research with synchrotron radiation - desy · 2-aug-06 e. weckert: research with synchrotron...
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 1
Research with Synchrotron Radiation
Edgar Weckert
• Introduction: what is synchrotron radiation ?
• Radiation sources at DESY
• Interaction of radiation with matter
• Experiments at Storage Rings
- Diffraction/Scattering
- Spectroscopy
- Imaging
• Experiments at Free Electron Lasers
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Spektrum einerWolfram Röntgen-Röhre
wide spectral range
high intensity
pulsed
polarised
time
wiggler / undulators
strongly collimated
Production of synchrotronRadiation:
Opening angle:
Bending magnet: Undulator:
γ= E/mec2
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Bending magnets / Wigglers (60’s)
I ∝ nm × ne
Undulators (60’s)
I ∝ nm2 × ne
Free-electron-lasers FEL (70’s)
I ∝ nm2 × ne
2
e-
e-
e-
Production of synchrotron radiation
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Wiggler at DORIS III
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The SASE-principle for free electron lasers
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Characteristics of FEL radiation
• 1012-1013 photons/pulse• 100 fs pulse length• intrinsic energy resolution: 0.1%• from single pulse to ~40000 pulses/s
FEL:
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DORIS III38 beamlines
PETRA III13 beamlines
XFEL
VUV-FEL
Photon Facilities at DESY
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Photon Facilities at DESY
DORIS III VUV-FEL
PETRA II/III XFEL
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Source Properties
FELs
PETRA III
DORIS III
PhotonsProperties:- high brilliance and flux- infrared up to hard X-rays (>100keV)- polarization- time structure
Applications:- spectroscopy- diffraction/scattering- imaging
Fields:- solid state physics- crystallography- structural biology- chemistry/catalysis- geo-/environmental science- materials science, nano science- medical science- atoms, molecules and clusters- magnetism- engineering science
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Radiation source properties:• flux: F [ph/(s 0.1%BW)]
• brilliance: B=F/((2π)2σTxσTx’σTyσTy’) [ph/(s mm2mrad20.1%BW)]
• coherent flux: Fc = B(λ/2)2 [ph/(s 0.1% BW)]λ: wavelength; σTx: photon source size; σTx’: photon source divergence
Electron beam properties:
• horizontal emittance: εx = σx·σx’ ~ E2/NB3; NB: No. of B-Magnets
• vertical emittance: εy = σy·σy’ = κ·εx; κ: horiz./vert. couplingσx: electron beam size; σx’: electron beam divergence
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Beamlines at DORIS III
38 beamlines, 70 experimental stations
11 Stations operated by external organizations:- EMBL: 7 - MPG: 1 - GKSS: 1- GFZ: 2
16 stations operated with supportfrom external institutions: - BMBF-Verbundforschung- FZ Jülich- University Hamburg- University Kiel- University Aachen- Debye Inst. Utrecht- RISØ- MPI Golm
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http://petra3.desy.de
The PETRA-III Project
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PETRA III Project
P
Parameters:- rebuild of 1/8 of PETRA- refurbishment of 7/8 of PETRA- energy: 6 GeV- current: 100 mA- emittance: 1 nmrad- undulators: 14- undulator length: 2, 5, 20 m- top up operation mode
Brilliance Comparison
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20 m undulator
Labs and offices
ID-sectors
max. BL-length 103 m (from the source)
9 straight sectionsseparation: 5°
Use of canted undulators(5 mrad, 2 m device length):
14 separate undulator BLs
Sector 1
Sector 9A/B
Sector 2 Sector 3A/B
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23 m
Canted undulators beam separation 5 mrad
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FLASH user facility
100 μm
20 μm/unfocused
10 μm
VLS gratingspectrometer
high resol. PGMmonochromator
opticallaser
100 μmmicrofocus
20 m
~42 m to undulatorGas absorber
intensity monitor(gas ionization)
Start of userOperation: 2005 superconducting linac: 1 GeV
minimal wavelength: 6nmfive experimental platforms with different focal spots/optics
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VUV-FEL
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VUV-FEL
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PG2BL1
