateral inhomogeneity of the Mg/(Zn+Mg) composition at the (Zn,Mg)O/CuIn(S,Se)2 thin-film solar cell inter-face revealed by photoemission electron microscopy, J. Appl. Phys. 113 ( 2013 ) 193709-193709-5

11. M. Bär, S. Pookpanratana, L. Weinhardt , R. G. Wilks, B. A. Schubert, B. Marsen, T. Unold, M. Blum, S. Krause, Y. Zhang, A. Ranasinghe, K. Ramanathan, I. Repins, M. A. Contreras, S. Nishi-waki, X. Liu, N. R. Paudel, O. Fuchs, T. P. Niesen, W. Yang, F. Karg, A. D. Compaan, W. N. Shafarman, R. Noufi, H. Schock, C. Heske Soft X-rays shedding light on thin-film solar cell surfaces and inter-faces, Journal of Electron Spectroscopy and Related Phenomena 190 ( 2013 ) 47-53

12. N. Batuk, D. V. Szabó, M. A. Denecke, T. Vitova, S. N. Kalmykov Synthesis and characterization of thorium, uranium and cerium ox-ide nanoparticles, Radiochim. Acta 101 ( 2013 ) 233-239

13. O. Bauder, P. Piekarz, A. Barla, I. Sergueev, R. Rüffer, J. Łažewski, T. Baumbach, K. Parlinski, S. Stankov Lattice dynamics of the ra-re-earth element samarium, Phys. Rev. B 88 ( 2013 ) 224303

14. A. Beleanu, J. Kiss, G. Kreiner, C. Köhler, L. Müchler, W. Schnelle, U. Burkhardt, S. Chadov, S. Medvediev, D. Ebke, C. Felser Large resistivity change and phase transition in the antiferromagnet-

ic semiconductors LiMnAs and LaOMnAs, Phys. Rev. B (2013) 184429

15. B. D. Belviso, F. Italiano, R. Caliandro, B. Carrozzini, A. Costan-za, M. Trotta Cobalt binding in the photosynthetic bacterium R. sphaeroides by X-ray absorption spectroscopy, BioMetals 26 (2013) 693-703

16. P. J. Bereciartua, F. J. Zuñiga, J. M. Perez-Mato, V. Petříček, E. Vila, A. Castro, J. Rodríguez-Carvajal, S. Doyle Superspace De-scription of the System Bi2(n+2)Mon O6(n+1) (n=3, 4, 5 and 6) , Aperiodic Crystals (2013) 149-155

17. J. Bielecki, J. Jarzyna, S. Bożek, J. Lekki, Z. Stachura, W.M. Kwi-atek Computed microtomography and numerical study of porous rock samples, Radiat. Phys. Chem. 93 (2013) 59-66

18. S. Blahuta, A. Bessière, B. Viana, P. Dorenbos, V. Ouspenski Evi-dence and Consequences of Ce4+ in LYSO:Ce,Ca and LYSO:Ce,Mg Single Crystals for Medical Imaging Applications, IEEE Transact. Nucl. Sci. 60 (2013) 3134-3141 R.

19. M. Bolanz, M. Wierzbicka-Wieczorek, M. Čaplovičová, P. Uhlík, J. Göttlicher, R. Steininger, J. Majzlan Structural Incorporation of As5+ into Hematite, Environ. Sci. Technol. 47 (2013) 9140-9147

20. F. Bonfigli, A. Cecilia, S. Heidari Bateni, E. Nichelatti, D. Pelliccia, F. Somma, P. Vagovic, M. A. Vincenti, T. Baumbach, R. M. Montereali In-line X-ray lensless imaging with lithium fluoride film, detectors Radiat. Meas. 56 (2013) 277-280

21. A. Boubnov, A. Gänzler, S. Conrad, M. Casapu, J.-D. Grunwaldt Oscillatory CO Oxidation Over Pt/Al2O3 Catalysts Studied by In-situ XAS and DRIFTS, Top. Catal. 56 (2013) 333-338

22. A. Boubnov, H. Lichtenberg, S. Mangold, J.-D. Grunwaldt Structure and reducibility of a Fe/Al2O3 catalyst for selective catalytic reduc-tion studied by Fe K-edge XAFS spectroscopy, J. Phys.: Conf. Ser. 430 (2013) 012054

23. G. L. Bovenkamp, A. Prange, W. Schumacher, K. Ham, A. P. Smith, J. Hormes Lead uptake in diverse plant families: a study applying X-ray Absorption Near Edge spectroscopy, Environ. Sci. Technol. 47 (2013) 4375-4382

24. C. Bube, V. Metz, D. Schild, J. Rothe, K. Dardenne, M. Lagos, M. Plaschke, B. Kienzler Combining thermodynamic simulations, el-ement and surface analytics to study U(VI) retention in corroded cement monoliths upon > 20 years of leaching, Physics and Chem-istry of the Earth doi: http://dx.doi.org/10.1016/j.pce.2013.11.006 (2013)

25. D. J. Bull, L. Helfen, I. Sinclair, S. M. Spearing, T. Baumbach A com-parison of multi-scale 3D X-ray tomographic inspection techniques for assessing carbon fibre composite impact damage, Composites Science and Technology 75 (2013) 55-61

26. D. J. Bull, S. M. Spearing, I. Sinclair, L. Helfen Three-dimensional assessment of low velocity impact damage in particle toughened composite laminates using micro-focus X-ray computed tomogra-phy and synchrotron radiation laminography, Composites: Part A 52 (2013) 62-69

27. G. Buth, E. Huttel, S. Mangold, R. Steininger, D. Batchelor, S. Doyle, R. Simon Experimental Test of Data Analysis Methods from Staggered Pair X-ray Beam Position Monitors at Bending Magnet Beamlines, J. Phys.: Conf. Ser. 425 (2013) 042004

28. U. Carvajal Nunez, L. Martel, D. Prieur, E. Lopez Honorato, R. Eloir-di, I. Farnan, T. Vitova, J. Somers Coupling XRD, EXAFS, and 13C NMR to Study the Effect of the Carbon Stoichiometry on the Local Structure of UC1±x, Inorg. Chem. 52 (2013) 11669-11676

29. S. Casalbuoni, T. Baumbach, S. Gerstl, A. Grau, M. Hagelstein, C. Heske, T. Holubek, D. Saez de Jauregui, C. Boffo, W. Walter Sta-tus of the development of superconducting undulators at ANKA, J. Phys.: Conf. Ser. 425 (2013) 032008

