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In situ high temperature powder x-ray diffraction technique using a sapphire single-crystal flat cell.

S Kobayashi1, S Kawaguchi1, H Yamada1

  • 1Japan Synchrotron Radiation Research Institute, Sayo, Hyogo, Japan.

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|December 8, 2023
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Summary
This summary is machine-generated.

A new high-temperature X-ray diffraction (XRD) system was developed for studying material behaviors under various gas conditions. This advanced system enables in situ analysis of solid-gas reactions and phase transitions up to 1400°C.

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Area of Science:

  • Materials Science and Engineering
  • Solid-State Chemistry
  • Analytical Chemistry

Background:

  • Understanding material behavior in operational and manufacturing environments is crucial for industrial material design.
  • High-temperature studies are essential for characterizing materials under extreme conditions.
  • Existing methods may lack the capability to analyze materials under diverse gas atmospheres simultaneously.

Purpose of the Study:

  • To develop and validate a novel high-temperature X-ray diffraction (XRD) system.
  • To enable in situ analysis of materials under vacuum, oxidative, and reductive gas atmospheres up to 1400°C.
  • To integrate gas analysis tools for comprehensive study of solid-gas interactions.

Main Methods:

  • Development of a high-temperature XRD system utilizing a small microscope heating stage at the SPring-8 BL02B2 beamline.
  • Design of specialized sapphire single-crystal sample cells for powdered samples.
  • Integration of in situ gas analysis tools including a remote gas-pressure control system, gas chromatograph, and mass spectrometer.

Main Results:

  • Successful operation of the XRD system under vacuum, air, inert gas (up to ~1400°C), and reduction gas flow (up to ~900°C).
  • Demonstration of the system's capability to analyze gas-adsorption/desorption and solid-gas reaction processes.
  • Validation through experiments including reduction of Fe oxides, phase transitions of ZrO2 and BaCO3, and synthesis of BaZrO3.

Conclusions:

  • The developed high-temperature XRD system with integrated gas analysis is effective for studying material behaviors under diverse conditions.
  • The system provides valuable insights into chemical reactions, phase transitions, and material synthesis.
  • This technology advances the design and application of industrial materials by enabling detailed characterization.