Journal
MICROSCOPY AND MICROANALYSIS
Volume 12, Issue 1, Pages 36-48Publisher
CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927606060193
Keywords
tomography; spectral imaging; multivariate statistical analysis; multivariate curve resolution; 3D chemical analysis; tomographic spectral imaging; serial sectioning; 3D microanalysis
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A comprehensive three-dimensional (31)) 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.
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