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Characterization of WSe2 Films Using Reflection Kikuchi Diffraction in the Scanning Electron Microscope and
Tianbi Zhang1, Jakub Holzer2, Tomáš Vystavěl2
1Department of Materials Engineering, University of British Columbia, 309-6350 Stores Road, Vancouver, V6T 1Z4 BC, Canada.
ACS Nano
|October 28, 2025
Summary
Reflection Kikuchi diffraction (RKD) combined with multivariate statistical methods (MSA) effectively characterizes thin films and 2D materials like WSe2. This technique simultaneously assesses thickness and crystallographic orientation, crucial for optimizing device performance.
Area of Science:
- Materials Science
- Condensed Matter Physics
- Nanotechnology
Background:
- Thin films and 2D materials, such as tungsten diselenide (WSe2), are crucial for advanced sensors and quantum technologies.
- Characterizing these materials' thickness and crystallographic orientation is vital for optimizing device functionality.
Purpose of the Study:
- To evaluate the efficacy of scanning electron microscope (SEM)-based Reflection Kikuchi Diffraction (RKD) coupled with Multivariate Statistical Analysis (MSA) for characterizing thin WSe2 films.
- To compare RKD/MSA with conventional Electron Backscatter Diffraction (EBSD) and Atomic Force Microscopy (AFM) for thickness and orientation measurements.
Main Methods:
- Utilized SEM with pixelated electron-counting detectors in both RKD and EBSD geometries.
- Applied MSA, including Principal Component Analysis (PCA), to analyze diffraction patterns for thickness and orientation variations.
- Validated thickness measurements using AFM.
Main Results:
- RKD combined with MSA effectively differentiated thickness variations and crystal orientations in WSe2 thin films.
- Simultaneous assessment of thickness and crystallographic orientation was achieved.
- Monolayer, bilayer, and trilayer WSe2 samples were successfully analyzed.
- Thickness dependency in RKD patterns was attributed to inelastic electron scattering.
Conclusions:
- RKD coupled with MSA is a powerful, non-destructive technique for characterizing thin films and 2D materials.
- This method offers simultaneous evaluation of thickness and crystallographic orientation, enhancing materials characterization capabilities.
- SEM-based techniques like RKD are valuable additions to the materials analysis toolkit for nanoscale materials.

