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Evaluation of Two Methods for Determining Shell Thicknesses of Core-Shell Nanoparticles by X-ray Photoelectron

C J Powell¹, W S M Werner², A G Shard³

¹Materials Measurement Science Division, National Institute of Standards and Technology, Gaithersburg, Maryland 20899-8370, United States.

The Journal of Physical Chemistry. C, Nanomaterials and Interfaces

|February 1, 2017

Summary

Determining nanoparticle shell thickness using X-ray photoelectron spectroscopy (XPS) requires careful method selection. The Shard equation method proved accurate for core-shell nanoparticles, outperforming a planar film method.

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Area of Science:

Materials Science
Surface Science
Nanotechnology

Background:

Accurate determination of shell thickness in core-shell nanoparticles (NPs) is crucial for understanding their properties.
X-ray photoelectron spectroscopy (XPS) is a common surface-sensitive technique for elemental analysis and chemical state determination.
Existing methods for thickness determination may not be suitable for the unique geometry of NPs.

Purpose of the Study:

To evaluate and compare two distinct methods for determining the shell thicknesses of core-shell nanoparticles (NPs) using XPS.
To assess the performance of these methods under varying conditions, including the presence and absence of elastic scattering effects.
To identify the most reliable method for accurate shell thickness quantification in NPs.

Main Methods:

Simulated X-ray photoelectron spectroscopy (XPS) Cu 2p_3/2 spectra were generated for copper core/copper shell NPs.
Two methods were evaluated: one for planar films and another specifically developed for NPs (Shard equation).
Simulations allowed for the evaluation of methods with and without elastic scattering effects.

Main Results:

The method developed for planar films was found to be unsatisfactory for NP shell thickness determination.
The Shard equation method, specifically designed for NPs, provided satisfactory results across all simulated conditions.
Average deviations from true shell thicknesses were -4.1% (with elastic scattering) and -2.2% (without elastic scattering) using the Shard equation.

Conclusions:

The empirical equation developed by Shard is a reliable method for determining shell thicknesses in core-shell nanoparticles via XPS.
The choice of electron transport parameter (effective attenuation length vs. inelastic mean free path) depends on whether elastic scattering is considered.
Accurate shell thickness analysis of NPs using XPS necessitates employing methods tailored to their unique morphology.