DUBBLE @ ESRF Netherlands Organisation for Scientific ... · Meet the Röntgens So you think this...
Transcript of DUBBLE @ ESRF Netherlands Organisation for Scientific ... · Meet the Röntgens So you think this...
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Wim BrasDUBBLE @ ESRFNetherlands Organisation for Scientific Research (NWO)
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Outline
• Short introduction synchrotron radiation• European Synchrotron Radiation Facility• European Synchrotron Radiation Facility• DUBBLE• Examples of research on Dubble
Commercial possibilities indicated in Italics
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Meet the RöntgensSo you think this is funny mr Röntgen?
I’ll kick him out of my school.
Prof. Conrad RöntgenFirst Nobel price winner1845 - 19231848-1865 Apeldoorn
Mrs. Röntgen1864
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How do we conventionally generate X-rays?
• With an X-ray generator
• Synchrotron radiation
Panalytical Almelo
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“Conventional” X-ray tube
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Synchrotron radiation
• X-rays generated by fast moving electrically charged particles forced to electrically charged particles forced to change their direction
• Natural phenomenon
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Crab Nebula: Blue stuff is SR
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‘slow’ electrons(dipole radiation)(think of antenna)
‘fast’ electrons
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1947
Why would General electric be interested……?
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1953
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Family treeCERN
1936
ESRF
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Magnet lattice
Undulator or insertion device
Bending magnet
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Synchrotron radiation sourcesBending magnet
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What is the advantage of SR?
• High flux• Continues spectrum
1013
1014
1012
10000 1000 100 10 1 0.1
Wavelength (Å)Numberof photons
• Good collimation• Beams 1 – 300 micron
1 eV 10 eV 100 eV 1 keV 10 keV 100 keV
Energy
109
1010
1011
108
107
sunlight conventional X-ray generator
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Boessenkool BV Almelo
undulator
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Synchrotron labs
• These labs are set up as user facilities• They are relatively large scale• Belgium and the Netherlands have • Belgium and the Netherlands have
made the choice to participate in international facilities
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Dutch ESRF participation
• 6% of the experimental time on public beam lines is for the Benesync consortium (50/50 Be/Nl)
• This is not sufficient for the Dutch/Belgian • This is not sufficient for the Dutch/Belgian demand for some techniques
• Two ‘own’ beam lines• DUBBLE (part of the Dutch research
infrastructure)
• 6% of ESRF expenditure should be in Belgium-Netherlands
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European Synchrotron Radiation Facility
Grenoble France
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European Synchrotron Radiation Facility
• ∼ 50 beam lines (= experimental set ups)
• ∼ 25 different techniques• 6 days/ week, 24 hours/day• 6 days/ week, 24 hours/day• 270 days/year (minus strike days, after all it is
France….)
• ∼ 1500 publications/year
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Many different experiments
Protein crystallographyAbout 25% of the beam linesAbout 35% of publication output
Crystal distortions due to highCrystal distortions due to high(30 Tesla) magnetic fields
Chocolate butter crystallisation
Spider silk
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270 meter
the ESRF
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ESRF accelerator
• 1 km circumference– 1 km high vacuum– 1 km of electronics controls required– 1 km of electronics controls required– 1km of diagnostics of all kinds required– metrology
– Feenstra (Dalfsen), supports for vacuum vessels
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Around 50 experimental stations
• Beam line optics– High vacuum– Fine mechanical engineering– Fine mechanical engineering– Mostly custom built
• Experimental station– Large variety of requirements/sales
opportunities
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X-ray optics
• X-rays come out of machine– Slightly divergent– Polychromatic– Polychromatic
• For most experiments– Requires monochromatic– Requires focusing
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Scheme beam line
storage
Opticsmonochromatorfocussing
experiment
Control cabin
storagering
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Mirror: grazing incidence: focussing
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Conventional mirror
X-ray mirror, Si of semiconductor grade, shallow angles, otherwise absorptionX-ray mirror, Si of semiconductor grade, shallow angles, otherwise absorptionLength up to 1.5 m
roughness < 1.5 Åslope error < 1.5 mradbending radii >15 km
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In real life
Positioning accuracy, angular mrad, linear 2-5 micron, bending very accurate
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Monochromator
• Most often two pieces of silicon
• Positioning accuracy to beam, angular to beam, angular very high
• To each other high– Roll– Yaw– Offset– Pitch
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Monochromator
Some specialized companies existRelatively small market
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Monochromators and mirrors
• High vacuum (10-7 – 10-9)• High radiation environment• Positioning all done remotely• Positioning all done remotely• Positioning all required to be vacuum
compatible and accurate• Cooling issues• Most vacuum vessels custom made
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Sample environment
• Large variation in requirements• Pressure/temperature control• Gas mixtures/controlled flow• Gas mixtures/controlled flow• Stop-flow, temp jump, pH control• Magnetic/electric fields• Deformation rigs
• Etc. etc.
