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Transcript of Text optional: Institutsname Prof. Dr. Hans Mustermann Mitglied der Leibniz-Gemeinschaft Member of...
Text optional: Institutsname Prof. Dr. Hans Mustermann www.fzd.de Mitglied der Leibniz-Gemeinschaft Member of the Helmholtz Association
High-Speed PIXEFast Elemental Analysis
with a Colour X-ray Camera
Josef BuchrieglerJ.v. Borany, D. Hanf, S. Merchel, F. Munnik, S.H. Nowak, A.D. Renno, O. Scharf, R. Ziegenrücker
ICNMTA, 11th July 2014, Padova
11th July 2014, Padova 2
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association© Google Earth
Dresden
Padova
Overview
11th July 2014, Padova 3
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Outline
1. Motivation Needs for a new PIXE set-up, Competitive methods
2. Experimental set-upIBC-overview, High-Speed PIXE set-up, SLcam®
3. Data evaluationiXCC-Imager, GeoPIXE
4. First resultsLateral resolution, Trace element detection
5. Summary & Outlook
11th July 2014, Padova 4
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Motivation
Why new analysis methods should be developed?
urgent requirement for resource technology
for exploration, mining, sustainable use and recycling of mineral and metalliferous resources
due to:
rising energy costs
increasing environmental protection
requirements
declining quality of geogenic resources
growing demand for metalliferous raw
materials Source: Stephen Codrington
11th July 2014, Padova 5
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Motivation
How new analysis methods should be developed?
Foundation of Helmholtz Institute Freiberg for Resource Technology (in June 2011): joint venture between TU Bergakademie Freiberg & Helmholtz-Zentrum Dresden-Rossendorf
aim of the new institute:
research of new technologies designed
for:
utilize resources more efficiently
assure supply of raw materials
environmentally friendly
technologies
11th July 2014, Padova 6
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Motivation
Why a new PIXE analysis method should be developed?
Analytical chain for chemical analysis at Helmholtz Institute Freiberg:
fast
• X-ray fluorescence (XRF)• Mineral liberation analyser (MLA)
• Electron microprobe analyser (EPMA)• High-Speed PIXE lower background
• Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)*
• Ion microprobe (RBS, ERDA, PIXE, PIGE, NRA)
sensitiv
• Accelerator mass spectrometry (AMS)• Super-SIMS*
* under construction
11th July 2014, Padova 7
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Motivation
How High-Speed PIXE can be competitive?
fast laterally resolved elemental information
high sensitivity for trace elements (concentrations < 0.1 at.%)
high throughput
large/heavy samples
grain size determination, intergrowth analysis, etc.
High-SpeedPIXE
novel combination of
PIXE as analytical method
position sensitive detector pixel-detector
X-ray optics polycapillaries
fast data acquisition system
established evaluation software GeoPIXE
11th July 2014, Padova 8
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Experimental set-up
Ion Beam Center overview
Proton beam
Scanningsystem
Beam diagnosticchamber
Sample chamber
SLcam®
Dataacquisition
approximately 90 m from ion source to sample surface
2 – 4 MeV protons
up to 1 µA current
un-scanned spot-
size: 0.25 × 1.00
mm²
Opticalmicroscope
Quadrupole
11th July 2014, Padova 9
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Experimental set-up
High-Speed PIXE set-up
A. Renno, D. Hanf, O. Scharf
Proton beam
Scanningsystem
Beam diagnosticchamber
Sample chamber
SLcam®
Dataacquisition
Opticalmicroscope
Quadrupole
25 cm
11th July 2014, Padova 10
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Experimental set-up
Classical µ-beam set-up
Object50x50 μm2
Aperture1x1 mm2
Lens
Sample surfaceHigh-energyproton beam
(3 µA)
focused beam (1-5 µm) and scan across sample big detector as close as possible to sample
proton currenton sample: 0.5 nA
Sample surface
High-energyproton beam
(<1 µA)
broad beam use of pixel detector (pnCCD) local fields of view defined by suitable X-ray optics combining X-ray optics and pnCCD:
laterally resolved PIXE images
New approach: position sensitive detector & X-ray optics
