Research with Synchrotron Radiation
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- Patience Boyd
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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 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 1
2 Production of synchrotron Radiation: Opening angle: wiggler / undulators Bending magnet: Undulator: γ= E/m e c 2 strongly collimated polarised pulsed Spektrum einer time Wolfram Röntgen-Röhre high intensity wide spectral range 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 2
3 Production of synchrotron radiation Bending magnets / Wigglers (60 s) Undulators (60 s) I n m n e I n m2 n e e - e - Free-electron-lasers FEL (70 s) I n m2 n e 2 e - 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 3
4 Wiggler at DORIS III 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 4
5 The SASE-principle for free electron lasers 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 6
6 Characteristics of FEL radiation FEL: photons/pulse 100 fs pulse length intrinsic energy resolution: 0.1% from single pulse to ~40000 pulses/s 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 7
7 Photon Facilities at DESY DORIS III 38 beamlines XFEL VUV-FEL PETRA III 13 beamlines 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 8
8 Photon Facilities at DESY DORIS III VUV-FEL PETRA II/III XFEL 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 9
9 Source Properties FELs PETRA III Properties: Photons - high brilliance and flux - infrared up to hard X-rays (>100keV) -polarization - time structure DORIS III 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 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 10
10 Radiation source properties: flux: F [ph/(s 0.1%BW)] brilliance: B=F/((2π) 2 σ Tx σ Tx σ Ty σ Ty ) [ph/(s mm 2 mrad 2 0.1%BW)] coherent flux: F c = B(λ/2) 2 [ph/(s 0.1% BW)] λ: wavelength; σ Tx : photon source size; σ Tx : photon source divergence Electron beam properties: horizontal emittance: ε x = σ x σ x ~E 2 /NB 3 ; NB: No. of B-Magnets vertical emittance: ε y = σ y σ = κ ε y x ; κ: horiz./vert. coupling σ x : electron beam size; σ x : electron beam divergence 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 11
11 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 support from external institutions: - BMBF-Verbundforschung - FZ Jülich - University Hamburg - University Kiel - University Aachen - Debye Inst. Utrecht -RISØ -MPI Golm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 12
12 The PETRA-III Project 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 13
13 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 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 15
14 ID-sectors Sector 1 Sector 2 Sector 3A/B Labs and offices 20 m undulator 9 straight sections separation: 5 Use of canted undulators (5 mrad, 2 m device length): Sector 9A/B 14 separate undulator BLs max. BL-length 103 m (from the source) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 16
15 23 m Canted undulators beam separation 5 mrad 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 17
16 FLASH user facility 20 m 100 μm 20 μm/ unfocused 100 μm micro focus 10 μm VLS grating spectrometer optical laser high resol. PGM monochromator intensity monitor (gas ionization) Start of user Operation: 2005 Gas absorber ~42 m to undulator superconducting linac: 1 GeV minimal wavelength: 6nm five experimental platforms with different focal spots/optics 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 18
17 VUV-FEL 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 20
18 VUV-FEL 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 21
19 FLASH experimental hall BL1 PG2 BL2 BL3 visible laser light 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 23
20 European XFEL Project More than 1000 scientists contributed to the Technical Design Report The XFEL part is based on 8 workshops with 190 participants stand alone facility 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 24
21 XFEL: Schematic Layout injector Linear accelerator in superconducting TESLA technology Electron beam switchyard with undulators experimental hall Linac: 20GeV min. wavelength: ~1Å photons per pulse: ~10 12 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 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 25
22 XFEL Accelerator Tunnel 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 26
23 XFEL Site Schenefeld phase I phase II 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 27
24 Experimental Hall of the 0.1 nm European X-ray FEL Project Experiments building, Nov Aug-06 E. Weckert: Research with Synchrotron Radiation 28
25 DESY site: Injector complex, infra-structure 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 29
26 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 30
27 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 31
28 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 32
29 Interaction of electromagnetic radiation with matter 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 33
30 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 34
31 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 35
32 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 36
33 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 37
34 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 38
