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$Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction$

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Electron diffraction characterization of nanocrystalline materials using a Rietveld-based approach. Part I.

Ankur Sinha¹, Mauro Bortolotti¹, Gloria Ischia¹

¹Department of Industrial Engineering, University of Trento, Via Sommarive 9, Trento, 38123, Italy.

Journal of Applied Crystallography

|August 17, 2022

Summary

This summary is machine-generated.

This study adapts X-ray powder diffraction (XRPD) analysis methods for electron powder diffraction (EPD). This enables faster characterization of nanocrystalline materials and reveals surface details often missed by bulk techniques.

Keywords:

Rietveld refinement instrumental broadening functions transmission electron microscopy

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Area of Science:

Materials Science
Crystallography
Nanotechnology

Background:

Transmission electron microscopy (TEM) is crucial for characterizing nanocrystalline materials.
Electron powder diffraction (EPD) combined with spectroscopy identifies crystalline phases and microstructural features.
EPD offers potential similar to X-ray powder diffraction (XRPRPD) for detailed material analysis.

Purpose of the Study:

To adapt full-pattern fitting procedures, commonly used for XRPD, to EPD analysis.
To accelerate the characterization of nanocrystalline materials, especially metastable structures.
To leverage EPD's reduced sampling volume for detecting surface alterations.

Main Methods:

Extending full-pattern fitting procedures from XRPD to EPD.
Implementing Rietveld refinement for quantitative analysis of EPD data.
Developing a reliable calibration protocol to account for instrumental broadening.

Main Results:

Demonstrated methodology for determining instrumental broadening in EPD.
Successful quantitative analysis of EPD data using Rietveld refinement.
Identified key characteristics for effective calibration standards in EPD.

Conclusions:

The adapted methodology enhances the speed and detail of nanocrystalline material characterization using EPD.
Accurate calibration is essential for separating instrumental effects from material properties.
EPD analysis provides unique insights into surface phenomena and microstructural details.