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Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples
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Depth-selective x-ray diffraction using energy-dispersive x-ray detector and straight capillary optics.

Shotaro Fukumoto1, Masaki Okuda1, Tsugufumi Matsuyama1

  • 1Department of Chemistry and Bioengineering, Graduate School of Engineering, Osaka Metropolitan University, 3-3-138 Sugimoto, Sumiyoshi-ku, Osaka 558-8585, Japan.

The Review of Scientific Instruments
|June 25, 2024
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Summary

A new depth-selective X-ray Diffraction (XRD) technique uses an energy dispersive (ED) detector for detailed material analysis. This method enables precise examination of layered samples by analyzing X-ray diffraction patterns at varying depths.

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Area of Science:

  • Materials Science
  • Crystallography
  • Analytical Chemistry

Background:

  • Traditional X-ray Diffraction (XRD) provides bulk material information.
  • Depth-resolved analysis is crucial for understanding layered materials and thin films.
  • Existing methods for depth profiling can be complex or destructive.

Purpose of the Study:

  • To develop and demonstrate a novel depth-selective X-ray Diffraction (XRD) technique.
  • To enable non-destructive, layer-by-layer analysis of material composition and structure.
  • To showcase the utility of energy-dispersive (ED) detection for depth profiling.

Main Methods:

  • Utilized a depth-selective XRD setup with two straight capillary optics to define incident and detected X-ray beams.
  • Employed an energy dispersive (ED) X-ray detector to measure diffraction spectra at fixed angles.
  • Varied the sample position to achieve depth selectivity, analyzing the intersection of the two capillary-defined beams.
  • Investigated a layered sample composed of silicon (Si) powder film and a muscovite film.

Main Results:

  • Successfully demonstrated depth-selective XRD measurements on a layered sample.
  • Observed distinct XRD peaks in the high-energy range (>10 keV) of the ED spectrum, beneficial for low absorption.
  • Confirmed the capability of the technique to differentiate and analyze individual layers within the sample.
  • Showcased the advantage of depth-selective measurement over conventional XRD.

Conclusions:

  • The developed depth-selective ED-XRD technique is effective for analyzing layered materials.
  • High-energy XRD peaks detected by ED offer advantages for depth analysis due to reduced sample absorption.
  • This method provides a valuable tool for non-destructive, depth-resolved structural characterization.