from diffraction to scattering holographyilsf.ipm.ac.ir/news/2014-03-03beamlineopwrkshp/... · slit...
TRANSCRIPT
![Page 1: From Diffraction to Scattering Holographyilsf.ipm.ac.ir/News/2014-03-03BeamlineOpWrkshp/... · slit sistem 4-circle goniometer . w: [0-75 deg]; c: [0-90 deg] 1377 pixels 5 sec/pixel](https://reader033.vdocument.in/reader033/viewer/2022060819/6098cfd1b791ae01ea711585/html5/thumbnails/1.jpg)
From Diffraction to Scattering Holography
A Lausi
Sincrotrone Trieste, S.S. 14 - Km 163.5, Area Science Park, 34012 Basovizza - Trieste, ITALY
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Fourier holography Gabor (in-line) holography
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Gabor Internal source
T
XFH
Szöke 1985
T
T
T
E E
E
MXFH
EEH
XFH
Tegze et al 1991
Tegze et al 1996 Gog et al 1996
XFH – Timeline Milestones
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XFH – the internal source scheme
I(k)
A
j
rj
R
FE ,k
A - reference atom
j r - position vector of j-th atom
F E - energy of x-ray fluorescence from A
k - wave vector
R - sample - to - detector distance
A. Szöke, AIP Conf. Proc. 147, 361 (1986)
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XFH – theoretical background
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XFH – theoretical background
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XFH – theoretical background
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MXFH – the internal detector scheme
I(k)
rj
j
X-rayfluorescence
E, k
EF
reference wave
scattererobject waves
detectoratom
T. Gog, P.M. Len, G. Materlik, D. Bahr, C.S. Fadley and C. Sanchez-Hanke
Phys. Rev. Lett. 76, 3132 (1996).
U(r) = Uk (r)e- ikr
k
å
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The angular region Jmax determines the resolution of the reconstructed images:
The angular resolution of the experiment DJ determines the maximum radius rmax of the region
around the emitter where meaningful information can be obtained:
e.g. rmax = 10 l D 1 deg.
)cos1()kk(
2r
maxminmax
lD
2r
lD
maxr
2k
D
maxr
lD
The effect of experimental parameters
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Internal source scheme
Internal detector scheme
Source:
scanning detector
scanning source
Flux The higher the better
Collimation NOT REQUIRED Low-pass filter
Monocromaticity NOT REQUIRED YES
Sample:
An ensemble of emitters, surrounded by an arrangement of scatteres which appears the same from whichever
of the emitters it is seen.
Detector:
Energy selective
YES, to get rid of the exciting radiation scattering
Sensitive area Low-pass filter TBTB
Count rate YES YES
Designing the experiment
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ionizationchamber
w
csample (GaAs)
4-circle goniometer
foil filter
E+E
E, k
entranceslits
sample holder(precession movement)
alignment base
photodiode
F
EF
Suitable for both schemes
PIN diode
Analyser crystal
+ fast scintillation counter
Foil filter + photodiode
experimental set-up at ELETTRA
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Precession Sample Holder
tilt angle adj.
sample
attachment support
motor
rotation axis
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ionization
chamber
X ray Fluorescence Holography experiment at the ELETTRA diffraction beamline
alignment
base
slit sistem
4-circle
goniometer
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w: [0-75 deg]; c: [0-90 deg] 1377 pixels
5 sec/pixel
3 hours total time
4 106 counts/sec per pixel
Normalization for primary beam
Low pass filter (~ 8 deg)
High pass filter
Measurement
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Reconstructed holographic image of GaAs(001), plane z=0
XF Hologram of GaAs
E.Busetto, M.Kopecky, A.Lausi, R. Menk, M.Miculin, and A.Savoia Phys. Rev. B, 62 5273 (2000)
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Area detector experimental set-up
E+EF
spindle axis
imaging plate alignement base
sample
beamstopper
slits
imagingplate
E , kF
foilfilter
incidentbeam
Sample size: 2 x 2 x 0.05 mm3
Filter size: 100 x 100 mm2
Sample-to-detector distance: 80 mm
64 images:
filter moved on a 8x8 mesh of positions with 2
mm pitch
+64 normalization images
about 3 h for 128 images
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Area detector raw data
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Area detector hologram + Kossel lines
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Area detector hologram
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Area detector hologram reconstructed image
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Area detector alternative experimental set-up
CoO sample size: 2 x 2 x 1 mm3
Fe filter size: 100 x 100 mm2 , 50 mm thick
E = 8.0 keV (Co K-edge @ 7.7 keV)
EF = 6.9 keV
Sample-to-detector distance: 80 mm
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Area detector raw data 2
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Area detector hologram + Kossel lines 2
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Area detector hologram 2
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CoO hologram
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M.Kopecky, E.Busetto, A.Lausi, M.Miculin, and A.Savoia J Appl Phys 78, 2985 (2001)
CoO hologram - detail
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Application to diffraction pattens
Scattering from a cluster of atoms
Diffraction pattern calculated
for a small cluster (eight unit
cells) of rock salt at an
energy of 18.2 keV. The plot
coordinates are defined as
k’= k/k.
