传输电子显微镜中的质量厚度测量:用于定量EDS分析的单一标准方法
Thomas J Zega1, Jane Y Howe2, Devin L Schrader3
1Lunar and Planetary Laboratory, Materials Science and Engineering, University of Arizona, 1629 E. University Blvd., Tucson, AZ 85721, USA.
概括
在扫描传输电子显微镜 (STEM) 中优化X射线分析对于材料科学至关重要. 调整样本持有器的方向可以最大限度地减少X射线遮,从而实现定量组合分析的高精度.
科学领域:
- 材料科学 材料科学 材料科学
- 分析化学 分析化学
- 电子显微镜电子显微镜
背景情况:
- 在扫描传输电子显微镜 (STEM) 中使用能量分散式X射线光谱 (EDS) 的定量组成分析对于材料的表征至关重要.
- 聚焦离子束 (FIB) 制备通常用于创建电子透明样本,但可以引入影响分析的工件.
研究的目的:
- 评估FIB准备的SrTiO3,CaTiO3和Fe硫化物样本的定量EDS分析的单一标准方法.
- 调查和减轻X射线影像对定量EDS准确度的影响.
- 优化分析几何学,以提高STEM-EDS的精度和准确性.
主要方法:
- 使用STEM对SrTiO3,CaTiO3和Fe硫化物的FIB段进行了定量EDS分析.
- 绘制和分析了X射线影像效应.
- 传输电子显微镜中的样本持有器方向被调整以优化对EDS探测器的视线.
- 结果与电子微探针的定量波长分散光谱学 (WDS) 进行了比较.
主要成果:
- 证实X射线的遮蔽是影响定量EDS分析的重要因素.
- 在STEM样本持有器中调整FIB半网格的方向有效地减少了X射线遮蔽.
- 当将STEM-EDS数据与电子微探测器WDS进行比较时,获得了2%的精度.
- 通过优化分析几何学,获得了5%内的精度.
结论:
- 优化的分析几何学,特别是样本持有者的方向,对于STEM中精确的定量EDS分析至关重要.
- 单一标准的方法,当与优化的几何学相结合时,为材料科学应用提供可靠的组成数据.
- 这种方法提供了一种途径,可以在FIB准备的样本中实现高精度,准确的元素定量.
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