research with synchrotron radiation · electron k shell nucleus n m l l k k l fluorescent x-ray...
TRANSCRIPT
![Page 1: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/1.jpg)
DESY
HASYLAB at DESYDESY Summer Student Common Lectures.July 30, 2009
Research with Synchrotron Radiation.Part II - Experimental Techniques
Jens Viefhaus
![Page 2: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/2.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 1
synchrotronradiation
sampleabsorption
ionselectrons
photoemission flourescence
photons
photons
photons
transmission
inelastic/Comptonscattering
elasticscattering/diffraction
ionspectrocopy
>Synchrotron Radation enables the use of various experimental techniques
> Imaging analyzes the scattered particles (e,γ) in real space>Diffraction analyzes the scattered particles (e,γ) in reciprocal space>Spectroscopy analyzes the energy of the emitted/transmitted particles (e,i,γ)
Interaction of Synchrotron Radiation with Matter
![Page 3: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/3.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 2
Imaging - Van Gogh
![Page 4: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/4.jpg)
>X-ray radiograph
• reveals hidden face
• difficult to identify
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 3
Imaging - Van Gogh
![Page 5: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/5.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 4
www.spring8.or.jp/ENGLISH/general_info/ overview/pri_fl_x.jp
XX--rayray
ElectronElectron
K ShellNucleus
NM
L
L�
K�
K�
�L
Fluorescent XFluorescent X--rayray
>X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called “fluorescence”
• Characteristic energy of fluorescence for each element
• Intensity of fluorescence is proportional to the number of excited atoms
• suitable for quantitative analysis
Imaging with X-ray Fluorescence
![Page 6: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/6.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 5
DORIS-IIImicroscope
fluorescencedetector(HPGe)
sample onplatform
micro-capillary
ionizationchamber
beamstop
>The experiment at DORIS: • scanning the picture with a micro beam
• detection of the emitted fluorescence photons
Imaging - The X-ray Fluorescence Setup
![Page 7: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/7.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 6
Imaging - Van Gogh at Beamline L of DORIS
![Page 8: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/8.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 7
Imaging - Van Gogh at Beamline L of DORIS
![Page 9: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/9.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 8
>Painting is scanned with 0.5 mm resolution
• For each of the 90,000 pixels a full spectrum is recorded:
Imaging - Van Gogh Pixel by Pixel
![Page 10: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/10.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 9
Imaging - Van Gogh
![Page 11: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/11.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 10
Imaging - Van Gogh (Zn K-shell Fluorescence)
![Page 12: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/12.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 11
Imaging - Van Gogh (Ba K-shell Fluorescence)
![Page 13: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/13.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 12
Imaging - Van Gogh (Pb L-shell Fluorescence)
![Page 14: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/14.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 13
Imaging - Van Gogh (Sb K-shell and Hg L-shell Fluorescence)
![Page 15: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/15.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 14
> In order to identify the actual colour used by Vincent van Gogh, additional XANES scans were taken:
Sb K-edge (DORIS) Sb L3 and L2-edge (ESRF)
Pigment painting
Pb2Sb2O7, Naples yellow
NaSbO3OH*3H2O
KSbO3*3H2O
Sb3O6OH, stibiconite
Sb2O4
Sb2S2O, kermesite
Sb2O3 valentinite mod.
Sb2O3 senarmontite mod.
X-ray Absorption Near Edge Structure - Paint Fingerprint
![Page 16: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/16.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 15
>To verify the fact that Sb and Hg are predominantly at the 2nd layer additonal µ-XRF scans were performed:
Van Gogh - Micro X-ray Fluorescence
![Page 17: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/17.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 16
> In conclusion, the analytical techniques above nicely complement each other.
• Anal. Chem., 80, 16, 6436 - 6442, 2008
Visualizing a Lost Painting by Vincent van Gogh
![Page 18: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/18.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 17
>µ-XRF can determine the concentration of trace-level distributions within a water flea Daphnia magna • combining 2D/3D fluorescence with micro-probe and X-ray absorption tomography allows to create a detailed map of metal concentrations.
