National Institute for Nanotechnology, 11421 Saskatchewan Drive, Edmonton, Canada T6G 2M9.
Micron. 2012 Jan;43(1):8-15. doi: 10.1016/j.micron.2011.07.003. Epub 2011 Jul 14.
Scattering contrast measurements were performed on thin films of amorphous carbon and polycrystalline Au, as well as single-crystal MgO nanocubes. Based on the exponential absorption law, mass-thickness can be obtained within 10% accuracy by measuring the incident and transmitted intensities in the same image. For mass-thickness measurement of a thin amorphous specimen, a small collection semiangle improves the measurement sensitivity, whereas for the measurement of polycrystalline or single-crystal specimens, a large collection semiangle should be used to reduce diffraction-contrast effects. EELS thickness measurements on MgO nanocubes suggest that the Kramers-Kronig sum-rule method (with correction for plural and surface scattering) gives 10% accuracy at medium collection semiangles but overestimates the thickness at small collection semiangles, due to underestimation of the surface-mode scattering. The log-ratio method, with a formula for inelastic mean free path proposed by Malis et al. (1988), provides 10% accuracy at small collection semiangle, while that proposed by Iakoubovskii et al. (2008a) is preferable for medium and large collection semiangles. As a result of this work, we provide recommendations of preferred methods and conditions for local-thickness measurement in the TEM.
对非晶态碳和多晶金薄膜以及单晶 MgO 纳米立方体进行了散射对比测量。基于指数吸收定律,通过在同一图像中测量入射和透射强度,可以在 10%的精度内获得质量厚度。对于薄非晶样品的质量厚度测量,小的采集半角可以提高测量灵敏度,而对于多晶或单晶样品的测量,应该使用大的采集半角以减少衍射对比效应。对 MgO 纳米立方体的 EELS 厚度测量表明,Kramers-Kronig 求和规则方法(对于多重和表面散射进行了修正)在中等采集半角下可达到 10%的精度,但在小采集半角下会高估厚度,这是由于对表面模式散射的低估。对数比法,采用 Malis 等人(1988 年)提出的非弹性平均自由程公式,在小采集半角下可达到 10%的精度,而 Iakoubovskii 等人(2008a)提出的方法则更适合中等和大采集半角。由于这项工作,我们为 TEM 中的局部厚度测量提供了推荐的首选方法和条件。