X-ray diffractometry for the structure determination of a submicrometre single powder grain

Area of Science:

• Materials Science
• Crystallography
• Synchrotron Radiation Physics

Background:

• Accurate crystal structure determination typically requires larger sample sizes.
• Analyzing submicrometre-scale single grains presents significant challenges due to beam focusing and sample alignment.

Purpose of the Study:

• To develop a high-precision diffractometer for analyzing submicrometre-scale single powder grains.
• To enable accurate diffraction intensity data collection from individual micro-scale samples.

Main Methods:

• Utilized a focused synchrotron radiation beam from the SPring-8 BL40XU undulator beamline.
• Employed a phase zone plate for beam focusing and a low-eccentric goniometer with high-precision stages for sample alignment.
• Collected diffraction pattern data from individual BaTiO(3) powder grains (approx. 600 x 600 x 300 nm).

Main Results:

• Successfully measured accurate diffraction intensity data from submicrometre-scale single powder grains.
• Determined the crystal structure of a single BaTiO(3) grain with a reliable factor of 5.24%.
• Demonstrated the capability to analyze micro-scale crystalline materials.

Conclusions:

• The developed diffractometer is effective for submicrometre-scale single-grain structure analysis.
• This technique opens new possibilities for materials characterization at the microscale.
• High-precision instrumentation is crucial for advancing powder crystallography.