30. A. Charnukha, D. Pröpper, T. I. Larkin, D. L. Sun, Z. W. Li, C. T. Lin, T. Wolf, B. Keimer, A. V. Boris Spin-density-wave-induced anomalies in the optical conductivity of AFe2As2,(A = Ca, Sr, Ba) single-crystalline iron pnictides, Phys. Rev. B 88 (2013) 184511

31. R. Chen, R. Heinzmann, S. Mangold, V.S. K. Chakravadhanula, H.

Anton plech: [email protected]

Appendix




Lett. 102 (2013) 241916 98. J. L. S. Lopes, D. Orcia, A. P. U. Araujo, R. DeMarco, B. A. Wallace

Folding Factors and Partners for the Intrinsically Disordered Protein Micro-Exon Gene 14 (MEG-14), Biophys. J. 104 (2013) 2512-2520

99. J. Majzlan, H. Schlicht, M. Wierzbicka-Wieczorek, G. Giester, H. Pöllmann, B. Brömme, S. Doyle, G. Buth, C. Bender Koch A contri-bution to the crystal chemistry of the voltaite group: solid solutions, Mössbauer and infrared spectra, and anomalous anisotropy, Miner. Petrol. 107 (2013) 221-233

100. S. Mangold, R. Steininger, T. dos Santos Rolo, J. Göttlicher Full field spectroscopic imaging at the ANKA-XAS- and -SUL-X-Beam-lines, J. Phys.: Conf. Ser. 430 (2013) 012130

101. S. Mangold, R. Steininger, T. Spangenberg High throughput data acquisition at the XAS and SUL-X beamline at ANKA, J. Phys.: Conf. Ser. 430 (2013) 012022

102. P. Marsik, C. N. Wang, M. Rössle, M. Yazdi-Rizi, R. Schuster, K. W. Kim, A. Dubroka, D. Munzar, T. Wolf, X. H. Chen, C. Bern-hard Low-energy interband transitions in the infrared response of Ba(Fe1-xCox)2As2 , Phys. Rev. B 88 (2013) 180508

103. M. C Martin, C. Dabat-Blondeau1, M. Unger, J. Sedlmair, D. Y. Par-kinson, H. A. Bechtel, B. Illman, J. M. Castro, M. Keiluweit, D. Bus-chke, B. Ogle, M. J. Nasse, C. J. Hirschmugl: 3D spectral imaging with synchrotron Fourier transform infrared spectro-microtomogra-phy, Nature Methods 10 (2013) 861–864

104. V. Maurel, L. Helfen, R. Soulignac, T. F. Morgeneyer, A. Koster, L. Rémy Three-Dimensional Damage Evolution Measurement in EB-PVD TBCs Using Synchrotron Laminography, Oxid. Met. 79 (2013) 313-323

105. P. Meyer, F. J. Pantenburg Monte Carlo study of the primary absorbed energy redistribution in X-ray lithography, Microsyst. Technol. DOI 10.1007/s00542-013-1966-x (2013)

106. F. Meyer, L. Weinhardt, M. Blum, M. Bär, R.G. Wilks, W. Yang, C. Heske, F. Reinert Non-equivalent carbon atoms in the resonant inelastic soft X-ray scattering map of cysteine, J. Chem. Phys. 138 (2013) 034306

107. J. Moosmann, J. Ershov, A. Altapova, V. Baumbach, T. Prasad, M.S. Labonne, C. Xiao, X., Kashef, J., R. Hofmann X-ray phase-contrast in vivo microtomography probes new aspects of Xenopus gastrulation, Nature 497 (2013) 374-377

108. J. Moosmann, V. Altapova, L. Helfen, D. Hänschke, R. Hofmann, T Baumbach High-resolution X-ray phase contrast tomography from single-distance radiographs applied to developmental stages of Xenopus laevis, Journal of Physics: Conference Series 425 (2013) 192003-1 - 192003-5

109. T.F. Morgeneyer, L. Helfen, H. Mubarak, F. Hild 3D Digital Volume Correlation of Synchrotron Radiation Laminography Images of Ductile Crack Initiation: An Initial Feasibility Study, Experimental Mechanics 53 (2013) 543-556

110. G. Muruganandam, J. Bürck, A. S. Ulrich, I. Kursula, P. Kursula Lip-id Membrane Association of Myelin Proteins and Peptide Segments Studied by Oriented and Synchrotron Radiation Circular Dichroism Spectroscopy, J. Phys. Chem. B 117 (2013) 14983-14993

111. A. Myagotin, A. Voropaev, L. Helfen, D. Hänschke, T. Baumbach Efficient Volume Reconstruction for Parallel-Beam Computed Lami-nography by Filtered Backprojection on Mulit-Core Clusters, IEEE Transactions on Image Processing 22 (2013) 5348-5361

112. M. Myllykoski, A. Raasakka, M. Lehtimäki, H. Han, I. Kursula, P. Kursula Crystallographic Analysis of the Reaction Cycle of 2’,3’-Cyclic Nucleotide 3’ Phosphodiesterase, a Unique Member of the 2H Phosphoesterase Family, J. Mol. Biol. 425 (2013) 4307-4322

113. D. Naglav, B. Tobey, A. Schnepf Application of GaCp as a Ligand in Coordination Chemistry: Similarities and Differences to GaCp Eur. J., Inorg. Chem. 2013 (2013) 4146-4149

114. M. J. Nasse, M. Schuh, S. Naknaimueang, M. Schwarz, A. Plech, Y.-L. Mathis, R. Rossmanith, P. Wesolowski, E. Huttel, M. Schmel-ling, A.-S. Müller FLUTE: A versatile linac-based THz source, Rev. Sci. Instrum. 84 (2013) 022705

115. V. Nazmov, J. Mohr, R. Simon Mosaic-like micropillar array for hard x-ray focusing—one-dimensional version, J. Micromech. Microeng. 23 (2013) 095015

116. A. Neumann, R. Kaegi, A. Voegelin, A. Hussam, A. K. M. Munir, S. J. Hug Arsenic Removal with Composite Iron Matrix Filters in Bangladesh: A Field and Laboratory Study, Environ. Sci. Technol. 47 (2013) 4544-4554

117. T. Neumann, F. Scholz, U. Kramar, M. Ostermaier, N. Rausch, Z. Berner Arsenic in framboidal pyrite from recent sediments of a shallow water lagoon of the Baltic Sea, Sedimentology 60 (2013) 1389-1404

