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Tomographic Spectral Imaging with Multivariate Statistical Analysis: Comprehensive 3D Microanalysis

Published online by Cambridge University Press:  24 January 2006

Paul G. Kotula ,
Michael R. Keenan  and
Joseph R. Michael
Paul G. Kotula
Affiliation:
Sandia National Laboratories, Materials Characterization Department, P.O. Box 5800, MS0886, Albuquerque, NM 87185-0886, USA
Michael R. Keenan
Affiliation:
Sandia National Laboratories, Materials Characterization Department, P.O. Box 5800, MS0886, Albuquerque, NM 87185-0886, USA
Joseph R. Michael
Affiliation:
Sandia National Laboratories, Materials Characterization Department, P.O. Box 5800, MS0886, Albuquerque, NM 87185-0886, USA
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Abstract

A comprehensive three-dimensional (3D) microanalysis procedure using a combined scanning electron microscope (SEM)/focused ion beam (FIB) system equipped with an energy-dispersive X-ray spectrometer (EDS) has been developed. The FIB system was used first to prepare a site-specific region for X-ray microanalysis followed by the acquisition of an electron-beam generated X-ray spectral image. A small section of material was then removed by the FIB, followed by the acquisition of another X-ray spectral image. This serial sectioning procedure was repeated 10–12 times to sample a volume of material. The series of two-spatial-dimension spectral images were then concatenated into a single data set consisting of a series of volume elements or voxels each with an entire X-ray spectrum. This four-dimensional (three real space and one spectral dimension) spectral image was then comprehensively analyzed with Sandia's automated X-ray spectral image analysis software. This technique was applied to a simple Cu-Ag eutectic and a more complicated localized corrosion study where the powerful site-specific comprehensive analysis capability of tomographic spectral imaging (TSI) combined with multivariate statistical analysis is demonstrated.

Keywords

tomographyspectral imagingmultivariate statistical analysismultivariate curve resolution3D chemical analysistomographic spectral imagingserial sectioning3D microanalysis
Type
50 YEARS OF X-RAY MAPPING
Information
Microscopy and Microanalysis , Volume 12 , Issue 1 , February 2006 , pp. 36 - 48
Copyright
2006 Microscopy Society of America

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References

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Figure6 Ag

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Figure6 Cu

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Figure8 Ag anaglyph

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Figure8 Cu anaglyph

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Figure11 corrosion

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