# Presentation: 343791

## Science With Microbeams

- APS Science Advisory Committee Cross-Cut Review
- January 21, 2004
- Introduction, J. Murray Gibson

**Notes:**
Sample: Cu/W Intel chip

50 μm x 50 μm fly-scan
50 nm x 50 nm pixels
2 ms/pixel dwell

1 + 1*22 bunch mode
Counts/pixel       ~ 9000RMS noise/pixel ~   110
Shot noise limit  ~     95

Orientations of heteroepitaxial layers in a high Tc superconductor are closely aligned with the substrate grain orientations. Micro-diffraction data obtained at7-ID and 34-ID.

## Purpose of the Review

- Science Advisory Committee does sector-by-sector reviews
- Cross-cut gives an important perspective
- focus of review is retrospective (“where are we now”)
- additional experts invited
- Report will advise APS on strengths and opportunities
- Session is open for healthy information exchange

**Notes:**
Remember that Gerd should ask SAC first for questions

## How did we select the program?

- Current research programs involving x-rays focused to < 10m
- Asked sectors for their best science
- Only one presentation per sector, due to time
- Sectors included based on scale of activity
- Further information provided as backup
- to be posted on the web

**Notes:**
Thank Ian McNulty, Gerd, Susan and others

## 8:45 a.m.: Overview and Charge to the Review Committee

**8:45 a.m.: Overview and Charge to the Review Committee**
**(Murray Gibson)**

**9:00 a.m.: Three-dimensional polychromatic microdiffraction studies of mesoscale structure and dynamics**
**(Gene Ice - Sector 34)**
**9:35 a.m.:  Microbeam imaging of crystals by coherent diffraction at 34-ID-C**
**(Ian Robinson - Sector 34)**

**10:00 a.m.: Applications of x-ray microbeams at the PNC-CAT beamlines**
**(Steve Heald - Sector 20)**

**10:45 a.m.: High-pressure geoscience at GSECARS**
**(Guoyin Shen - Sector 13)**
**11:15 a.m.: Earth and environmental science at the microscale level at GSECARS**
**(Matt Newville - Sector 13)**

**11:45 a.m.: The study of ferroelectric switching using x-ray synchrotron radiation**
**(Carol Thompson - Sector 12)**
**2:00 p.m.: Current and planned use of micro-beams for mineral-water interface studies at BESSRC**
**(Paul Fenter - Sector 12) **

**2:30 p.m.: Probing ferroelectricity, charge density wave dynamics, and magnetism with submicron x-ray diffraction**
**(Paul Evans - Sector 7)**

**3:30 p.m.: Magnetism studies with microbeams**
**(George Srajer - Sector 4) **

**1:30 p.m.:  Strain effects in thin film/Si substrates revealed by x-ray microdiffraction (Cev Noyan - Sector 2) **
**4:00 p.m.: Intracellular manipulation by TiO****2**
**(Gayle Woloschak - Sector 2) **

** ****4:30 p.m.:**
**Future of Nanobeam Studies**
**(Eric Isaacs)**

## APS X-ray Microbeam Techniques

**APS X-ray Microbeam Techniques**

**Coherent scattering**
**Coherent diffraction imaging**
**Full-field microscopy**
**Fluorescence microtomography**
**Inelastic x-ray scattering**
**Magnetic microscopy**
**Micro-EXAFS**
**Micro-XANES**
**Micro/nanodiffraction**
**Scanning nanotomography**
**Scanning transmission/DPC microscopy**
**Scanning fluorescence microscopy**

**Key**

## X-ray microbeam techniques in use at APS

**Scanning transmission/DPC microscopy**
**X-ray optics are used to form a microfocused spot on the sample, which is raster-scanned to form images in absorption and differential phase contrast modes. STXM is fast and can**
**be combined with XANES as for SFXM.**
**Scanning fluorescence microscopy**
**X-ray optics are used to form a microfocused spot on the sample, which is raster-scanned to form images in x-ray fluorescence contrast. SFXM is highly sensitive to elemental makeup and chemical state information.**