118. O. Noked, A. Melchior, R. Shuker, T. Livneh, R. Steininger, B.J. Kennedy, E. Sterer Pressure-induced amorphization of La1/3TaO3 ,,J. Solid State Chem. 202 (2013) 38-42

119. W. Olovsson, L. Weinhardt, O. Fuchs, I. Tanaka, P. Puschnig, E. Umbach, C. Heske, C. Draxl The Be K-edge in beryllium oxide and chalcogenides: soft x-ray absorption spectra from first-princi-ples theory and experiment, J. Phys.: Condens. Matter 25 (2013) 315501

120. D. Oriwol, E.-R. Carl, A. N. Danilewsky, L. Sylla, W. Seifert, M. Kittler, H. S. Leipner Small-angle subgrain boundaries emanating from dislocation pile-ups in multicrystalline silicon studied with syn-chrotron white-beam X-ray topography, Acta Materialia 61 (2013) 6903-6910

121. B. Pacakova Bittova, M. Kalbac, S. Kubickova, A. Mantlikova, S. Mangold, J. Vejpravova Structure and magnetic response of a residual metal catalyst in highly purified single walled carbon nanotubes, Phys. Chem. Chem. Phys. 15 (2013) 5992-6000

122. A. Pareek, G. N. Ankah, S. Cherevko, P. Ebbinghaus, K. J. J. Mayrhofer, A. Erbe, F. U. Renner Effect of thiol self-assembled monolayers and plasma polymer films on dealloying of Cu–Au alloys, RSC Advances 3 (2013) 6586-6595

123. I. V. Pekov; N. V. Chukanov; Y. E. Filinchuk; A. E. Zadov; N. N. Kononkova; S. G. Epanchintsev; P. Kaden; A. Kutzer; J. Göttlicher Kasatkinite, Ba2Ca8B5Si8O32(OH)3 · 6H2O6, a new mineral from the Bazhenovskoe deposit, the Central Urals, Russia, Geology of Ore Deposits 55 (2013) 558-566

124. B. Pemmer, A. Roschger, A. Wastl, J. G. Hofstaetter, P. Wobraus-chek, R. Simon, H. W. Thaler, P. Roschger, K. Klaushofer, C. Streli Spatial distribution of the trace elements zinc, strontium and lead in human bone tissue Bone 57 (2013) 184-193

125. S. Permien, H. Hain, M. Scheuermann, S. Mangold, V. Mereacre, A. K. Powell, S. Indris, U. Schürmann, L. Kienle, V. Duppel, S. Har-ma, W. Bensch Electrochemical insertion of Li into nanocrystalline MnFe2O4: a study of the reaction mechanism RSC Adv. 3 (2013) 23001-23014

126. I. Pidchenko, S. Salminen-Paatero, J. Rothe, J. Suksi Study of ura-nium oxidation states in geological material, J. Environm. Radioac-tivity 124 (2013) 141-146

127. A. Plech, S. Ibrahimkutty, D. Issenmann, V. Kotaidis, A. Siems Ul-trafast x-ray scattering on nanoparticle dynamics, J. Phys.: Conf. Ser. 425 (2013) 092008

128. D. Prieur, P. Martin, F. Lebreton, T. Delahaye, D. Banerjee, A. C. Scheinost, A. Jankowiak Accommodation of multivalent cations in fluorite-type solid solutions: Case of Am-bearing UO2 , J. Nucl. Mat. 434 (2013) 7-16

129. D. Prieur, U. Carvajal-Nunez, T. Vitova, J. Somers Local and Elec-tronic Structure of Americium-Bearing PuO2 , Eur. J. Inorg. Chem. 2013 (2013) 1518-1524

130. D. Prodius, F. Macaev, Y. Lan, G. Novitchi, S. Pogrebnoi, E. Stin-gaci, V. Mereacre, C. E. Anson, A. K. Powell Evidence of slow re-laxation of magnetization in dysprosium-based ionic liquids, Chem. Commun. 49 (2013) 9215-9217

131. T. Prüßmann, M. A. Denecke, A. Geist, J. Rothe, P. Lindqvist-Reis, M. Löble, F. Breher, D. R. Batchelor, C. Apostolidis, O. Walter, W. Caliebe, K. Kvashnina, K .Jorissen, J. J. Kas, J. J. Rehr, T. Vitova Comparative investigation of N donor ligand-lanthanide complexes

Temperature-dependent formation of metallic copper and metal sulfide nanoparticles during flooding of a contaminated soil, Geo-chimica et Cosmochimica Acta 103 (2013) 316-332

67. T. Hofmann, T. H. Yu, M. Folse, L. Weinhardt, M. Bär, Y. Zhang, B. V. Merinov, D. J. Myers, W. A. Goddard, III, C. Heske Reply to “Comment on ‘Using Photoelectron Spectroscopy and Quantum Mechanics to Determine d-Band Energies of Metals for Catalytic Applications’ ” J. Phys. Chem. C 117 (2013) 6916-6917

68. R. Hofmann The fate of statistical isotropy, Nature Physics 9 (2013) 686-689

69. M. Høj, A. D. Jensen, J.-D. Grunwaldt Structure of alumina sup-ported vanadia catalysts for oxidativedehydrogenation of propane prepared by flame spray pyrolysis, Applied Catalysis A: General 451 (2013) 207-215

70. K. Holliday, K. Dardenne, C. Walther T. Stumpf The incorporation of europium into apatite: a new explanation, Radiochimica Acta 101 (2013) 267-272

71. T. Holubek, S. Casalbuoni, S. Gerstl, A. Grau, D. Saez de Jauregui, W. Goldacker, R. Nast Magnetic Performance of a Laser Structured YBCO Tape Suitable for Insertion Devices Technology, IEEE Trans-actions on Applied Superconductivity 23 (2013) 4602204

72. T. Holubek, T. Baumbach, S. Casalbuoni, S. Gerstl, A. Grau, M. Hagelstein, D. Saez de Jauregui, C. Boffo, W. Walter Towards a Cryogen Free Superconducting Switch, IEEE Transactions on Ap-plied Superconductivity 23 (2013) 3800104