BL3
BL2visible laser light
FLASH experimental hall
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European XFEL Project
More than 1000 scientists contributed to the Technical Design Report
The XFEL part is based on8 workshops with190 participants
stand alone facility
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XFEL: Schematic Layout
injector
Linear accelerator in superconducting TESLA technology
Electron beam switchyardwith undulators
expe
rimen
tal h
all
Linac: 20GeVmin. wavelength: ~1Åphotons per pulse: ~1012
pulse length: ~100fs
2 X-ray SASE FELs, 1 SASE XUV-FELs, and 2 beamlines for short pulse
physics using spontaneous radiation
10 experimental stations
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XFEL Accelerator Tunnel
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XFEL Site Schenefeld
phase II
phase I
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Experiments building, Nov 2004
Experimental Hall of the 0.1 nm European X-ray FEL Project
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DESY site: Injector complex, infra-structure
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Interaction of electromagnetic radiation with matter
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Structural Biology at DORIS IIIBeamlines and experimental stationsfor structural biology are operatedby the EMBL and MPG outstation:
EMBL:• in total 5 stations for proteincrystallography (PX)
• biological EXAFS• biological SAXS• one PX station in collaboration
with German universities• serving the community by anumber of training activities
MPG:• one beamline for protein crystallography
• three groups for structural biology
Protein crystallography
EXAFS
s, nm-1 0 1 2 3 4
lg I, relative
1
2
3 (1)(2)(3)(4)
His110
N
NH
N
NH
NHN
O
O
O
NHN
ZnOH
ZnO NH
NHis56
His54 Asp58
His59
His173Asp134
SAXS
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Macromolecules
Polychromatic
Monochromatic
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Macromolecules: representations
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Important macromolecular structure
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Extremely large complexes (virus)
J.M. Grimes, J.N. Burroughs, P. Guet, J.M. Diprose, R. Malby, S. Zientra, P. Mertens, D.I. Stuart, Nature, 395, 470-478 (1998)
example: Blue Tongue Virus
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e.g. due to radiation damage
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Powder Diffraction
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Technische Universität Darmstadt Material- und Geowissenschaften
Schematic setup of the powder diffractometer at B2
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Technische Universität Darmstadt Material- und Geowissenschaften
Multidetector concept for high resolution studies
W.-H. Kaps
J. Ihringer
W. Prandl
…
Detektor 4Detektor 3
Detektor 2
Detektor 1
Si(111) Analysator
Blenden
SpiegelMonochromator
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Powder Diffraction
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Texture Analysis
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Materials science
Energy range: 50-100 keV; 5cm in Al
Grain properties to be determined: position, morphology, orientation, deformation (plastic/elastic), composition
Achievable resolution: 1.5 x 5 x 50 μm3
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Diffraction with nm spatial resolution
Investigation of the strain of SiO2 on Si
Focussing by wave guides
S. Di Fonzo et al. Nature, 403, 638 (2000)
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SurfaceDiffraction
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 53
Surface Diffraction
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 54
Diffraction from interfaces: Structure close to thesolid-liquid interface
System: Si(001)-Pb(liquid; TM+10K)
Energy: ~80 keV
H. Reichert et al., Nature, 408, 839 (2000)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 55
Diffractionfromliquids
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 56
Small Angle Scattering (SAXS)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 57
USAXS (4000Å)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 58
Micro SAXS
Orientation of microfibrils in wood cells.