**Scanning differential phase contrast image of a diatom, taken with 1.8 keV x-rays at 2-ID-B.**

**Visible light and epifluorescence micrographs, false-color SFXM element maps, and x-ray phase contrast image of a silicoflagellate from the Southern Ocean. Data from 2-ID-E.**

## X-ray microbeam techniques in use at APS

**Similar to SFXM, but incident energy is scanned over a wide range to obtain extended x-ray absorption fine-structure spectra (usally fluorescence mode) at each sample point. Spectra are Fourier- inverted to discern atomic structure.**
**Micro-XANES**
**Similar to SFXM, but incident energy is scanned in fine steps to obtain x-ray absorption near-edge spectra (e.g. by fluorescence) at each sample point.**

**(a) Optical and (b) Cu K****a****  images of a vapor phase fluid inclusion in quartz taken at 13-ID, showing that Cu is uniformly distributed in the fluid phase. Cu K micro-XANES spectra show reversible changes in Cu oxidation with temperature. This may control speciation behavior during formation of important Cu deposits.**

**U and Fe fluorescence maps taken at 20-ID from a sediment thin section from beneath a leaking rad-waste storage tank at Hanford.**

**X-ray microbeam techniques in use at APS**

## X-ray microbeam techniques in use at APS

**Full-field microscopy**
**High resolution x-ray optics are used to image the sample directly onto an array detector such as a CCD camera. Main advantages are speed and amenability to phase contrast methods.**
**Fluorescence microtomography**
**Similar to SFXM, but sample is rotated through a large angular range to record many views of it. Projection data are filtered and reconstructed to form 3D images of the sample.**

**Quantitative 3D reconstructions of the real part of the refractive index of a silicon atomic force microscope tip. Coherent full-field projections taken at 2-ID-B.**

**Reconstructed slice showing trace Fe content in a SiC nuclear fuel shell, using Fe K fluorescence microtomography data recorded at 2-ID-D.**

## X-ray microbeam techniques in use at APS

**Micro/nanodiffraction**
**Microfocusing optics such as KB mirrors and zone plates are used to isolate specific sample regions ****and increase the x-ray flux density in diffraction experiments.**
**Scanning nanotomography**
**Similar to STXM, but sample is rotated through a large angular range to record many views through it. Projection data are filtered and reconstructed to form 3D images of the sample.**

**Reconstruction of 13 projections (1573 eV) through two-level chip sample, showing W vias and Al interconnects in (8 μm)****3**** volume. Data from 2-ID-B.**

## X-ray microbeam techniques in use at APS

**Microfocusing optics such as KB mirrors are used to increase the x-ray flux density on the sample in inelastic scattering experiments.**
**Magnetic microscopy**
**Similar to SFXM, but incident x-ray beam is linearly or circularly polarized to form images of the sample with magnetic charge contrast by absorption or diffraction methods.**

**Temperature effect on sound velocitie s in iron at high pressure measured at room temperature (except red crosses) at 3-ID-B**.

**Magnetic diffraction contrast image of superposed (********,0,1) (red) and (0,********,1) (green) incommensurate reflections from spin density wave domains in a Cr single crystal at 110 K****. Data recorded at 2-ID-D.**

**X-ray microbeam techniques in use at APS**

## X-ray microbeam techniques in use at APS

**Microfocusing optics such as zone plates are used to tailor the x-ray beam phase space to the sample in coherent scattering and speckle experiments.**
**Coherent diffraction imaging**
**Microfocusing optics such as KB mirrors are used to increase the x-ray flux density on the sample in coherent diffraction imaging experiments.**