73. A. A. Hummer, P. Heffeter, W. Berger, M. Filipits, D. Batchelor, G. E. Buchel, M. A. Jakupec, B. K. Keppler, A. Rompel X-ray Absorption Near Edge Structure Spectroscopy to Resolve the in Vivo Chem-istry of the Redox-Active Indazolium trans-[Tetrachlorobis(1H-inda-zole)ruthenate(III)] (KP1019), J. Med. Chem. 56 (2013) 1182-1196

74. A. A. Hummer, A. Rompel The use of X-ray absorption and syn-chrotron based micro-X-ray fluorescence spectroscopy to investi-gate anti-cancer metal compounds in vivo and in vitro, Metallomics 5 (2013) 597-614

75. D. Issenmann, N. Wehmeier, S. Eon, H. Bracht, G. Buth, S. Ibra-himkutty, A. Plech Determination of nanoscale heat conductivity by time-resolved x-ray scattering, Thin Solid Films 541 (2013) 28-31

76. D. Issenmann, S. Ibrahimkutty, R. Steininger, J. Göttlicher, T. Ba-umbach, N. Hiller, A-S. Müller, A. Plech Ultrafast laser pump x-ray probe experiments by means of asynchronous sampling, J. Phys.: Conf. Ser. 425 (2013) 092007

77. B. Kallinger, S. Polster, P. Berwian, J. Friedrich, A. N. Danilewsky Experimental verification of the model by Klapper for 4H-SiC ho-moepitaxy on vicinal substrates, J. Appl. Phys. 114 (2013) 183507

78. B. Kallinger, P. Berwian, J. Friedrich, C. Hecht, D. Peters, P. Frie-drichs, B. Thomas SXRT investigations on electrically stressed 4H-SiC PiN diodes for 6.5 kV, Materials Science Forum 740-742 (2013) 899-902

79. S. Kaserer, K. M. Caldwell, D. E. Ramaker, C. Roth Analyzing the Influence of H3PO4 as Catalyst Poison in High Temperature PEM Fuel Cells Using in-operando X-ray Absorption Spectroscopy, J. Phys. Chem. C 117 (2013) 6210-6217

80. S. P. Kilias, P. Nomikou, D. Papanikolaou, P. N. Polymenakou, A. Godelitsas, A. Argyraki, S. Carey, P. Gamaletsos, T. J. Mertzime-kis, E. Stathopoulou, J. Goettlicher, R. Steininger, K. Betzelou, I. Livanos, C. Christakis, K. Croff Bell, M. Scoullos New insights into hydrothermal vent processes in the unique shallow-submarine arc-volcano, Kolumbo (Santorini), Greece, Scientific Reports 3 (2013) 2421

81. J. Klanke, E. Rentschler, K. Medjanik, D. Kutnyakhov, G. Schön-hense, S. Krasnikov, I.V. Shvets, S. Schuppler, P. Nagel, M. Merz, H. J. Elmers Beyond the Heisenberg Model: Anisotropic Ex-change Interaction between Cu-Tetraazaporphyrin Monolayer and Fe3O4(100), Phys. Rev. Lett. 110 (2013) 137202

82. T. Koenig, E. Hamann, S. Procz, R. Ballabriga, A. Cecilia, Zuber, X. Llopart, M. Campbell, A. Fauler, T. Baumbach, M. Fiederle Charge Summing in Spectroscopic X-Ray Detectors with High-Z Sensors,

IEEE Transations on nuclear science 60 (2013) 4713-4718 83. M. Köhl, P. Schroth, A. A. Minkevich, T. Baumbach Retrieving the

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84. M. K. A. Koker, J. Schaab, N. Zotov, E. J. Mittemeijer X-ray diffrac-tion study of the reverse martensitic transformation in NiTi shape memory thin films, Thin Solid Films 545 (2013) 71-80

85. D. Korytár, P. Vagovic, K. Végsö, P. Siffalovic, E. Dobrocka, W. Jark, V. Ác, Z. Záprazný, C. Ferrari, A. Cecilia, E. Hamann, P. Mikulík, T. Baumbach, M. Fiederle, M. Jergel Potential use of V-channel Ge(220) monochromators in X-ray metrology and imaging, J. Appl. Cryst. 46 (2013) 945-952

86. B. Krause, S. Darma, M. Kaufholz, S. Mangold, S. Doyle, S. Ulrich, H. Leiste, M. Stüber, T. Baumbach Composition-dependent struc-ture of polycrystalline magnetron-sputtered V–Al–C–N hard coat-ings studied by XRD, XPS, XANES and EXAFS, J. Appl. Cryst. 46 (2013) 1064-1075

87. S. J. B. Kurz, C. Ensslen, U. Welzel, A. Leineweber, E. J. Mitte-meijer The thermal stability of Ni–Mo and Ni–W thin films: Solute segregation and planar faults, Scripta Mater. 69 (2013) 65-68

88. F. Latteyer, H. Peisert, J. Uihlein, T. Basova, P. Nagel, M. Merz, S. Schuppler, T. Chassé Chloroaluminum phthalocyanine thin films: chemical reaction and molecular orientation, Anal. Bioanal. Chem. 405 (2013) 4895-4904

89. S. Lazarev, M. Barchuk, S. Bauer, K. Forghani, V. Holý, F. Scholz, T. Baumbach Study of threading dislocation density reduction in Al-GaN epilayers by Monte Carlo simulation of high-resolution recip-rocal-space maps of a two-layer system, J. Appl. Cryst. 46 (2013) 120-127

90. S. Lazarev, S. Bauer, T. Meisch, M. Bauer, I. Tischer, M. Barchuk, K. Thonke, V. Holy, F. Scholz, T. Baumbach Three-dimensional recip-rocal space mapping of diffuse scattering for the study of stacking faults in semipolar (1122) GaN layers grown from the sidewall of an r-patterned sapphire substrate, J. Appl. Cryst. 46 (2013) 1425-1433

91. S. Lazarev, S. Bauer, K. Forghani, M. Barchuk, F. Scholz, T. Baum-bach High resolution synchrotron X-ray studies of phase separation phenomena and the scaling law for the threading dislocation den-sities reduction in high quality AIGaN heterostructure, Journal of Crystal Growth 370 (2013) 51-56

92. A. A. Legkodymov, A. V. Bryanskaya, R. Simon, V. Altapova, V. I. Kondratyev, M. R. Mashkovtec, T. E. Aleshina, T. K. Malup, G. N. Kulipanov, S. E. Peltek Optical and X-Ray Imaging Analysis of Chemical Elements Associated with Microbial Communities, Bul-letin of the Russian Academy of Scienes Physics 77 (2013) 1185-1189