35 Structural Biology at DORIS III Beamlines and experimental stations for structural biology are operated by the EMBL and MPG outstation: SAXS lg I, relative 3 (1) (2) (3) (4) 2 EMBL: in total 5 stations for protein crystallography (PX) biological EXAFS biological SAXS one PX station in collaboration with German universities serving the community by a number of training activities s, nm -1 Protein crystallography MPG: one beamline for protein crystallography three groups for structural biology EXAFS His56 His54 HN N H N N Zn N N H O OH O Asp58 O O His59 N Zn NH NH N Asp134 His173 His110 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 39
36 Macromolecules Monochromatic Polychromatic 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 40
37 Macromolecules: representations 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 41
38 Important macromolecular structure 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 42
39 Extremely large complexes (virus) example: Blue Tongue Virus J.M. Grimes, J.N. Burroughs, P. Guet, J.M. Diprose, R. Malby, S. Zientra, P. Mertens, D.I. Stuart, Nature, 395, (1998) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 43
40 e.g. due to radiation damage 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 44
41 Powder Diffraction 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 45
42 Schematic setup of the powder diffractometer at B2 Technische Universität Darmstadt Material- und Geowissenschaften 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 46
43 Multidetector concept for high resolution studies Detektor 3 Detektor 4 Detektor 2 Detektor 1 Si(111) Analysator Blenden Monochromator Spiegel W.-H. Kaps J. Ihringer W. Prandl Technische Universität Darmstadt Material- und Geowissenschaften 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 47
44 Powder Diffraction 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 48
45 Texture Analysis 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 49
46 Materials science Energy range: kev; 5cm in Al Grain properties to be determined: position, morphology, orientation, deformation (plastic/elastic), composition Achievable resolution: 1.5 x 5 x 50 μm 3 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 50
47 Diffraction with nm spatial resolution Investigation of the strain of SiO 2 on Si Focussing by wave guides S. Di Fonzo et al. Nature, 403, 638 (2000) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 51
48 Surface Diffraction 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 52
49 Surface Diffraction 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 53
50 Diffraction from interfaces: Structure close to the solid-liquid interface System: Si(001)-Pb(liquid; T M +10K) Energy: ~80 kev H. Reichert et al., Nature, 408, 839 (2000) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 54
51 Diffraction from liquids 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 55
52 Small Angle Scattering (SAXS) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 56
53 USAXS (4000Å) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 57
54 Micro SAXS Orientation of micro fibrils in wood cells. Spatial resolution: 2 μm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 58
55 Micro focus applications (SAXS) I. Dobbie, M. Linari, G. Piazzesi, M. Reconditi, N. Koubassova, M.A. Ferenczi, V. Lombardi, M. Irving, Nature, 396, (1998) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 59
56 Intravenous Coronary Angiography 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 60
57 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 61
58 Microtomography at HASYLAB/DESY sample manipulator z X-ray camera y x beamstop sample monochromatic beam CCD camera lens optical mirrors fluorescent screen 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 62
59 Porous PLGA scaffold (In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland) µct at BW2 using 9 kev sample diameter: 5 mm slice (2 x 2 mm²) spatial resolution: 5.4 µm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 63
60 Titania hollow spheres (TiO 2 ) (In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland) µct at BW2 photon energy: 19 kev sample height: 1.05 mm spatial resolution: 2.1 µm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 64
61 Titania hollow spheres (TiO 2 ) (In cooperation with E. Wintermantel, B. Müller, ETH Zürich, Switzerland) µct at BW2 using 19 kev spatial resolution: 2.1 µm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 65
62 Absorption micro tomography Parallel radiation, high resolution 2D-detector example: wetting of Al-grain boundaries by Ga (ESRF ID19) 3D-grain distribution Investigation of deformed Al 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 66
63 Phase-contrast Microtomography sample manipulator X-ray camera sample in liquid z x y rotating phase shifter CCD camera lens fluorescent screen interferometer monochromatic beam 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 67
64 Rat trigeminal nerve (PµCT at 12 kev) nerve fibers (diameter 25 µm) noticeable density change 1 mg/cm³ 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 68
65 Mouse kidney: µct and PµCT at 12 kev µct: τ Z 4 E -3 ρ PµCT: Φ σe -1 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 69
66 Phase contrast imaging requirement: lateral partially coherent radiation Lateral coherence length: ξ ~ λl/s L: distance from the source; s: source size 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 70
67 Phase contrast images 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 71