Detector
X-ray g
uidance
11th July 2014, Padova 11
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Experimental set-up
Functional principle
sample surface tilted by 15°:
undistorted PIXE images
high X-ray yield
two types of polycapillary optics:
1. straight capillaries high depth of focus
2. conical capillaries 6:1 magnification
Ø 19 mm
82 mm
1.2 mm
11th July 2014, Padova 12
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Experimental set-up
SLcam®
12 cm
Name Value
number of pixel 264 × 264 = 69 696
pixels size 48 × 48 µm²
image area 12 × 12 mm²
frame rate 1000 Hz
sensitive energy range 2 – 20 keV
active sensor thickness 450 µm
energy resolution 152 keV @ Mn Kα
quantum efficiency>95% @ 3-10 keV>30% @ 20 keV
window 50 µm Be
X-ray opticsparallel (76 mm, 1:1)conical (82 mm, 6:1)
11th July 2014, Padova 13
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Data evaluation
iXCC-Imager: real-time data analysis (IFG X-Ray Colour Camera)
Geological sample “Kischa” (S04):70 minutes @ ~300 nA 22×106 events
11th July 2014, Padova 14
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Data evaluation
iXCC-Imager: real-time data analysis (IFG X-Ray Colour Camera)
~4 cm
Ti Kα Ca KβCl KαK KαMn KαSi Kα
12 mm
11th July 2014, Padova 15
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Data evaluation
Limits of iXCC-Imager: Overlapping peaks
Intensity
106
105
104
103
0 4 8 12 16 20 keV Energy
Geological sample “Columbite” (S20):4.5 hours @ ~300 nA 113×106 events
12 mm
11th July 2014, Padova 16
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Data evaluation
GeoPIXE: Established evaluation software for geological samples
Quantitative evaluation:• detector properties• sample properties (matrix)• corrections for the optics• X-ray line model• background model• pileup correction
Deconvolution of spectra
12 mm
GeoPIXE
iXCC
11th July 2014, Padova 17
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
First results
Visual lateral resolution
Visual lateral resolution ~67 µm
intensity along green line
Measurement of known structures:
67 µm Cu-stripes on Si-waferspacing: 200 / 135 / 67 µm
Px
Cu-stripes (S08):97 minutes @ ~500 nA 363×106 events
pixel
3 mm
11th July 2014, Padova 18
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
“Cr on Si” (S16):75 minutes @ ~400 nA 120×106 events
Sigmoid fits
Calculated lateral resolution
intensity perpendicular to Cr-edge
Cr-pattern on Si-wafer
First results
Line-Nr. Edge position Width (0.12-0.88)
67 95.09 0.9
68 95.21 1.3
69 95.08 1.4
70 95.00 1.5
71 94.96 0.9
72 94.93 1.5
73 94.79 2.3
74 94.79 1.4
75 94.81 2.2
76 94.92 2.2
77 94.86 1.7
78 94.71 1.6
Mean (94,93±0,15) px (1,58±0,47) px
Calculated lateral resolution: (76±23) µm
pixel
11th July 2014, Padova 19
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
First results
Cassiterite (Tin Stone)proton energy: 3 MeVcurrent: ~ 700 nAmeas. time: ~ 45 min
Ta-Lα concentration map (<0.1 at.%)
Trace element detection in geological samples
11th July 2014, Padova 20
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Summary & Outlook
Summary
new PIXE set-up built at HZDR novel combination of SLcam® and PIXE motivation: resource technology comparison with competitive methods first assessment of lateral resolution promising results with trace elements
Outlook
o quantitative evaluation accurate fluence monitoring
o automation
o windowless operation lighter elements (Z<16)
o full integration of GeoPIXE:
concentration maps in real-time
11th July 2014, Padova 21
Josef Buchriegler | Institute of Ion Beam Physics and Materials Research | www.hzdr.de/iba | [email protected]
Member of the Helmholtz Association
Acknowledgements
This work is supported by Marie Curie Actions - Initial Training Networks (ITN) as an Integrating Activity Supporting Postgraduate Research with Internships in Industry and Training Excellence
(SPRITE) under EC contract no. 317169
Helmholtz-Zentrum Dresden-Rossendorf, Dresden
Shavkat Akhmadaliev
Johannes von Borany
Daniel Hanf
Silke Merchel
Frans Munnik
Axel Renno
René Ziegenrücker
Operator team
IFG Institute for Scientific Instruments, Berlin
Stanisław H. Nowak
Oliver Scharf
Thank you for your attention !