**Coherent x-ray scattering experiment using zone plate microfopcusing optics,  as at 2-ID and 8-ID.**

**Coherent x-ray diffraction pattern of a single silver nanocube obtained by chemical synthesis, recorded at 34-ID-C. **

**X-ray microbeam techniques in use at APS**

## APS X-ray Microbeam Applications by Scientific Discipline

**APS X-ray Microbeam Applications by Scientific Discipline**

**Materials science**
**Life science**
**Geoscience**
**Environmental science**
**Chemical science**

**Key**

## APS microbeam publications by sector (2002-2003)

## Allocated GUPs by sector (2003)

## New microbeam initiatives

**Nanoprobe beamline (Nano-CDT, 26-ID)**
**Funded, MOU signed, construction underway**
**Inelastic x-ray scattering beamline (IXS-CDT, 30-ID)**
**Funded, MOU signed, construction underway**
**Micro XAS and Diffraction capability at BIOCAT**
**Under development ( operational 2005)**
**Environmental microspectroscopy beamline (EnviroCAT)**
**Proposed and partially-funded**
**Multiplexed microfocusing beamline (UNI-CAT, 34-BM)**
**Partner User Proposal Letter of Intent submitted**
**1-4 keV coherent imaging/scattering beamline (XOR)**
**Partner User Proposal in preparation**
**Microfocus x-ray crystallography**
**Needed at APS (UC Review Committee/Janet Smith)**

## 8:45 a.m.: Overview and Charge to the Review Committee

**8:45 a.m.: Overview and Charge to the Review Committee**
**(Murray Gibson)**

**9:00 a.m.: Three-dimensional polychromatic microdiffraction studies of mesoscale structure and dynamics**
**(Gene Ice - Sector 34)**
**9:35 a.m.:  Microbeam imaging of crystals by coherent diffraction at 34-ID-C**
**(Ian Robinson - Sector 34)**

**10:00 a.m.: Applications of x-ray microbeams at the PNC-CAT beamlines**
**(Steve Heald - Sector 20)**

**10:45 a.m.: High-pressure geoscience at GSECARS**
**(Guoyin Shen - Sector 13)**
**11:15 a.m.: Earth and environmental science at the microscale level at GSECARS**
**(Matt Newville - Sector 13)**

**11:45 a.m.: The study of ferroelectric switching using x-ray synchrotron radiation**
**(Carol Thompson - Sector 12)**
**2:00 p.m.: Current and planned use of micro-beams for mineral-water interface studies at BESSRC**
**(Paul Fenter - Sector 12) **

**2:30 p.m.: Probing ferroelectricity, charge density wave dynamics, and magnetism with submicron x-ray diffraction**
**(Paul Evans - Sector 7)**

**3:30 p.m.: Magnetism studies with microbeams**
**(George Srajer - Sector 4) **

**1:30 p.m.:  Strain effects in thin film/Si substrates revealed by x-ray microdiffraction (Cev Noyan - Sector 2) **
**4:00 p.m.: Intracellular manipulation by TiO****2**
**(Gayle Woloschak - Sector 2) **