68 Phase contrast tomography example: SiC in Al: Micro tomographic reconstructions 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, (1996) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 72
69 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 73
70 experimental set up of X-ray absorption spectroscopy I 0 I (Fluorescence) reference Quelle sample monochromator I 1 I 2 J. Wienold
71 Features of X-ray absorption spectroscopy I = I 0 *exp(-μd) (Lambert's law) -0.6 Intensity, au absorption [a.u.] μ d = ln(i 0 /I) Photon energy, kev μ = linear absorption coefficent photon energy, kev 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 75
72 Regions in the XAS spectra 0.0 EXAFS (Extended X-Ray Absorption Fine Structure) absorption [a.u.] XANES (X-Ray Absorption Near Edge Structure) NEXAFS (Near Edge X-Ray Absorption Fine Structure) photon energy [kev] 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 76
73 Fermis Golden rule: I XAS ~ <Φ f ê r Φ i > 2 δ E f-ei-ħω Φ i = inital state Φ f = final state = Φ outgoing + Φ backscattered ê r = dipol matrix element ê = electriv field polarisation vector of the photon, r = coordinate vector of the electron h*ν Fluorescence Auger electrons Absorption X-ray emission 2-Aug-06 J.Wienold, E. Geometrische Weckert: Strukturen, Research Abt. AC, Fritz-Haber-Institut(MPG), with Synchrotron Berlin, Germany Radiation 77
74 XANES absorption [a.u.] Kantenlage (Valenz) XANES is, Fingerprint of a single material and can be used via Principal Component Analysis (PCA, Faktor Analyse) for quantitative analysis photon energy [kev] Pre edge (inneratomare Übergänge) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 78
75 EXAFS absorption [a.u.] Energie calibration, background substraction, normalization norm. absorption [a.u.] photon energy [kev] photon energy [kev] konversion norm. absorption [a.u.] χ(k) = μ(k) - μ 0 (k) μ 0 (k) k = Substraction of μ 0 2m h norm. absorption [a.u.] ( E E ) k [Å -1 ] 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 79 k [Å -1 ]
76 χ(k) 2.0 χ(k)*k k [Å -1 ] 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 80
77 SR μ-xrf setup at Strahl L, HASYLAB, Hamburg XYZ XYZ Sample Sample stage stage Mono Mono capillary HPGe-detector capillary HPGe-detector Microscope Microscope 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 81
78 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 82
79 Refractive optics in the X-ray regime Snigirev et al., Applied Optics 37, 653 (1998) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 84
80 Micro fluorescence tomography example: root of mahagoni tree Lengeler et al. JSR, 6, (1999) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 85
81 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) 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 86
82 Inelastic scattering under high pressure 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 87
83 Geo-Science Experiments Activities of GFZ at DESY 1750t press for in situ studies of large sample volumes. pressure: ~25GPa temperature: >2000K One further similar facility at SPring8. Study of material under the conditions of the earths lower mantle. 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 88
84 Inelastic scattering under high pressure Speed of sound of Fe under pressure (ESRF: 2 ph/min) P=28GPa diamond X ray gasket sample G. Fiquet et al., Science (2000) 1 mm 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 89
85 VUV-FEL (phase 1) Achieved performance at VUV-FEL (phase 1): Radiation wavelength nm Radiation pulse energy at saturation μj Radiation pulse duration (FWHM) fs Radiation peak power 1 GW Spectrum width (FWHM) 1% Radiation spot size [FWHM] 200 μm Radiation angular divirgence [FWHM] 260 μrad Radiation peak brilliance up to Number of photons per bunch transverse coherence 1x10-4 1x10-5 1x10-6 1x10-7 TTF FEL saturation September 10, 2001 λ = 98.1 nm L g = 0.68 m E sat = 90 μj VUV-FEL (phase 1) in saturation at 98nm E [J] 1x10-8 1x10-9 1x E = E sh exp(z/l g ) W sh ~ 1-2 W Aug-06 E. Weckert: Research with Synchrotron Radiation 90 z [m] Undulator length [m] V. Ayvazyan et al., PRL 88(2002)104802
86 VUV-FEL (phase 1) First Experiments Xe-cluster experiment E phot = 12.8eV E ion = 12.1eV N~ N~ Xe intensity [arb. units] N~2-20 Xe atom Cluster size dependence Wabnitz et al., Nature, 420 (2002) Xe tim e of flight [ns] 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 91
87 Results: Time-Resolved Microscopy Silicon Graphite (HOPG) K. Sokolowski-Tinten et al. 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 92
88 First demonstration of ultrafast coherent X-ray diffraction Pulse #1: Diffraction reveals structure before radiation damage occurs Pulse #2 sees structure destroyed by pulse #1 Incident FEL pulse: 30 fs, 32 nm, 3x10 13 W cm o -15 o sample multilayer mirror CCD To beam dump H. Chapman, J. Hajdu et al. 2-Aug-06 E. Weckert: Research with Synchrotron Radiation 93
89 Example: Time resolved investigation of the photo ionization of CO-myoglobin at ID9 (ESRF): - pump-probe technique - X-ray crystallography Variable delay between laser pump pulse and X-ray probe pulse. 32 exposures per image pink Laue technique, range: Å Time resolved investigation Schotte et al., Science 300(2003) Aug-06 E. Weckert: Research with Synchrotron Radiation 94
90 Time resolved crystallography XFEL: 1000 times better time resolution than today Schotte et al., Science 300(2003) Aug-06 E. Weckert: Research with Synchrotron Radiation 96
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