The incident wavevector k0 =
(0, 0, k) is supposed to be
perpendicular to a
face of the unit cell; plot axes
coincide with the
crystallographic axes.
ji
i j
*
ji2
0 iexpFFR
I)(I rrkkk,kk,kk 000
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Real-space image
The function P(r) in the
plane z = 0 obtained from
the simulated diffraction
pattern. The positions of
local maxima coincide with
interatomic distances.
ij
ij
i j
ij0
*
ji2
0k00
k
ksiniexpFF
R
Idiexp,I)(P
rr
rrrrkrkkkkr
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Test: diffuse scattering from crystal
Photon energy 18.2 keV.
Sample surface in the xy
plane oriented
perpendicular to the
incident beam with a
wavevector k0 = (0, 0, k).
Diffuse X-ray scattering from an NaCl crystal recorded on a CCD detector.
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Diffuse scattering reconstruction
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X-Ray Diffuse Scattering Holography - theory
(Kopecký M.: J. Appl. Cryst. 37, (2004), 711)
rn º (0,0,0)If and
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X-Ray Diffuse Scattering Holography - theory, continued
(Kopecký M.: J. Appl. Cryst. 37, (2004), 711)
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X-Ray Diffuse Scattering Holography - data
Diffraction patterns Hologram
Rubidium Chloride E = 15.06 keV, E = 60 eV
z=0 z=0
(Kopecký et al., Appl. Phys. Lett. 87 (2005), 231914
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X-Ray Diffuse Scattering Holography - reconstruction
Pair distribution function Electron density
z=0 z=0
(Kopecký et al., Appl. Phys. Lett. 87 (2005), 231914)
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GaMnAs layers
= diluted magnetic semiconductor (magnetic and semiconducting properties) promising for spin electronics
Magnetic properties (e.g. Curie temperature TC) are strongly related to Mn sites:
Mn in substitutional position act as an acceptor and created a hole
Mn in interstitial position acts as a double donor and passivates two holes
c-RBS and c-PIXE (channeling Rutherford backscattering and particle induced x-ray emission
- presence of interstitials can be verified
Indirect methods
Concentration of interstitial atoms is often estimated by comparing experimental data with theoretical models using:
- changes of a lattice parameter due to interstitial atoms
- integral intensities of weak Bragg reflections
XFH (x-ray fluorescence holography)
a three-dimensional atomic image around Mn atoms in Zn0.4Mn0.6Te
application to very thin Ga1-xMnxAs layers with low concentration of dopants (x < 0.1) is problematic because of the weak
fluorescence signal
XDSH (x-ray diffuse scattering holography)
a three-dimensional atomic image around Mn atoms in GaMnAs
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GaMnAs layers -Experimental Configuration
material science beamline ID11 at the European
Synchrotron Radiation Facility in Grenoble, France
(J. P. Wright)
GaMnAs layers grown by low-temperature MBE,
Institute of Physics, Prague (M. Cukr, V. Novák, K.
