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Inelastic mean free path measurement by STEM-EELS technique using needle-shaped specimen.

Keiichiro Oh-Ishi¹, Tetsu Ohsuna¹

¹Toyota Central R&D Labs., Inc., 41-1 Yokomichi, Nagakute, Aichi 480-1192, Japan.

Ultramicroscopy

|February 23, 2020

Summary

Electron energy loss spectroscopy (EELS) determined the inelastic mean free path (IMFP) to accurately measure TEM thin foil thickness. This method, using needle-shaped specimens, provides reliable thickness estimations for materials like Al, Si, and Fe.

Keywords:

EELS Inelastic mean free path Number density Plasmon STEM Thickness

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Area of Science:

Materials Science
Solid State Physics
Analytical Chemistry

Background:

Accurate thickness measurement of Transmission Electron Microscopy (TEM) thin foils is crucial for material characterization.
Electron Energy Loss Spectroscopy (EELS) is a powerful technique for analyzing the electronic structure and composition of materials.
Determining the Inelastic Mean Free Path (IMFP) is essential for quantitative EELS analysis and thickness determination.

Purpose of the Study:

To establish a reliable method for estimating the accurate thickness of TEM thin foils using EELS.
To determine the Inelastic Mean Free Path (IMFP) for Aluminum (Al), Silicon (Si), and Iron (Fe) using a novel approach.
To investigate the influence of specimen geometry and collection semi-angle on IMFP measurements.

Main Methods:

Utilized needle-shaped specimens of 99.99% Al, Si wafer, and 99.99% Fe for TEM analysis.
Performed Electron Energy Loss Spectroscopy (EELS) measurements at an accelerated voltage of 200 kV.
Analyzed the linear relationship between TEM thin foil thickness and the ratio of total EELS spectrum intensity to zero-loss spectrum intensity.
Employed weighted least-square fitting to estimate IMFP values.

Main Results:

Confirmed linear relationships between foil thickness and spectral intensity ratios for Al, Si, and Fe.
Estimated IMFP values: 143-150 nm for Al, 159-165 nm for Si (with amorphous layer), and 92-94 nm for Fe.
Demonstrated that the dependence of IMFP on the collection semi-angle (β = 11.9–35.7 mrad) is not dominant.
Observed that the accuracy of the method is influenced by the roundness of the needle-shaped specimen's cross-section.

Conclusions:

The EELS-based method using needle-shaped specimens provides an accurate means to determine TEM thin foil thickness.
The derived IMFP values are consistent with existing literature, validating the methodology.
The study highlights the importance of specimen geometry for achieving high accuracy in quantitative EELS analysis.