Kotula Paul G, Keenan Michael R, Michael Joseph R
Sandia National Laboratories, Materials Characterization Department, P.O. Box 5800, MS0886, Albuquerque, NM 87185-0886, USA.
Microsc Microanal. 2006 Feb;12(1):36-48. doi: 10.1017/S1431927606060193.
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.
已开发出一种使用配备能量色散X射线光谱仪（EDS）的组合扫描电子显微镜（SEM）/聚焦离子束（FIB）系统的全面三维（3D）微分析程序。首先使用FIB系统为X射线微分析准备一个特定位置区域，然后获取电子束产生的X射线光谱图像。然后用FIB去除一小部分材料，接着获取另一幅X射线光谱图像。重复此连续切片程序10 - 12次以对一定体积的材料进行采样。然后将一系列二维光谱图像拼接成一个由一系列体积元素或体素组成的单一数据集，每个体素都有完整的X射线光谱。然后使用桑迪亚的自动X射线光谱图像分析软件对这个四维（三个实空间和一个光谱维度）光谱图像进行全面分析。该技术应用于简单的铜 - 银共晶以及更复杂的局部腐蚀研究，其中展示了断层光谱成像（TSI）强大的特定位置综合分析能力与多变量统计分析相结合的情况。