Spatial resolution: 2 μm
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 59
Micro focus applications (SAXS)
I. Dobbie, M. Linari, G. Piazzesi, M. Reconditi, N. Koubassova, M.A. Ferenczi, V. Lombardi, M. Irving, Nature, 396, 383-387 (1998)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 60
Intravenous Coronary Angiography
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 61
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 62
Microtomography at HASYLAB/DESY
xy
z
X-ray camera
sample manipulator
CCD camera lens fluorescent screen
monochromaticbeam
sample
optical mirrors
beamstop
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 63
Porous PLGA scaffold(In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland)
µCT at BW2 using 9 keVsample diameter: 5 mm
slice (2 x 2 mm²)spatial resolution: 5.4 µm
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 64
Titania hollow spheres (TiO2)(In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland)
µCT at BW2photon energy: 19 keV
sample height: 1.05 mm
spatial resolution: 2.1 µm
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 65
Titania hollow spheres (TiO2)(In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland)
µCT at BW2
using19 keV
spatial resolution: 2.1 µm
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 66
Absorption micro tomographyParallel radiation, high resolution 2D-detector
example: wetting of Al-grain boundaries by Ga (ESRF ID19)
3D-grain distributionInvestigation of deformed Al
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 67
Phase-contrast Microtomography
xy
z
X-ray camera
sample manipulator
interferometerCCD camera lens fluorescent screenmonochromatic
beam
rotating phase shiftersample in liquid
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 68
Rat trigeminal nerve (PµCT at 12 keV)
nerve fibers (diameter 25 µm)
noticeable density change 1 mg/cm³
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 69
Mouse kidney: µCT and PµCT at 12 keV
µCT: τ ∝ Z4 E-3 ρ PµCT: Φ ∝ σ E-1
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 70
Phase contrast imaging
requirement: lateral partially coherent radiation
Lateral coherence length: ξ ~ λL/sL: distance from the source; s: source size
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 71
Phase contrast images
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 72
Phase contrast tomography
example: SiC in Al:
Micro tomographicreconstructions for different strains.
Energy: 25 keV
Distance sample-detector: 82 cm
P. Cloetens, R. Barret, J. Baruchel, J. Guigay, M. Schlenker, J. Phys. D, 29,133-145 (1996)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 73
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monochromator
I0
I1 I2
sample
reference
Quelle
I (Fluorescence)
experimental set up of X-ray absorption spectroscopy
J. Wienold
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 75
-0.6
-0.7
-0.8
-0.9
-1.020 20.25 20.5 20.75
abso
rptio
n [a
.u.]
photon energy, keV
I = I0*exp(-μd) (Lambert's law)
1750
2000
2250
2500
20 20.25 20.5 20.75
Inte
nsity
, au
Photon energy, keV
Features ofX-ray absorption spectroscopy
μ = linear absorption coefficent
μd = ln(I0/I)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 76
0.00.0
-0.25
-0.5
-0.75
20 20.25 20.5 20.75
abso
rptio
n [a
.u.]
photon energy [keV]XANES (X-Ray Absorption Near Edge Structure)NEXAFS (Near Edge X-Ray Absorption Fine Structure)
EXAFS (Extended X-Ray Absorption Fine Structure)
Regions in the XAS spectra
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 77J.Wienold, Geometrische Strukturen, Abt. AC, Fritz-Haber-Institut(MPG), Berlin, Germany
Fermis Golden rule:
IXAS ~ |<Φf|ê•r| Φi>|2δEf-Ei-ħω
Φi = inital state
Φf= final state= Φoutgoing+ Φbackscattered
ê•r = dipol matrix elementê = electriv field polarisationvector of the photon, r = coordinatevector of the electron
h*ν ⇒ Fluorescence⇒ Auger electrons⇒ Absorption⇒ X-ray emission
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 78
0.00.0
-0.25
-0.5
-0.75
20 20.05 20.1 20.15
abso
rptio
n [a
.u.]
photon energy [keV]
Pre edge (inneratomare Übergänge)
Kantenlage(Valenz)
XANES is, ‘Fingerprint’ of a single material and can be used via Principal Component Analysis(PCA, Faktor Analyse) for quantitative analysis
XANES
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 79
EXAFS
0.00.0
-0.25
-0.5
-0.75
20 20.25 20.5 20.75
abso
rptio
n [a
.u.]
photon energy [keV]
0.0
0.25
0.5
0.75
1.0
0.0
20 20.25 20.5 20.75
norm
. abs
orpt
ion
[a.u
.]
photon energy [keV]
Energie calibration, background substraction,normalization
0.0
0.25
0.5
0.75
1.0
0.0
0 5 10 150-5
norm
. abs
orpt
ion
[a.u
.]
k [Å -1 ]
konversion
( )02 EEmk −=h
0.0
0.25
0.5
0.75
1.0
0.0
0 5 10 150-5
norm
. abs
orpt
ion
[a.u
.]