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Sample environments
3.0 m
0.2 m
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Technique combinations
Some experiments:- Raman- Raman- UvVis- Mass Spectrometry- DSC/DTA- Etc. etc
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Sample stages
• Samples + sample environment have to be mounted and positioned
• Fine mechanical engineering• Fine mechanical engineering
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Biochemical research
• Most important single subject of ESRF• Strong connections with pharmaceutical
industry industry • About 25% of ESRF beamlines
dedicated to protein crystallography
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tuberculosis
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Rv2991Rv2428Rv1908c
TB Crystals
Rv3628Rv2610
Rv0813c
Rv2667Rv2883cRv2461c
Rv0877
ML2640
Rv0014c279
Rv2238
Rv0018cRv0014c331
Rv0733
Rv1846c
Rv2276
Rv2438c
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Protein crystallographie
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“=“ Fourier transformof electron density
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Rv2991Rv3247c
tmK
3D Structures
ML2640
Rv2461c clpP
Rv0733adK
Rv0813c
Rv2428ahpC
Rv0014cpknB
adK
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What can we do with this?
• Understanding live cycle of bacteria• Better understanding about action of
antibiotics• Maybe, just maybe, one day, design new
drugs to combat diseases
• If no new drugs have been developed due to PX what is the use now?
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taxolsource
Human tests
Isolation compound
Cell cultures
Animal tests
Finish line:Approval for patients use
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The time path
1962discovery taxol
1992Approved for treatment of
ovarian cancer
Thanks to better understanding of protein structuresnowadays such a time path is reduced to about 15 years
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X-ray scattering
detector1 – 8 meter
sample
X-rays
Diffracted X-rays
2 sindλ θ= θ small d large
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1 limit q → 0electron density
contrastdensity fluctuations
2 Guinier rangeparticle size
SAXS/WAXS
1
1
2
3
4
5
3 particle shape
4 Porod rangeparticle surface
5 Intermolecular/atomicordering
0.2 nm500 nm
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X-ray scattering and diffraction• Combined SAXS-WAXS experiments• WAXS crystalline structure• Small angle: shape and size of clumps of
atoms
• SR not only staticalso time-resolved
• 0.4 – 200 nm ‘visible’
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Multidisciplinary applications
Unwashed Eskimo hair fibrinogen, Car exhaustSoot of diesel
polymer fibersCeramic membranes
Etc., etc., etc….
hip replacements
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SAXS
WAXSmelt
uni-directional
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melt
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The perfect garbage bag
Groepen:P. LemstraH.E.H. Meijer
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Fundamental research with industrial undertones
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1974
A plastic bag
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2011
This bag is 6 x lighter but just as strongas strong6x less oil6x less pollution
This is not irrelevant: we produceenough of this material to cover the earth 3 times/year
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Dutch Polymer Institute support
• To obtain funding also industry support required
• so far 14 postdoc years, 4 PhD years funded• some sale of beam time• even proprietary research largely published
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X-ray spectroscopy
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X-ray spectroscopy
‘electron orbits’
deformed‘electron orbits’
Metal atom
Metal atom
‘neighbours’
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ionisation
Röntgen photon
absorbed ( )0
tIE
I
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Difference in surroundings of metal atom; difference in absorption spectrum
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Incoming intensity
Powder diffraction
absorbed intensity
Sample cell
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Again multidisciplinary
catalysis
pharmaceuticals
liquid metals
electro chemistrycultural heritage
Environmental pollution
Hydrogen storage
Etc., etc., etc….
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Technique combinations
How do I make a working catalyst?
Groep Bert Weckhuijsen, Utrecht (Spinoza price 2013)
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Structure grows
1. Early in reaction, no crystal, X-ray spectroscopy (XAFS)
2. A little later, X-ray diffraction WAXS2. A little later, X-ray diffraction WAXS3. When it has grown sufficient, SAXS4. In the end catalytic activity XAFS,
(UvVis, Raman spectroscopy)
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All these steps one wants to study on-line
• Infrastructure
• Industrially relevant conditionsconditions
• High gas pressure
• Flow
• Operando conditions
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In-situ multi-technique approach of zeolite synthesis
640 660 680
66.7
50
Raman Shift cm-1
Raman XAFS
7700 7800 7900
0.0
0.5
1.0
1.5
B
Nor
mal
ised
Abs
orpt
ion
Energy (eV)
0 20 30 40
A
400 600 800
1.0
1.5
525470
625584
Abs
orba
nce
Wavelength (nm)
*
542
0 .01 0 .1
0 .0000
0 .0008
0 .0016
I(q)
.q3.
3 [a.u
]
log(q) Å -1
UV-VisSAXS
WAXS
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Unique instrumentation
• Sample at high pressure/temperature• Simultaneous 5 techniques possible• Simultaneous 5 techniques possible• All aspects of the sample and kinetics
can be studied simultaneously
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• Follow particle growth• Study the catalytic actions• Follow the life cycle of the
We can:
Catalyst crystals
• Follow the life cycle of the catalyst
All in a single experiment !
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Also very fundamental work
Distortions of crystallinelattices in 30 Tesla pulsed lattices in 30 Tesla pulsed fields
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Dus je wilt de ESRF als klant?
Drie belangrijke zaken
Frans, Frans en Frans
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Dubble: vacuum chamber
Drawings exist: ready for tender
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Bellows: large diameter; edge welded; support structure needed
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Please remember:
-I don’t work for the ESRF-I don’t work for the ESRF- I work for NWO and don’t have much influence on the ESRF buying process
- Sometimes we can help a bit…
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Thanks for your attention