93. Y. Li, R. Deng, W. Lin, Y. Tian, H. Peng, J. Yi, B. Yao, T. Wu Electro-static tuning of Kondo effect in a rare-earth-doped wide-band-gap oxide, Phys. Rev. B 87 (2013) 155151

94. J. Li, T. Kleintschek, A. Rieder, Y. Cheng, T. Baumbach, U. Obst, T. Schwartz, P. A. Levkin Hydrophobic Liquid-Infused Porous Polymer Surfaces for Antibacterial Applications, ACS Appl. Mater. Interface 5 (2013) 6704-6711

95. P. Lindqvist-Reis, C. Apostolidis, O. Walter, R. Marsac, N. L. Banik, M. Y. Skripkin, J. Rothe, A. Morgenstern Structure and spectrosco-py of hydrated neptunyl(VI) nitrate complexes, Dalton Transact. 42 (2013) 15275-15279

96. M. W. Löble, P. Oña-Burgos, I. Fernández, C. Apostolidis, A. Mor-genstern, O. Walter, F. Bruchertseifer, P. Kaden, T. Vitova, J. Rothe, K. Dardenne, N. L. Banik, A. Geist, M. A. Denecke, F. Breher Ex-ploring the solution behavior of f-element coordination compounds: a case study on some trivalent rare earth and plutonium complexes, Chem. Sci. 4 (2013) 3717-3724

97. J. Lohmiller, A. Kobler, R. Spolenak, P. A. Gruber The effect of sol-ute segregation on strain localization in nanocrystalline thin films: Dislocation glide vs. grain-boundary mediated plasticity, Appl. Phys.

Appendix




163. P. Vrśanský, T. van de Kamp, D. Azar, A. Prokin, L. Vidlička, P. Vagovič Cockroaches Probably Cleaned Up after Dinosaurs, PLoS ONE 8 (2013) e80560

164. P. Wagener, S. Ibrahimkutty, A. Menzel, A. Plech, S. Barcikowski Dynamics of silver nanoparticle formation and agglomeration in-side the cavitation bubble after pulsed laser ablation in liquid, Phys. Chem. Chem. Phys. 15 (2013) 3068-3074

165. A. Walshe, T. Prüßmann, T. Vitova, and Robert J. Baker An EXAFS and HR-XANES study of the uranyl peroxides [UO2(η

2-O2)(H2O)2]•n-H2O(n= 0, 2) and uranyl (oxy)hydroxide [(UO2)4O(OH)6]•6H2O Dal-ton Transact. DOI:10.1039/c3dt52437j (2013)

166. C. Walther, M. A. Denecke Actinide Colloids and Particles of Envi-ronmental Concern, Chem. Rev. 113 (2013) 995-1015

167. L. Weinhardt, M. Blum, O. Fuchs, S. Pookpanratana, K. George, B. Cole, B. Marsen, N. Gaillard, E. Miller, K.-S. Ahn, S. Shet, Y. Yan, M.M. Al-Jassim, J.D. Denlinger, W. Yang, M. Bär, C. Heske Soft X-ray and electron spectroscopy to determine the electronic struc-ture of materials for photoelectrochemical hydrogen production, J. Electr. Spectr. Rel. Phenom. 190 (2013) 106-112

168. L. Weinhardt, M. Blum, O. Fuchs, A. Benkert, F. Meyer, M. Bär, J. D. Denlinger, W. Yang, F. Reinert, C. Heske RIXS investigations of liquids, solutions, and liquid/solid interfaces, J. Electr. Spectr. Rel. Phenom. 188 (2013) 111-120

169. A. Weisenburger, A. Jianu, S. Doyle, M. Bruns, R. Fetzer, A. Heinzel, M. DelGiacco, W. An, G. Müller Oxide scales formed on Fe–Cr–Al-based model alloys exposed to oxygen containing mol-ten lead, J. Nucl. Mat. 437 (2013) 282-292

170. L. H. E. Winkel, B. Casentini, F. Bardelli, A. Voegelin, N. P. Nikolaid-is, L. Charlet Speciation of arsenic in Greek travertines: Co-precip-itation of arsenate with calcite, Geochimica et Cosmochimica Acta 106 (2013) 99-110

171. Y. Yang, R. Heine, F. Xu, H. Suhonen, L. Helfen, A. Rosenhahn, T. Gorniak, S. Kirchen, T. Schwartz, T. Baumbach Correlative Imaging of Structural and Elemental Composition of Bacterial Biofilms, J. Phys.: Conf. Ser. 463 (2013) 012053

172. S. R. Yeduru, A. Backen, S. Fähler, L. Schultz, M. Kohl Transforma-tion behaviour of freestanding epitaxial Ni–Mn–Ga films, J. Alloys Comp. 577S (2013) 353-357

173. J. B. Yi, N. N. Bao, X. Luo, H. M. Fan, T. Liu, S. Li Ferromagnetism in Cr doped In2O3 , Thin Solid Films 531 (2013) 481-486

174. T. H. Yu, T. Hofmann, Y. Sha, B. V. Merinov, D. J. Myers, C. Hes-ke, W. A. Goddard Finding Correlations of the Oxygen Reduction Reaction Activity of Transition Metal Catalysts with Parameters Obtained from Quantum Mechanics, J. Phys. Chem. C 117 (2013) 26598−26607

175. S. Zabler, A. Ershov, A. Rack, F. Garcia-Moreno, T. Baumbach, J. Banhart Particle and liquid motion in semi-solid aluminium alloys: A quantitative in situ microradioscopy study, Acta Materialia 61 (2013) 1244-1253

176. S. Ziegler, K. Dolch, K. Geiger, S. Krause, M. Asskamp, K. Eus-terhues, M. Kriews, D. Wilhelms-Dick, J. Goettlicher, J. Majzlan, J. Gescher Oxygen-dependent niche formation of a pyrite-dependent acidophilic consortium built by archaea and bacteria, The ISME Journal 7 (2013) 1725-1737

