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X-ray Diffraction of Biological Samples01:10

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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
According to Bragg's law, when X-rays strike the sample positioned on a stage, the rays are  scattered by the electron clouds around the sample atoms. The  X-ray diffraction or scattering is caused by constructive interference of the X-ray waves that reflect off the internal...
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High Pressure Single Crystal Diffraction at PX^2
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HTD2: a single-crystal X-ray diffractometer for combined high-pressure/low-temperature experiments at laboratory

Andreas Fischer1, Jan Langmann1, Marcel Vöst1

  • 1CPM, Institut für Physik, Universität Augsburg, 86159 Augsburg, Germany.

Journal of Applied Crystallography
|October 17, 2022
PubMed
Summary

Researchers designed a new low-temperature/high-pressure (LT/HP) diffractometer for single-crystal X-ray diffraction. This instrument enables detailed study of subtle structural changes under extreme conditions using a laboratory source.

Keywords:
HTD2high pressureinstrumentationlow temperaturesingle crystals

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Area of Science:

  • Materials Science
  • Crystallography
  • Physical Chemistry

Background:

  • High-pressure (HP) and low-temperature (LT) X-ray diffraction experiments demand specialized equipment and techniques, particularly for cryogenic temperatures below 80 K.
  • Studying subtle structural changes in pressure-temperature (p-T) phase diagrams requires single-crystalline samples and extreme LT/HP conditions, typically necessitating synchrotron facilities.

Purpose of the Study:

  • To describe the design of a novel LT/HP diffractometer (HTD2) for single-crystal X-ray diffraction.
  • To enable experiments using a laboratory X-ray source under extreme conditions.

Main Methods:

  • Development of a dedicated LT/HP diffractometer (HTD2).
  • Implementation of non-standard sample environments and measurement strategies for cryogenic temperatures (2-400 K) and high pressures (up to 20 GPa).

Main Results:

  • The HTD2 instrument facilitates single-crystal X-ray diffraction experiments at temperatures between 2 K and 400 K and pressures up to 20 GPa.
  • The design allows for detailed investigation of subtle structural changes in the p-T phase diagram.

Conclusions:

  • The developed LT/HP diffractometer provides a laboratory-based solution for advanced single-crystal X-ray diffraction studies under extreme conditions.
  • This instrument expands the accessibility of research into material phase diagrams at cryogenic temperatures and high pressures.