High
Pressure
X
‐
ray
Imaging
Techniques
Wenge Yang
HPSynC,
Geophysical
Laboratory,
Carnegie
Institution
of
Washington
Ad
d Ph t
S
A
N ti
l L b
t
Advanced
Photon
Source,
Argonne
National
Laboratory
Financial Support from
Depart of Energy‐Basic Energy Sciences
Short course on High Pressure Synchrotron Techniques, September 17, 2010
Bone X‐ray (radiography)
An x‐ray radiograph is a noninvasive medical test that helps physicians
diagnose and treat medical conditions Imaging with x‐rays involves diagnose and treat medical conditions. Imaging with x‐rays involves
exposing a part of the body to a small dose of ionizing radiationto
produce pictures of the inside of the body. X‐rays are the oldest and
most frequently used form of medical imaging.
Computed tomography (CT)
A l f i l li CT
Description Uses
An example of a single‐slice CT
image of the brain.
Computed tomography (CT) scanning, also called
computerized axial tomography (CAT) scanning, is
a medical imaging procedure that uses x‐rays to
show cross‐sectional images of the body
CT can help diagnose or rule out a
disease or condition. CT has become
recognized as a valuable medical tool,
for: show cross sectional images of the body.
A CT imaging system produces cross‐sectional
images or "slices" of areas of the body, like the
slices in a loaf of bread. These cross‐sectional
for:
Diagnosis of disease, trauma, or
abnormality;
Planning, guiding, and monitoring
images are used for a variety of diagnostic and
therapeutic purposes.
What can we benefit from synchrotron radiation? What can we benefit from synchrotron radiation? High brilliance fast data acquisition
Coherence coherent diffraction
Polarization differential polarize enhance imaging Broad energy spectrum
soft x‐ray imaging nanoscopes, interior of biologic, soft matter hard x‐rayy imagingg g nondestructive,, internal or hidden componentsp Time resolved dynamic study, evolution
High energy resolution spectroscopy
High energy resolution spectroscopy
Hard X‐ray Imaging
Nondestructive, phase contrast, scanning probe, diffraction contrast, tomography, topography Basically there are two experimental approaches:
Full field imaging and scanning probe
Full field imaging needs homogeneous illumination, while the scanning probe Full field imaging needs homogeneous illumination, while the scanning probe
uses focusing devices to illuminate small area point by point
In both cases, there must be a physical property to give contrast.
Th ld b i d i l i d i h i i d i
They could be magnetic domain, electric domain, phase, orientation, density,
Orientation percolation map between substrate and film (2d scan) 2d raster‐scan on film and substrate, both crystals diffract
simultaneously. Indexing of the individual grain orientation
gives the orientation maps and percolative region by small
Ni (001) CeO2
angle grain boundries. Ni (001)
Ni CeO2 CCD 2 X‐rays Ni CeO2 Film Ni
Orientation maps produced by X‐ray microdiffraction. Black lines indicate boundaries between pixels where the total
misorientation (including both in‐plane and out‐of plane components) is greater than 5°.Each coloured area shows a
percolative region connected by boundaries of less than 5°. J.D. Budai et al., “X‐ray microdiffraction study of growth
X‐ray Imaging of Shock Waves Generated by High‐Pressure Fuel Sprays
Example 2
Time‐resolved full field imaging gives the x‐ray absorption contrast
from the compressed SF6 gas
Time‐resolved radiographic images of fuel sprays and the shock waves generated by the sprays for time instances of
Soft X‐ray Imaging
M tl d f bi l i t i l ft tt ti
Mostly used for biologic materials, soft matter, nanomagnetism
Cryo X‐ray tomography of whole
yeast, S. cerevisiae, viewed using
l i l ith
several processing algorithms
after reconstruction.
C.A. Larabell and M.A LeGros,
X‐ray Tomography Generates 3‐D Reconstructions of the Yeast,
S h i i 60
Saccharomyces cerevisiae, at 60‐
nm Resolution
Molecular Bio. Cell 15, 957 (04)
Vortex core – driven magnetization dynamics
Time‐resolved x‐ray imaging shows that the magnetization dynamics of a micron‐
sized pattern containing a ferromagnetic vortex is determined by its chirality Time‐resolved x‐ray Photoemission electron microscope (PEEM)
Was used to resolve the motion of magnetic vortices of micro‐pattern in
response to an excitation filed pulse.
What do we learn from these imaging techniques and how to apply to high pressure ?