** ****4:30 p.m.:**
**Future of Nanobeam Studies**
**(Eric Isaacs)**

## Slide 17

## X-ray Microbeam-Related Honors and Awards

- L. Bermudez, "Mycobacterial environment within macrophages," NIH grant, 2000-2004. Funded  $336K for work conducted at APS.
- B. Lai, Z. Cai, J. Maser, P. Ilinski, D. Legnini, and W. Yun, "Hard x-ray scanning microprobe," R&D 100 Award (2000).
- C.C. Retsch, "X-ray intensity fluctuation spectroscopy in the energy range from 1 to 4 keV," Ph.D. dissertation, University of Hamburg, Germany (2001).
- C.C. Retsch, Award for Best Student Poster , APS Annual User Meeting (2000).
- William Rodrigues, "Growth and characterization of Si/Ge heterostructures on Si(001) surface and Ge nano-dots on patterned Si(001) surface," Ph.D. dissertation, Northwestern University (2000).
**3-ID**
- W. Sturhahn and J. Zhao, awarded funding for beamline postdoc in nationwide competition through 2003 proposal to COMPRES (high pressure research consortium funded by NSF).
**7-ID**
- Y. Picard, University of Michigan, Ph.D. candidate, Student Presentation Award at the New Mexico Chapter Symposium of the American Vacuum Society, August 2003.
- W. Schlotter, Senior in Engineering Physics, 2002-3 Andrew Kucher Award for Best Undergraduate Research in the College of Engineering, University of Michigan.
- Z.-D. Wang, "Epitaxial Nanomagnets in Ni-MgO," Finalist for AVS Student Research Award, Annual Meeting of the American Vacuum Society, Baltimore, November 2003.
**13-ID**
- P. Eng, design of a popular microfocusing KB mirror system in use at many beamlines worldwide. Installed KB systems including 13 at APS, 3 at the NSLS, 2 at the Beijing Synchrotron (China), and 1 at SPRing-8 (Japan). At least 3 more KB systems are on order by various laboratories.
- S. Merkel, American Geophysical Union Outstanding Student Award, Ecole Normale Supérieure de Lyon, France (2002).
- M. Newville, International XAFS Society Outstanding Young Scientist Award for Theory or Instrumentation Award, University of Chicago (2003).
- S.-H. Shim, American Geophysical Union Outstanding Student Award, Princeton University (2001).
**Cont’d next slide**

**X-ray Microbeam-Related Honors and Awards**

## X-ray Microbeam-Related Honors and Awards

- Y. Arai, "Reaction dynamics and chemical speciation of phosphorus and arsenic (III and V) at the metal oxide-water interface and in soils," Ph.D. dissertation, University of Delaware (2002).
- S. Bosze, "Surface structure controlled sectoral zoning in fluorite: Implication to understanding heterogeneous reactivity at the mineral-water interface," Ph.D. dissertation, Miami University of Ohio (2001).
- C. Guest, "Manganese transformation in soils during waterlogging and subsequent drying," Ph.D. dissertation, Purdue University (2001).
- N.E. Keon, "Controls on Arsenic Mobility in Contaminated Wetland and Riverbed Sediments," Ph.D. dissertation, Massachusetts Institute of Technology (2002).
- J.-F. Lin, "Alloying effects of silicon and nickel on iron in the Earth’s core," Ph.D. dissertation, University of Chicago Jung-Fu (2002).
- S. Merkel, "Elasticité et orientations préférentielles dans la Terre profonde: approche expérimentale, Laboratoire des sciences de la Terre," Ph.D. dissertation, Normale Supérieure de Lyon (2002).
- W. Panero, "Experimental observations of basaltic crust in the lower mantle," Ph.D. dissertation, University of California at Berkeley (2001).
- S. Rekhi, "Study of the Physical Properties of Metals and Oxides at Extreme Pressure and Temperature Conditions," Ph.D. dissertation, Florida International University (2001).
- D.R. Roberts, "Speciation and sorption mechanisms of metals in soils using bulk and micro-focused spectroscopic microscopic techniques," Ph.D. dissertation, University of Delaware (2001).
- N. Sata, "High pressure studies on FexO: Quasi-isothermal compression experiments and applications to the Earth’s core," Ph.D. dissertation, University of Tokyo (2003).
- S. Shieh, "A high pressure and high temperature study of serpentine and its implications to Earth's lower mantle," Ph.D. dissertation, Princeton University  (2001).
- S.-H. Shim, "Stability, crystal structure, and equation of state of silicate perovskites in the Earth’s lower mantle," Ph.D. dissertation, Princeton University (2001).
- A. Templeton, "Lead and Selenium distributions and speciation at biofilm/metal-oxide interfaces," Ph.D. dissertation, Stanford University  (2002).
- Z. Wang, "The Study of Silicates and Refractory Materials at High Pressures and Temperatures," Ph.D. dissertation, Florida International University (2001).
- N. Taberlet, "High pressure and temperature studies on indium and selenium," masters thesis, Ecole Normale Supérieure de Lyone (2001).

**X-ray Microbeam-Related Honors and Awards**