High Pressure X ray Imaging Techniques

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1 High Pressure X ray Imaging Techniques Wenge Yang HPSynC, Geophysical Laboratory, Carnegie Institution of Washington Advanced d Photon Source, Argonne National Nti llb Laboratory Financial Support from Depart of Energy Basic Energy Sciences Short course on High Pressure Synchrotron Techniques, September 17, 2010

2 Medical X ray Imaging 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 exposing a part of the body to a small dose of ionizing radiation to produce pictures of the inside of the body. X rays are the oldest and most frequently used form of medical imaging. (RadiologyInfo.org)

3 Computed tomography (CT) An example of a single slice li CT image of the brain. Description Computed tomography (CT) scanning, also called computerized axial tomography (CAT) scanning, is a medical imaging procedure that uses x rays to show cross sectional 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 images are used for a variety of diagnostic and therapeutic purposes. Uses CT can help diagnose or rule out a disease or condition. CT has become recognized as a valuable medical tool, for: Diagnosis of disease, trauma, or abnormality; Planning, guiding, and monitoring therapy.

4 Synchrotron radiation What can we benefit from synchrotron radiation? High brilliance Coherence Polarization fast data acquisition coherent diffraction differential polarize enhance imaging Broad energy spectrum soft x ray imaging nanoscopes, interior of biologic, soft matter hard x ray imaging g nondestructive, internal or hidden components Time resolved High energy resolution High spatial resolution dynamic study, evolution spectroscopy push the spatial resolution to nanometer region

5 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 uses focusing devices to illuminate small area point by point In both cases, there must be a physical property to give contrast. They could be magnetic domain, electric domain, phase, orientation, i density, chemical composition, strain, etc.

6 Example 1 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 angle grain boundries. CeO 2 Ni (001) CeO 2 Film CCD Ni CeO 2 Ni X rays 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 modes and crystallographic tilts in oxide films on metal substrates, Nat. Mater. 2, 487 (2003).

7 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 SF 6 gas Time resolved radiographic images of fuel sprays and the shock waves generated by the sprays for time instances of 38, 77, 115, 154, and 192 ms after the start of the injection. A.G. MacPhee et al. Science 295, 1261 (2002)

8 Soft X ray Imaging Example 3,4 Mostly used for biologic i materials, soft matter, nanomagnetism Cryo X ray tomography of whole yeast, S. cerevisiae, viewed using several processing algorithms after reconstruction. C.A. Larabell and M.A LeGros, X ray Tomography Generates 3 D Reconstructions of the Yeast, Saccharomyces cerevisiae, ii 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 micronsized 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. Choe et al. Science 304, 420 (2004)

9 What do we learn from these imaging techniques and how to apply to high pressure? Diamond anvil cells Large volume press 16BM B 13BM D Only hard x ray can be used to penetrate gasket, surrounding materials and sample

10 In situ melting observation under pressure in Paris Edinburg Cell (hard x ray radiography) Example 5 Sample SeTe alloy 1 mm Pressure calibrator Au block RT and 1895 PSI Sample environment X ray 503 C and 2660 Psi 1192C and 3836 Psi Sample starts to melt Au starts to melt

11 Synchrotron x-ray DAC 3d microtomography 2 BM, Advanced Photon Source, Argonne National Laboratory

12 0 deg 45 deg Example deg 180 deg Sample: a ZrPd/Ag Goal: achieving the mass density / volume measurement of amorphous materials vs. pressure using a known crystalline phase as the internal reference

13 First success EoS measurement of a Se under pressure Pressure volume relations for Se. (A) The atomic volume change of amorphous Se under pressure determined from microtomography. (B) The time dependence of the volume change during crystallization. Snapshot from the 3D imaging Haozhe Liu et al. Anomalous high pressure movie of a Se sample in a DAC at behavior of amorphous selenium from 10.7 GPa at various viewing angles. synchrotron x ray diffraction and microtomography, PNAS, 105, (2008)

14 3d nanoscale tomography for EoS and in situ structure evolution studies Example 7 Transmission x ray microscopy (TXM) setup at 32ID C and 16ID E CCD Nano focusing zone plate Sample stage condenser Beamline capabilities: Beamline capabilities: Full field imaging with 180 degrees data collection; 3d reconstruction with FOV 25 microns and 30 nm resolution at energy 10 kev

15 Schematic of the TXM setup at 32ID C, 16ID E 30 nm feature

16 3d tomography study of recovered sample from High P T condition Separation of Fe from (Mg,Fe)SiO3 under high P T Fes-10%.mpg

17 Sample studied: single crystal Sn under pressure 2d projection view 4.7 GPa 5.7 GPa 10.6 GPa 13.7 GPa 22.2 GPa 37.7 GPa 48.0 GPa

18 3d shape change vs. phase transition and texturing (from diffraction data) 5g72.mpg 10g61.mpg 13g72.mpg Phase transition Beta tin > BCT around 11 GPa

19 22g2.mpg 37g.mpg 48g.mpg Stay at BCT phase, but more randomly oriented

20 Example 8 Coherent X ray diffraction imaging of strain at the nanoscale (Bragg geometry) Visualization of strain inside a Pb nanocrystal Ian Robinson and Ross Harder, Nature materials, 8, 291 (2009)

21 Coherent diffraction imaging (CDI) on single crystal under high pressure Experimental setup at 34ID C C, APS CCD Online Ruby Panoramic DAC on a kinematical mount K B Mirrors

22 Example 9 Sample: ~ 300 nm diameter gold single crystal on 15 um thick Si wafer Gold nanoparticles on Si wafer 10 um Average 300 nm size Au single crystals grown on Si wafer

23 CCD 0.05 degree/step rotation of sample Online Ruby system DAC Single crystal internal strain evolution vs. Pressure in DAC with 20 nm resolution in 3d Data collected on July 14, 2010 at APS 34ID C

24 Example 10 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 From John Miao, UCLS

25 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 ofthe image along the legs (shownin the inset), verifying a resolution of 71 nm. R. L. Sandberg, et al., High Numerical Aperture Tabletop Soft X ray Diffraction Microscopy with 70 nm Resolution, Proc. Natl. Acad. Sci. USA 105, (2008). 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. J. Miao, et al., Three Dimensional GaN Ga2O3 Core Shell Structure Revealed by X ray Diffraction Microscopy, Phys. Rev. Lett. 97, (2006).

26 Other ongoing developing imaging i techniques could be applied to high h pressure research Full field near edge absorption contrast imaging Magnetic probe (XMCD, XMLD, RIXS) Emission spectroscopy mapping Dynamic XPCS

27 Summary For in situ it high h pressure research, traditionally the x ray diffraction and spectroscopy are the two major tools. The promising developed x ray imaging gtechniques will provide many ways to view the evolution of sample in terms of the local microstructure, phase separation, chemical bonding, strain, magnetic domain etc., which iscomplementaryto to other in situ techniques.

28 Acknowledgements APS: Wenjun Liu Ross Harder Junyue Wang Steve Wang Xianghui Xiao Francesco De Carlo Deming Shu Ian McNulty NSLS II: Qun Shen Young Chu Diamond: Ian Robinson Stanford: Wendy Mao CIW: David Mao Guoyin Shen Lin Wang Yang Ding Malcolm Guthrie Changyong Park Curtis Kenney Benson Financial Supported by: EFree Energy Frontier Research Center DOE BES (Basic Energy Sciences) DOE NNSA (National Nuclear Security Administration)