Olejník)
photon energy 30 keV
conditions of total reflection (grazing angle of
0.07°)
beam size 300 μm (horizontal) × 10 μm (vertical)
16-bit CCD camera
FreLon2k16 (2048 × 2048 pixels, pixel size 46 ×
46 μm2)
sample-to-detector distance 65 mm
exposure time 20 s per frame
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GaMnxAs layers at lower concentration of Mn: x = 0.02
Diffraction patterns Hologram
isomorphous
replacement
GaMnAs ×
GaAs
Electron density
= local neighborhood of
dopants
Reconstruction
algorithm
Mn atoms in
SUBSTITUTIONAL
POSITIONS
(Kopecký et al., J. Appl. Cryst. 39 (2006), 735)
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X-Ray Diffuse Scattering Holography - advantages
X-ray fluorescence holography
- low signal-to-background ratio (~ 0.1 %)
- intense and dense Kossel line patterns
- virtual images
solved by XDSH
- signal-to-background ratio 1-10 %
- discrete (and thus removable) Bragg peaks instead
of Kossel lines
- virtual images can be removed by measuring a
complex hologram (for centrosymmetric samples,
virtual image = real image)
- wavelength of x rays of the same order as interatomic distances
=> strong artefacts in the reconstructed image
solved by multi-energy anomalous diffuse scattering
(MADS)
Overcomes experimental
difficulties:
Fundamental problem:
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Multi-Energy Anomalous Diffuse Scattering
MADS extends principles of XDSH to three dimensions
intensities measured at
TWO-DIMENSIONAL THREE-DIMENSIONAL
surface region
in the reciprocal space
reconstructed real-space-image
STRONG ARTEFACTS FREE OF ARTEFACTS
XDSH MADS vs
(Kopecký M., Fábry J., Kub J., Lausi A., Busetto E.: Phys. Rev. Lett. 100 (2008), 195504)
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Multi-Energy Anomalous Diffuse Scattering
vs
(Kopecký M., Fábry J., Kub J., Lausi A., Busetto E.: Phys. Rev. Lett. 100 (2008), 195504)
MADS applies principles of MAD to diffuse scattering
intensities measured in
DISCRETE POINTS CONTINUOUS REGION
(Bragg peaks) (diffuse scattering)
in the reciprocal space
provides information on
LONG-RANGE ORDERING SHORT-RANGE ORDERING
MAD MADS
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Multi-Energy Anomalous Diffuse Scattering
Three-dimensional pattern of
diffuse scattering intensity
of a SrTiO3 single crystal
collected at the photon energy
of 14 keV
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Multi-Energy Anomalous Diffuse Scattering
The anomalous diffuse
scattering pattern
obtained as a difference of
two diffuse scattering
patterns
recorded at energies of 14
keV and 16.055 keV
(i.e. 50 eV below the K
absorption edge of
strontium)
![Page 43: From Diffraction to Scattering Holographyilsf.ipm.ac.ir/News/2014-03-03BeamlineOpWrkshp/... · slit sistem 4-circle goniometer . w: [0-75 deg]; c: [0-90 deg] 1377 pixels 5 sec/pixel](https://reader033.vdocument.in/reader033/viewer/2022060819/6098cfd1b791ae01ea711585/html5/thumbnails/43.jpg)
Multi-Energy Anomalous Diffuse Scattering
Reconstructed image of the atomic planes parallel to the (001)
crystallographic plane at z = a and z = 3a/2 (a = 3.905 Å)
![Page 44: From Diffraction to Scattering Holographyilsf.ipm.ac.ir/News/2014-03-03BeamlineOpWrkshp/... · slit sistem 4-circle goniometer . w: [0-75 deg]; c: [0-90 deg] 1377 pixels 5 sec/pixel](https://reader033.vdocument.in/reader033/viewer/2022060819/6098cfd1b791ae01ea711585/html5/thumbnails/44.jpg)
Thanks…
M. KOPECKÝ, J. FÁBRY, J. KUB, Z. ŠOUREK Institute of Physics of AS CR, Prague, Czech Republic
E. BUSETTO Sincrotrone Trieste, Italy
J. P. WRIGHT ESRF, Grenoble, France
![Page 45: From Diffraction to Scattering Holographyilsf.ipm.ac.ir/News/2014-03-03BeamlineOpWrkshp/... · slit sistem 4-circle goniometer . w: [0-75 deg]; c: [0-90 deg] 1377 pixels 5 sec/pixel](https://reader033.vdocument.in/reader033/viewer/2022060819/6098cfd1b791ae01ea711585/html5/thumbnails/45.jpg)
M Kopecký
J Kub
E Busetto
Institute of Physics, Academy of
Sciences of the Czech Republic
ELETTRA