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Updated: Feb 15, 2026

Preparation of Nanoparticles for ToF-SIMS and XPS Analysis
Published on: September 13, 2020
Versatile technique for assessing thickness of 2D layered materials by XPS
Dmitry Y Zemlyanov1, Michael Jespersen2, Dmitry N Zakharov1
1Birck Nanotechnology Center, Purdue University, West Lafayette, IN 47907, USA.
X-ray photoelectron spectroscopy (XPS) offers a non-destructive method for accurately measuring the thickness of 2D materials up to 10 nm. This versatile technique enables rapid, large-area characterization, aiding in material growth optimization.
Area of Science:
- Materials Science
- Surface Science
- Nanotechnology
Background:
- Accurate thickness characterization is crucial for understanding and utilizing 2D materials.
- Traditional methods like transmission electron microscopy (TEM) offer limited sample area analysis.
- Developing rapid, large-area, non-destructive characterization techniques is essential for 2D material research and development.
Purpose of the Study:
- To establish and validate X-ray photoelectron spectroscopy (XPS) as a reliable method for determining the thickness of various 2D films.
- To demonstrate the applicability of XPS for 2D materials synthesized via different techniques.
- To highlight the advantages of XPS for large-area, non-destructive thickness assessment.
Main Methods:
- Utilized XPS to measure the intensity ratio of photoemission peaks from 2D films (few-layer graphene, MoS2, a-BN) and their substrates.
- Employed a proposed model incorporating atomic densities and electron attenuation lengths for thickness calculation.
- Validated XPS thickness measurements against cross-sectional transmission electron microscopy (TEM) data.
Main Results:
- XPS accurately measured the thickness of few-layer graphene, MoS2, and amorphous boron nitride films up to approximately 10 nm.
- Thickness calculations were validated through cross-sectional TEM measurements.
- The XPS method provides thickness values averaged over significantly larger areas compared to TEM.
Conclusions:
- X-ray photoelectron spectroscopy (XPS) is a versatile, rapid, and reliable technique for non-destructive thickness characterization of 2D materials over large areas.
- This method facilitates the optimization of growth conditions for producing thin 2D materials effectively.
- XPS analysis allows for subsequent processing or utilization of the same sample without special preparation.
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