177. F. Zimmermann, S. Richter, A. Plech, S. Döring, M. Hein-rich, M. Steinert, U. Peschel, E.-B. Kley, A. Tünnermann, S. Nolte The underlying structure of ultrashort pulse laser-in-duced nanogratings, Proceedings of SPIE 8611 (2013) 86110Y

other publications, Accelerator proceedings

1. A. Bernhard, E. Huttel, P. Peiffer, A. Bragin, N. Mezentsev, V. Sy-rovatin, K. Zolotarev, P. Ferracin, D. Schoerling Preparations for Beam Tests of a CLIC Damping Wiggler Prototype at ANKA, Pro-ceedings of IPAC2013, Shanghai, China (2013) TUPME005

2. M. Caselle, M. Balzer, S. Cilingaryan, M. Hofherr, V. Judin, A. Kop-mann, K. ll’in, A. Menshikov, A.-S. Müller, N. J. Smale, P. Thoma, S. Wuensch, M. Siegel, M. Weber Ultra-fast Data Acquisition System for Coherent Synchrotron Radiation Based on Superconducting Terahertz Detectors, Proceedings of IPAC2013, Shanghai, China (2013) WEOBB202

3. N. V. Chukanov, S. M. Aksenov, R. K. Rastsvetaeva, D. I. Belakovskiy, J. Göttlicher, S. N. Britvin, S. Möckel Christofschäferite-(Ce), (Ce,La,-Ca)4Mn2+(Ti,Fe3+)3(Fe3+,Fe2+,Ti) (Si2O7)2O8, a new chevkinite-group mineral from the Eifel area, Germany, Novye dannye o mineralakh (New data on minerals) 47 (2013) 33-42

4. P. Gamaletsos, A. Godelitsas, E. Dotsika, E. Tzamos, J. Göttli-cher, A. Filippidis Geological Sources of As in the Environment of Greece: A Review, in: The Handbook of Environmental Chemistry DOI 10.1007/698_2013_230 (2013)

5. S. Gerstl, S. Casalbuoni, A. W. Grau, D. Saez de Jauregui, T. Hol-ubek, R. Voutta, R. Bartolini, M. P. Cox, E. C. Longhi, G. Rehm, J. C. Schouten, R. Walker, M. Migliorati, B. Spataro Beam Heat Load Measurements with COLDDIAG at the Diamond Light Source, Pro-ceedings of IPAC2013, Shanghai, China (2013) WEPWA006

6. T. Goetsch, J. Feikes, M. Ries, G. Wüstefeld, A.-S. Müller Life-time Studies at Metrology Light Source and ANKA, Proceedings of IPAC2013, Shanghai, China (2013) MOPEA012

7. A. Grau, S. Casalbuoni, S. Gerstl, N. Glamann, T. Holubek, D. Saez de Jauregui First tests with a local and integral magnetic field measure-ment setup for conduction cooled superconducting undulator coils, Proceedings of IPAC2013, Shanghai, China (2013) WEPWA007

8. D. Haas, W. Mexner, T. Spangenberg, H. Pasic Implementation of an overall data management at the tomography station at ANKA, ICALEPS2013 (2013)

9. S. Hillenbrand, A.-S. Müller, R. W. Assmann Considerations for a Higgs Facility Based on Laser Wakefield Acceleration, IPAC’13, Shanghai, China (2013) 1643-1645

10. S. Hillenbrand, V. Judin, A.-S. Müller, R. W. Assmann, O. Jansen, A. Pukhov Study of Laser Wakefield Accelerators as Injectors for Synchrotron Light Sources, IPAC’13, Shanghai, China (2013) 2519-2521

11. N. Hiller, A. Borysenko, E. Hertle, E. Huttel, V. Judin, B. Kehrer, S. Marsching, A.-S. Müller, M. J. Nasse, A. Plech, M. Schuh, N. J. Smale, B. Steffen, P. Peier, V. Schlott Electro-optical bunch length measurements at the ANKA storage ring, Proceedings of IPAC2013, Shanghai, China (2013) MOPME014

12. V. Judin, A.-S. Müller, M. Schwarz, M. Klein Bursting Patterns of Coherent Synchrotron Radiation in the ANKA Storage Ring, Pro-ceedings of IPAC2013, Shanghai, China (2013) WEPEA011

13. B. Kehrer, A. Borysenko, E. Hertle, N. Hiller, E. Huttel, V. Judin, S. Marsching, A.-S. Müller, M. J. Nasse, M. Schuh Numerical wake-field calculations for electro-optical measurements, Proceedings of IPAC2013, Shanghai, China (2013) MOPME015

14. W. Mexner, D. Ressmann, T. Spangenberg, H. Pasic, E. Iurchenko A New Flexible Integration of NeXus Datasets to ANKA by Fuse File Systems, Proceedings of ICALEPCS 2013 (2013) TUPPC008

15. T. F. Morgeneyer, L. Helfen, F. Hild Feasibility Study of 3D Digital Volume Correlation of Synchrotron Radiation Laminography Data for Displacement Field Measurement During Ductile Crack Initia-tion, in: Imaging Methods for Novel Material 3 (2013) 211-215

16. A.-S. Müller Short-pulse operation of storage ring light sources, Proceedings of IPAC2013, Shanghai, China (2013) TUXB201

17. A.-S. Müller, V. Judin, M. Balzer, M. Caselle, N. Hiller, M. Hofherr,

from the metal and ligand point of view, J. Phys.: Conf. Ser. 430 (2013) 012115

132. J. Rabeah, M. Bauer, W. Baumann, A. E. C. McConnell, W. F. Ga-brielli, P. B. Webb, D. Selent, A. Bruckner Formation, Operation and Deactivation of Cr Catalysts in Ethylene Tetramerization Directly Assessed by Operando EPR and XAS, ACS Catal. 3 (2013) 95-102

133. A. Rack, F. García-Moreno, L. Helfen, M. Mukherjee, C. Jiménez, T. Rack, P. Cloetens, J. Banhart Hierarchical radioscopy using poly-chromatic and partially coherent hard synchrotron radiation, Appl. Opt. 52 (2013) 8122-8128

134. R. Rehm, M. Masur, J. Schmitz, V. Daumer, J. Niemasz, T. Vandervelde, D. DeMeo, W. Luppold, M. Wauro, A. Wörl, F. Rutz, R. Scheibner, J. Ziegler, M. Walther InAs/GaSb superlattice infrared detectors, Infrared Physics & Technology 59 (2013) 6-11

135. I. Reiche, K. Muller, M. Alberic, O. Scharf, A. Wahning, A. Bjeoumik-hov, M. Radtke, R. Simon Discovering Vanished Paints and Nat-urally Formed Gold Nanoparticles on 2800 Years Old Phoenician Ivories Using SR-FF-MicroXRF with the Color X-ray Camera, Anal. Chem. 85 (2013) 5857-5866