Diamond anvil cells Large volume press
13BM‐D 16BM‐B
Only hard x‐ray can be used to penetrate gasket, surrounding materials and sample
In‐situ melting observation under pressure in Paris‐Edinburg Cell (hard x‐ray radiography)
Sample SeTe alloy
P lib t A bl k
1 mm
RT and 1895 PSI
Pressure calibrator Au block 1 mm S l i Sample environment X ray 503 C and 2660 Psi 1192C and 3836 Psi X‐ray 2660 Psi
Synchrotron x-ray DAC 3d microtomography
0 deg 45 deg
135 deg 180 deg
Sample: a ZrPd/Ag Sample: a‐ZrPd/Ag
Goal: achieving the mass density / volume measurement of amorphous materials
First success EoS measurement of a‐Se under pressure
Pressure‐volume relations for Se. (A) The
atomic volume change of atomic volume change of
amorphous Se under pressure determined
from microtomography. (B) The time
dependence of the volume change during
Snapshot from the 3D imaging
movie of a Se sample in a DAC at
crystallization.
Haozhe Liu et al. “Anomalous high‐pressure
behavior of amorphous selenium from
10.7 GPa at various viewing angles. synchrotron x‐ray diffraction and
Transmission x‐ray microscopy (TXM) setup at 32ID‐C and 16ID‐E CCD Sample stage condenser Nano‐focusing zone plate zone plate Beamline capabilities: Beamline capabilities:
Full field imaging with 180 degrees data collection;
Schematic of the TXM setup at 32ID‐C, 16ID‐E
Separation of Fe from (Mg,Fe)SiO3 under high P‐T
Sample studied: single crystal Sn under pressure 2d projection view
4.7 GPa 5.7 GPa 10.6 GPa 13.7 GPa
5g72.mpg
10g61.mpg 13g72.mpg
22g2.mpg 37g.mpg 48g.mpg
Coherent X‐ray diffraction imaging of strain at the nanoscale (Bragg geometry)
Visualization of strain inside a Pb nanocrystal
Coherent diffraction imaging (CDI) on single crystal under high pressure Experimental setup at 34ID‐C APS
Experimental setup at 34ID C, APS
CCD CCD Online Ruby Panoramic DAC on a kinematical mount K‐B Mirrors
Sample:p ~ 300 nm diameter ggold singleg crystaly on 15 um thick Si wafer
Gold nanoparticles on Si wafer
10 um
Average 300 nm size Au single crystals
Online Ruby system
CCD
DAC
y y
0.05 degree/step rotation of sample
Data collected on July 14, 2010 at APS 34ID‐C
Coherent X‐ray diffraction Microscopy for nanoscience and biology(small angle geometry)
Schematic layout of coherent diffraction microscopy. The oversampled diffraction intensities are measured
from a finite specimens, and then directly phased to obtain a high resolution image. Limitation: missing data at the center of diffraction pattern
Advantage: single‐shot imaging for 3d (could be used in x‐ray free electron lasers), non‐crystalline specimens
f d f h d Lensless imaging using coherent soft x‐ray laser beams at 47
nm. (a) SEM image of a waving stick figure sample (scale bar =
1 micron). (b) Coherent soft x‐ray diffraction pattern after curvature correction. (c) Reconstructed image with curvature
correction (d) Line out of the image along the legs (shown in
Iso‐surface renderings of the reconstructed image
from a GaN quantum dot nanoparticle, showing (a)
the front view, (b) the back and (c) the side view.
(d) 3D internal structures of the nanoparticle. correction. (d) Line‐out of the image along the legs (shown in
the inset), verifying a resolution of 71 nm.
J. Miao, et al., “Three‐Dimensional GaN‐Ga2O3 Core Shell
Structure Revealed by X‐ray Diffraction Microscopy”, Phys.
Rev. Lett. 97, 215503 (2006). R. L. Sandberg, et al., “High Numerical Aperture Tabletop Soft X‐ray
Diffraction Microscopy with 70 nm Resolution”, Proc. Natl. Acad. Sci.
Full field near edge absorption contrast imaging Magnetic probe (XMCD, XMLD, RIXS)
Emission spectroscopy mapping Emission spectroscopy mapping
Dynamic XPCS ……
F i it hi h h t diti ll Summary
For in‐situ high pressure research, traditionally
the x‐ray diffraction and spectroscopy are the
two major tools. The promising developed x‐
rayy imagingg g techniquesq will providep manyy waysy
to view the evolution of sample in terms of the
local microstructure, phase separation,
chemical bonding, strain, magnetic domain
etc which is complementary to other in situ etc., which is complementary to other in‐situ
NSLS II CIW APS: Wenjun Liu Ross Harder NSLS‐II: Qun Shen Young Chu CIW: David Mao Guoyin Shen Ross Harder Junyue Wang Steve Wang Xianghui Xiao g Diamond: Ian Robinson y Lin Wang Yang Ding Malcolm Guthrie Changyong Park Francesco De Carlo Deming Shu Ian McNulty Changyong Park
Curtis Kenney‐Benson Stanford:
Wendy Mao
Financial Supported by:
EFree‐ Energygy Frontier Research Center DOE‐BES (Basic Energy Sciences)