k [Å -1 ]
μ(k) - μ0(k) μ0(k)χ(k) =
Substraction of μ0
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 80
0.0
2.0
0.0
-2.0
5 7.5 10 12.5
χ(k
)*k
3
k [Å -1 ]
χ(k)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 81
HPGe-detectorMono
capillary
XYZSamplestage
Microscope
SR μ-XRF setup at
Strahl L, HASYLAB,
HamburgHPGe-detector
Monocapillary
XYZSamplestage
Microscope
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 82
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 84
Refractive optics in the X-ray regime
Snigirev et al., Applied Optics 37, 653 (1998)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 85
Micro fluorescence tomography
example: root of mahagoni tree
Lengeler et al. JSR, 6, 1153-1167 (1999)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 86
XPCS (X-ray photon correlation spectroscopy)
requirement: coherent radiation
5-10 μm pinhole to mask the coherent part of the radiation
T. Seydel et al., Phys. Rev. B 63(7), (2001)
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 87
Inelastic scattering under high pressure
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 88
Geo-Science Experiments
1750t press for in situ studies of large sample volumes.pressure: ~25GPatemperature: >2000KOne further similar facility at SPring8.Study of material under the conditions of the earths lower mantle.
Activities of GFZ at DESY
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 89
Inelastic scattering under high pressure
Speed of sound of Fe under pressure (ESRF: 2 ph/min)
G. Fiquet et al., Science (2000)
gasket
sample
diamond
X ray
1 mm
P=28GPa
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 90
VUV-FEL (phase 1)
0 2 4 6 8 10 12 1410-12
10-11
1x10-10
1x10-9
1x10-8
1x10-7
1x10-6
1x10-5
1x10-4
E = Eshexp(z/Lg)Wsh ~ 1-2 W
TTF FEL saturation September 10, 2001λ = 98.1 nmLg = 0.68 mEsat = 90 μJ
E [J
]
z [m]
VUV-FEL (phase 1) in saturation at 98nm
Radiation wavelength 80-125 nmRadiation pulse energy at saturation 30-100 μJRadiation pulse duration (FWHM) 30-100 fsRadiation peak power 1 GWSpectrum width (FWHM) 1%Radiation spot size [FWHM] 200 μmRadiation angular divirgence [FWHM] 260 μradRadiation peak brilliance up to 1029
Number of photons per bunch 1012-13
Achieved performance at VUV-FEL (phase 1):
Undulator length [m] V. Ayvazyan et al., PRL 88(2002)104802
transverse coherence
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 91
VUV-FEL (phase 1) First Experiments
Xe-cluster experimentEphot= 12.8eVEion = 12.1eV
Wabnitz et al., Nature, 420 (2002) 4820 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 6 0 0 7 0 0
0 .0
0 .1
0 .2
0 .3
X e +
inte
nsity
[arb
. uni
ts]
t im e o f f l ig h t [n s ]
a to m
0 .0
0 .1
0 .2
0 .3
0 .4
6 +7 +
X e 3 +
8 +
X e + +
N ~ 2 -2 0
0 .0
0 .1
0 .2
0 .3
0 .4
5 +
4 +
N ~ 8 0
0 .0
0 .1
0 .2
0 .3
0 .4
0 .5
4 23876 5 1
N ~ 3 0 0 0 0
Cluster size dependence
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 92
Silicon Graphite (HOPG)
Results: Time-Resolved Microscopy
K. Sokolowski-Tinten et al.
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 93
multilayer mirror
CCD
15o
-15o
Pulse #1: Diffraction reveals structure before radiation damage occurs
Pulse #2 sees structure destroyed by pulse #1
To beam dump
Incident FEL pulse: 30 fs, 32 nm, 3 x 1013 W cm-2
sample
First demonstration of ultrafastcoherent X-ray diffraction
H. Chapman, J. Hajdu et al.
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 94
Schotte et al., Science 300(2003)1944
Example:Time resolved investigation of the photo ionization of CO-myoglobinat ID9 (ESRF):- pump-probe technique- X-ray crystallography
Time resolved investigation
Variable delay betweenlaser pump pulse and X-ray probe pulse.
32 exposures per image
‘pink’ Laue technique,range: 0.72-1.24 Å
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2-Aug-06 E. Weckert: Research with Synchrotron Radiation 96
XFEL: 1000 times better timeresolution than today
Time resolved crystallography
Schotte et al., Science 300(2003)1944