136. P. Reischig, L. Helfen, A. Wallert, T. Baumbach, J. Dik High-reso-lution non-invasive 3D imaging of paint microstructure by synchro-tron-based X-ray laminography, Appl. Phys. A 111 (2013) 983-995

137. K. Rink, U. Oelfke, M. Fiederle, M. Zuber, T. Koenig Investigating the feasibility of photon-counting K-edge imaging at high x-ray flux-es using nonlinearity corrections, Med. Phys. 40 (2013) 101908

138. K. Rink, T. Koenig, M. Zuber, A. Zwerger, A. Fauler, M. Fiederle, U. Oelfke Saturation effects of CdTe photon counting detectors under high photon fluxes, J. Instr. 8 (2013) C01026

139. A. Roschger, J.G. Hofstaetter, B. Pemmer, N. Zoeger, P. Wobraus-chek, G. Falkenberg, R. Simon, A. Berzlanovich, H. W. Thaler, P. Roschger, K. Klaushofer, C. Streli Differential accumulation of lead and zinc in double-tidemarks of articular cartilage, Osteoarthritis and Cartilage 21 (2013) 1707-1715

140. J. Rothe, B. Brendebach, C. Bube, K. Dardenne, M. A. Denecke, B. Kienzler, V. Metz, T. Prüßmann, K. Rickers-Appel, D. Schild, E. Soballa, T. Vitova Characterization of U(VI)-phases in corroded ce-ment products by micro(µ)-spectroscopic methods, J. Phys.: Conf. Ser. 430 (2013) 012114

141. S. Saouane, G. Buth, F. P. A. Fabbiani Crystal structure and pack-ing energy calculations of (+)-6-aminopenicillanic acid, Acta Crys-tallographica Section C 69 (2013) 1238-1242

142. C. Schenk, F. Henke, A. Schnepf [Ge12{FeCp(CO)2}8{FeCp(CO)}2]: A Ge12 Core Resembles the Arrangement of the High-Pressure Modification Germanium (II), Angew. Chem. Int. Ed. 52 (2013) 1834-1838

143. R. Schoch, W. Desens, T. Werner, M. Bauer X-ray Spectroscopic Verification of the Active Species in Iron-Catalyzed Cross-Coupling Reactions, Chemistry - A European Journal 19 (2013) 15816-15821

144. F. Scholz, K. Forghani, M. Klein, O. Klein, U. Kaiser, B. Neuschl, I. Tischer, M. Feneberg, K. Thonke, S. Lazarev, S. Bauer, T.Baum-bach Studies on Defect Reduction in AlGaN Heterostructures by Integrating an In-situ SiN Interlayer, Japanese Journal of Applied Physics 52 (2013) 08JJ07

145. M. Schroeder, S. Glatthaar, H. Geßwein, V. Winkler, M. Bruns, T. Scherer, V. Sai Kiran Chakravadhanula, J. R. Binder Post-doping via spray-drying: a novel sol–gel process for the batch synthesis of doped LiNi0.5Mn1.5O4 spinel material, J. Mater. Sci. 48 (2013) 3404-3414

146. K. C. Sekhar, S. Levichev, K. Kamakshi, S. Doyle, A. Chahboun, M. J. M. Gomes Effect of rapid thermal annealing on texture and properties of pulsed laser deposited zinc oxide thin films, Materials Letters 98 (2013) 149-152

147. P. Seredin, V. Kashkarov, A. Lukin, Y. Ippolitov, R. Julian S. Doyle Local study of fissure caries by Fourier transform infrared microsco-py and X-ray diffraction using synchrotron radiation, J. Synchrotron Rad. 20 (2013) 705-710

148. Y. Shen, T. F. Morgeneyer, J. Garnier, L. Allais, L. Helfen, J. Crépin

Three-dimensional quantitative in situ study of crack initiation and propagation in AA6061 aluminum alloy sheets via synchrotron lami-nography and finite-element simulations, Acta Materialia 61 (2013) 2571-2582

149. T. Slobodskyy, P. Schroth, A. Minkevich, D. Grigoriev, E. Fohtung, M. Riotte, T. Baumbach, M. Powalla, U. Lemmer, A. Slobodskyy Three-dimensional reciprocal space profile of an individual nano-crystallite inside a thin-film solar cell absorber layer, J. Phys. D: Appl. Phys. 46 (2013) 475104

150. D. Soltermann, M. Marques Fernandes, B. Baeyens, R. Dähn, J. Miehé-Brendlé, B. Wehrli, M. H. Bradbury Fe(II) Sorption on a Syn-thetic Montmorillonite. A Combined Macroscopic and Spectroscopic Study, Environ. Sci. Technol. 47 (2013) 6978-6986

151. B. K. Tanner, J. Wittge, P. Vagovic, T. Baumbach, D. Allen, P. J. Mc-Nally, R. Bytheway, D. Jacques, M. C. Fossati, D. K. Bowen, J. Ga-ragorri, M. R. Elizalde, A. N. Danilewsky X-ray diffraction imaging for predictive metrology of crack propagation in 450-mm diameter silicon wafers, Powder Diffraction 28 (2013) 95-99

152. P. Thoma, J. Raasch, A. Scheuring, M. Hofherr, K. Ilin, S. Wünsch, A. Semenov, H.-W. Hübers, V. Judin, A.-S. Müller, N. Smale, J. Hänisch, B. Holzapfel, M. Siegel Highly Responsive Y–Ba–Cu–O Thin Film THz Detectors With Picosecond Time Resolution, IEEE Transactions on Applied Superconductivity 23 (2013) 2400206

153. P. Thoma, A. Scheuring, S. Wunsch, K. Il’in, A. Semenov, H. Hu-bers, V. Judin, A.-S., Muller, N. Smale, M. Adachi, S. Tanaka, S. Kimura, M. Katoh, N. Yamamoto, M. Hosaka, E. Roussel, C. Szwaj, S. Bielawski, M. Siegel High-Speed Y–Ba–Cu–O Direct Detection System for Monitoring Picosecond THz Pulses, IEEE Transactions on Terahertz Science and Technology 3 (2013) 81-86

