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Improved Method for Electron Powder Diffraction-Based Rietveld Analysis of Nanomaterials.

Viktória K Kis^1,2, Zsolt Kovács³, Zsolt Czigány¹

¹HUN-REN Centre for Energy Research, Institute of Technical Physics and Materials Science, Konkoly-Thege Miklós út 29-33, H-1121 Budapest, Hungary.

Nanomaterials (Basel, Switzerland)

|March 12, 2024

Summary

A new in-situ transmission electron microscopy (TEM) method simplifies Rietveld analysis for multiphase nanomaterials. This technique accurately determines instrumental broadening, enhancing nanostructure analysis reliability without extra X-ray diffraction measurements.

Keywords:

Rietveld analysis electron diffraction instrumental broadening nanopowder nanostructure characterization

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Published on: August 22, 2017

Area of Science:

Materials Science
Nanotechnology
Crystallography

Background:

Multiphase nanomaterials are crucial in material science, requiring accurate nanostructure characterization for synthesis and application.
Electron powder diffraction combined with Rietveld analysis is vital for nanomaterial characterization.
Existing methods for determining instrumental broadening can be complex and time-consuming.

Purpose of the Study:

To introduce a novel, simplified, and more effective single-step in-situ transmission electron microscopy (TEM) method for Rietveld analysis of nanomaterials.
To enable direct determination of the instrumental broadening function from a single TEM measurement.
To improve the reliability of nanostructure information extracted from electron diffraction patterns.

Main Methods:

Developed a single-step in-situ TEM procedure for obtaining the instrumental broadening function.
Utilized a multilayer graphene calibration standard under controlled acquisition conditions on a spherical aberration-corrected microscope.
Modeled diffraction peak shapes using the Caglioti relation to incorporate instrumental broadening parameters into Rietveld analysis.

Main Results:

Achieved an instrumental broadening of ±0.01 Å in interplanar spacing.
Successfully separated instrumental broadening from nanostructure-related peak broadening effects.
Demonstrated the procedure's effectiveness through Rietveld analysis of hematite nanopowder and Cu-Ni nanocrystalline thin films.

Conclusions:

The proposed in-situ TEM method significantly simplifies and enhances the Rietveld analysis of nanomaterials.
Accurate determination of instrumental broadening improves the reliability of extracted nanostructure data.
This technique offers a more efficient approach for characterizing multiphase nanomaterials.