• This enables scientifically based environmental regulations
• J. Anal. At. Spectrom, 23, 829-839 (2008) , Anal Bioanal Chem, 390, 267-271 (2008)
Ca
Zn
Fe
Metal Contaminations in Small Water Fleas
![Page 19: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/19.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 18
xy
z
X-ray camera
sample manipulator
CCD camera lens fluorescent screen
monochromaticbeam
sample
optical mirrors
beamstop
>Principle: Measurement of many different projections • Numerical reconstruction of a 3-dimensional data set "absorption per voxel"
Micro-Tomography at DORIS III
![Page 20: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/20.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 19
Conventional rivetedairframe structure Welded metallic airframe
Courtesy: J. Herzen, F. Beckmann (GKSS)
>Characterization of Al-alloy T-joints • In aircraft construction so-called stingers are currently used as pore-free laser-welding is still too expensive
• Welded clips could instead reduce the weight provided that the technology is being further developed
Micro-Tomography of Complex Samples
![Page 21: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/21.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 20
Courtesy: J. Herzen, F. Beckmann (GKSS)
Aluminum Clip (I) und Skin (II)
II
Weld with pores
I
Laser
pore
>Characterization of Al-alloy T-joints, first results: • Visualisation of different sorts of pores
• Clear separation of the weld and raw materials
• High density resolution using absorption contrast
Micro-Tomography at 40 keV
Micro-Tomography of Complex Samples
![Page 22: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/22.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 21
H. F. Poulsen et al., J. Appl. Cryst. 34, 751 (2001)
5 µm
3D X-ray diffraction microscopy
>Change of microstructure of a material upon mechanical load and deformations?
>Grain properties to be determined: • position • morphology • orientation • deformation (plastic/elastic) • composition
Grain mapping of metals and alloys
![Page 23: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/23.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 22
DiffractionpatternIllumination
by a spatiallyextended beam
Array of scatterers A(x)
Position xMomentum transfer q
Intensity |A(q)|2
Relation between A(x) and A(q):
0kkq �= momentum transfer
k0k
q
dxexAqA xqi∫= )()(
Task: Determine A(x) from measured |A(q)|2
Problem: Eq. (1) cannot be simply inverted, because the phase is lost(Phase problem of crystallography)
(1)
Principles of Structure Determination
![Page 24: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/24.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 23
_
DiffractionpatternIllumination
by a spatiallyextended beam
Array of scatterers A(x)
Position xMomentum transfer q
Intensity |A(q)|2
k0k
q
Position of diffraction peaks given by Bragg‘s equation:
n = 2dh,k,lsinΘ
dΘ
Principles of Structure Determination
![Page 25: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/25.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 24
> Nobel prize in chemistry 1985:
• For the developement of direct methods for the structur determination of cristals
Herbert A. HauptmanJerome Karle
amplitudeand
phasecorrect
Fourier-transformed,
using thecorrect
amplitudebut
changingthe phase
X-ray Diffraction - The Phase Problem
![Page 26: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/26.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 25
>A priori information on the structure • ("educated guess" and then compare with model)
>MIR - Multiple Isomorphous Replacement • Besides the structure determination of the original crystal, at least two more crystals doped with heavy atoms have to be measured
>S/MIRAS - Single/Multiple Isomorphous Replacement with Anomalous Signal • In addition to the original crystal at least one more crystals has to be measured and its doped heavy atoms have to be excited to anomalous diffraction
>MAD - Multiple Anomalous Dispersion • The crystal has to be doped with an anomalously diffracting atom, which must be measured at several different wavelength
Finding Solutions for the Phase Problem in X-ray Diffraction
![Page 27: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/27.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 26
>Text
• item 1
• item 2
• item 3
>Text
• item 1
• item 2
• item 3
Measured electrondensity-distribution
Structure of thea priori information
Result
X-ray diffraction - "Guessing" the structure
![Page 28: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/28.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 27
> Naturally the quality of the resulting structure model depends strongly on the required resolution. Resolutions in the order of 120 pm are state-of-the-art.
300 pm
200 pm
120 pm
X-ray diffraction - resolution
![Page 29: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/29.jpg)
Measured quantities are theabsolute values of thescattering factors FP (original)and FPH (doped).