154. M. J. Tobin, L. Puskar, J. Hasan, H. K. Webb, C. J. Hirschmugl, M. J. Nasse, G. Gervinskas, S. Juodkazis, G. S. Watson, J. A. Wat-son, R. J. Crawford, E. P. Ivanova High-spatial-resolution mapping of superhydrophob cicada wing surface chemistry using infrared microspectroscopy and infrared imaging at two synchrotron beam-lines, Journal of Synchrotron Radiation 20 (2013) 482-489

155. M. Ukrainczyk, J. Stelling, M. Vuĉak, T. Neumann Influence of eti-dronic acid and tartaric acid on the growth of different calcite mor-phologies, Journal of Crystal Growth 369 (2013) 21-31

156. P. Vagovic, D. Korytár, A. Cecilia, E. Hamann, L. Švéda, D. Pellic-cia, J. Härtwig, Z. Zápražný, P. Oberta, I. Dolbnya, K. Shawney, U. Fleschig, M. Fiederle, T. Baumbach High-resolution high-efficiency X-ray imaging system based on the in-line Bragg magnifier and the Medipix detector, J. Synchrotron Rad. 20 (2013) 153-159

157. A. Vasilescu, B. Constantinescu, C. Chiojdeanu, D. Stan, R. Simon, D. Ceccato, A. Simon, Z. Kertesz, Z. Szikszai, I. Uzoniy, L. Csedre-ki, E. Furu Elemental characterization of bronze age copper objects by micro-beam measurements, Romanian Reports in Physics 65 (2013) 1222-1233

158. P. Verboven, E. Herremans, L. Borisjuk, L. Helfen, Q. Tri Ho, H. Tschiersch, J. Fuchs, B. M. Nicola, H. Rolletschek Void space in-side the developing seed of Brassica napus and the modelling of its function, New Phytologist 199 (2013) 936-947

159. V. Veselská, J. Majzlan, E. Hiller, K. Petková, L. Jurkovic, O. Ďurža, B. Voleková-Lalinská Geochemical characterization of arsenic-rich coal-combustion ashes buried under agricultural soils and the re-lease of arsenic, Applied Geochemistry 33 (2013) 153-164

160. T. Vitova, M. A. Denecke, J. Göttlicher, K. Jorissen, J. J. Kas, K. Kvashnina, T. Prüßmann, J. J. Rehr, J. Rothe Actinide and lantha-nide speciation with high-energy resolution X-ray techniques, J. Phys.: Conf. Ser. 430 (2013) 012117

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Appendix




K.S. Ilin, B. Kehrer, S. Marsching, S. Naknaimueang, M.J. Nasse, J. Raasch, A. Scheuring, M. Schuh, M. Schwarz, M. Siegel, N.J. Smale, J. Steinmann, P. Thoma, M. Weber, S. Wuensch Studies of bunch-bunch interactions in the ANKA storage ring with coherent synchrotron radiation using an ultra-fast terahertz detection system, Proceedings of IPAC2013, Shanghai, China (2013) MOPEA019

18. S. Naknaimueang, E. Huttel, S. Marsching, A-S. Muller, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schuh, M. Schwarz, M. Weber, P. Wesolowski, M. Schmelling Simulating the Bunch Structure in the THz Source FLUTE, IPAC’13, Shanghai, China (2013) 2141-2143

19. S. Naknaimueang, V. Judin, S. Marsching, A-S. Müller, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schuh, M. Schwarz, M. Weber, P. Wesolowski Design Studies for FLUTE, a linac-based source of Terahertz radiation, Proceedings of FEL2013 New York (2013) WEPSO44

20. M. J. Nasse, E. Huttel, S. Marsching, A.-S. Müller, S. Naknaimueang, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schuh, M. Schwarz, P. Wesolowsk, R. W. Assmann, M. Felber, K. Flottmann, M. Hoffmann, H. Schlarb, H.-H. Braun, R. Ganter, L. Stingelin FLUTE: A Versatile Linac-based THz Source Generating Ultra-short Pulses, IPAC’13, Shanghai, China (2013) 2147-2149

21. P. Schönfeldt, N. Hiller, V. Judin, A.-S. Müller, M. Schwarz, J. Stein-mann Comparison of different approaches to determine the burst-ing threshold at ANKA, Proceedings of IPAC2013, Shanghai, China (2013) MOPEA020

22. M. Schuh, E. Huttel, S. Marsching, A.-S. Mueller, S. Naknaimueang, M. J. Nasse, R. Rossmanith, R. Ruprecht, M. Schreck, M. Schwarz, M. Weber, P. Wesolowski, R. W. Assmann, K. Floettmann, H. Schlarb RF Bunch Compression Studies for FLUTE, IPAC’13, Shanghai, China (2013) 2144-2146

23. N. J. Smale, E. Hertle, E. Huttel, W. Mexner, A. Müller, S. Mar-sching, I. Kriznar The ANKA Control System: On a path to the Fu-ture, ICALEPS 2013 (2013)

24. P. Thoma, V. Judin At the Limits: How to Detect Relativistic Elec-trons? Real-time measurement of picosecond terahertz pulses at synchrotrons, Optik & Photonik 8 (2013) 58-61

25. P. Ungelenk, M.Höner, H. Huck, M. Huck, S. Khan, R. Molo, A. Schick, N. Hiller, V. Judin Temporal and spectral observation of laser-induced THz radiation at DELTA, Proceedings of IPAC2013, Shanghai, China (2013) MOPEA014

26. T. van de Kamp, A. Ershov, T. dos Santos Rolo, A. Riedel, T.Baum-bach Insect Imaging at the ANKA Synchrotron Radiation Facility, Entomologie heute 25 (2013) 147-160

27. C. Widmann, V. Afonso Rodriguez, A. Bernhard, N. Braun, B. Härer, O. Jäckel, M. Nicolai, P. Peiffer, M. Reuter, T. Rinck, R. Rossmanith, A. Sävert, M. Scheer, W. Werner, T. Baumbach, M. C. Kaluza Non-linear Beam Transport Optics for a Laser Wakefield Accelera-tor, Proceedings of IPAC2013, Shanghai, China (2013) TUPWO013

28. X. Yang, T. Jejkal, H. Pasic, R. Stotzka, A. Streit, J. van Wezel, T. dos Santos Rolo Data Intensive Computing of X-Ray Computed Tomography Reconstruction at the LSDF, 21st Euromicro Interna-tional Conference on Parallel, Distributed and Network-Based Pro-cessing (PDP) DOI 10.1109/PDP.2013.21 (2013) 86-93

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