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Updated: May 1, 2026

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction
Published on: April 1, 2017
Specimen-thickness effects on transmission Kikuchi patterns in the scanning electron microscope.
K P Rice1, R R Keller, M P Stoykovich
1Applied Chemicals and Materials Division, National Institute of Standards and Technology, Boulder, Colorado, U.S.A.
Specimen thickness significantly impacts transmission Kikuchi patterns in scanning electron microscopy. Optimal patterns for automated indexing were achieved across a wide thickness range, revealing scattering near the film
Area of Science:
- Materials Science
- Electron Microscopy
- Crystallography
Background:
- Transmission Kikuchi diffraction (TKD) is a powerful technique for analyzing crystalline materials.
- Understanding the influence of sample properties on TKD pattern quality is crucial for accurate microstructural analysis.
Purpose of the Study:
- To investigate the effect of specimen thickness on the generation of transmission Kikuchi patterns.
- To determine the optimal thickness range for obtaining high-quality TKD patterns for automated indexing.
- To identify the regions within a sample where electron scattering events are most likely to contribute to detectable transmission patterns.
Main Methods:
- Experiments were conducted using a scanning electron microscope (SEM).
- Specimens of varying thicknesses were prepared from materials including hafnium dioxide and aluminum.
- Monte Carlo simulations were employed to model electron scattering and transmission through the specimens.
Main Results:
- High-quality transmission Kikuchi patterns, suitable for automated indexing, were obtained from films spanning nearly three orders of magnitude in thickness (5 nm to 3 μm).
- This thickness range corresponds to a mass-thickness range of approximately 5 to 810 μg cm⁻².
- Analysis indicated that the most significant scattering events contributing to detectable transmission patterns occur very close to the exit surface of the specimen.
Conclusions:
- Specimen thickness has a demonstrable effect on transmission Kikuchi pattern generation.
- Automated indexing of TKD patterns is feasible across a broad range of specimen thicknesses.
- The findings provide valuable insights for optimizing sample preparation and data acquisition in TKD analysis.
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