The phase αP isunknown (circle):
If the location of the heavy atom is known, the originof FH is determined. This rersults in two solutionsfor the phase, which can be madeunique via a third measurementusing another heavy atomand its correspondingscattering factor FPH2
• Besides the structure determination of the original crystal, at least two more crystals doped with heavy atoms have to be measured
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 28
Phase Problem - Multiple Isomorphous Replacement
![Page 30: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/30.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 29
>Single crystal diffractomter in κ-geometry with CCD and scintillation counter. Crystal mounted on a glass fiber. the diffractometer has 3 rotations for the crystal and one for the detector
Single Crystal Diffractometer
![Page 31: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/31.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 30
Protein crystallography Diffraction pattern
Protein crystal(lysozyme)
X-rays
Carbon: GreyNitrogen: Blue Oxygen: Red Sulphur: Yellow
X-ray diffraction of Bio-Molecules
![Page 32: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/32.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 31
J .M. Grimes et al., Nature 395, 470-478 (1998)
Example: Blue Tongue Virus
X-ray diffraction of extremely large complexes
![Page 33: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/33.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 32
Research in geophysics
gasket
sample
diamond
X ray
1 mmDiamond anvil cell
X-ray Scattering from Samples Under High Pressure
![Page 34: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/34.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 33
1750 t press for in situ studies of large sample volumes
Maximum pressure ~ 25GPaTemperature: > 2000KStudy of material under the conditionsof the earths lower mantle
GFZ (GeoForschungs Zentrum Potsdam) @ DESY
X-ray Scattering Under High Pressure
![Page 35: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/35.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 34
Example: Determine t he speed of sound in Fe under pressure
G. Fiquet et al., Science (2000)
gasket
sample
diamond
X ray
1 mm
P = 28 GPa
Peaks aredue t o phonons
X-rays change energy due t o interaction with phonons
Inelastic X-ray Scattering under High Pressure
![Page 36: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/36.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 35
>Photons are resonantly absorbed near an absorption edge>The outgoing electron is scattered by the surrounding atoms> Interference of the outgoing electron wave with the backscattered electron waves: • Modulation of the cross section as a function of energy provides access to information on the distance of neighbour atoms:
X-ray Absorption Spectroscopy
![Page 37: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/37.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 36
monochromator
I0
I1 I2
sample
reference
Source
I (Fluorescence)
Intensitymonitor (0)
Intensitymonitor (1)
Intensitymonitor (2)
X-ray Absorption Spectroscopy: Experimental setup
![Page 38: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/38.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 37
X-ray absporption spectroscopy
0.25
0.5
0.75
1.0
0.00.0
5 10 150-5
norm
. abs
orpt
ion
[a.u
.]
k [Å -1 ]
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 ]
energy 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 ]
conversion
( )02 EEmk �−=h
µ(k) - µ0(k) µ0(k)χ(k) =
Substraction
of µ00.0
2.0
0.0
-2.0
5 7.5 10 12.5
χ (k)
*k3
k [Å -1 ]
χ(k)
![Page 39: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/39.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 38
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
Contains information about t he chemicalbinding state of the absorbing atoms
Contains information about t heinteratomic distances
Regions in the X-ray Absorption Spectrum
![Page 40: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/40.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 39
Rh K-edge absorption spectra
• spatial distribution of Rh oxidations states
• strong gradients within < 100 ��m
In-situ 2D-mapping of the catalyst inside a catalytic micro-reactor
J.-D. Grunwaldt et al., J. Phys. Chem. B 110, 8674 (2006)
Catalyst structure at the atomic level under industrial reaction conditions (dynamic, in situ, in operando)Example: partial oxidation of methane over Rh/Al2O3
promising reaction for the production of hydrogen from natural gas
CH4 + ½ O2 -> CO + 2 H2
2D-Mapping of the Structure of a Heterogeneous Catalyst
![Page 41: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/41.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 40
• Dramatic changes in the ion charge state at high power densities• One atoms has to absorb >50 photons
Phys. Rev. Lett. 99, 213002 (2007)
Photoelectric Effect at Ultrahigh Intensities of FLASH (13.5 nm)
![Page 42: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/42.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 41
>Single shot diffractive imaging • resolution 50 nm • next shot reveals that target is destroyed
Nature Physics 2, 839 (2006)
Diffraction image (1st shot)
Diffraction image (2nd shot)
reconstruction (1st shot)
Ultrafast Coherent Diffractive Imaging at FLASH
![Page 43: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/43.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 42
>Pump-probe investigation of damage evolution
Nature Photonics 2, 415–419 (2008)
2 µm
-5 ps 10 ps 15 ps 40 ps after Nd:YAG pulse
reconstruction reconstruction>"scale of destruction":
Ultrafast Movies of Nanoscale Dynamics
![Page 44: Research with Synchrotron Radiation · Electron K Shell Nucleus N M L L K K L Fluorescent X-ray > X-ray Fluorescence Spectrometry (XRF): • X-ray emission excited by X-rays is called](https://reader035.vdocument.in/reader035/viewer/2022063018/5fdb801e0a79a367a82451c0/html5/thumbnails/44.jpg)
DESYJens Viefhaus | DESY Summer Student Common Lectures, DESY Hamburg | July 30, 2009 | page 43
>Testbed for single shot imaging at SR ring • only 100 spectra with 108 photons each • resolution 25 nm
Phys. Rev. Lett. 100, 245503 (2008)
Diffraction image(and Fourier transform) Reconstruction (a), resolution test (b) and original structure (c)
Hard X-ray Holographic Diffraction Imaging