Nicolas Dumaresq, Nicolas Brodusch, Stéphanie Bessette, Raynald Gauvin
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引用次数: 0
摘要
随着对新型光束敏感材料(如锂离子电池中使用的锂基化合物)表征需求的不断增加,电子显微镜中的电子束损伤问题在材料研究中变得越来越严重。为了避免辐射损伤,使用低温电子显微镜(Cryo-EM)已成为一种常见的做法,但在传统的 TEM/STEM 中,高加速电压(200-300 keV)仍可能会产生连锁损伤。在这项工作中,对 h-BN、TiB2 和 TiN 化合物在 30、20 和 10 keV 加速电压下的电子能量损失光谱进行了探索。在低至 10 keV 的加速电压下,成功观测到了所有 Ti L2、3、N K 和 B K 边缘。使用多线性最小平方(MLLS)程序对所有三种样品进行了精确的元素定量,其标准偏差最多为 5%,完全在用于定量的非弹性部分截面计算误差范围之内。这些结果表明了使用低电压 EELS 的巨大潜力,这是向无损分析迈出的又一步。
Elemental quantification using electron energy-loss spectroscopy with a low voltage scanning transmission electron microscope (STEM-EELS)
Electron beam damage in electron microscopes is becoming more and more problematic in material research with the increasing demand of characterization of new beam sensitive material such as Li based compounds used in lithium-ion batteries. To avoid radiolysis damage, it has become common practice to use Cryo-EM, however, knock-on damage can still occur in conventional TEM/STEM with a high-accelerating voltage (200–300 keV). In this work, electron energy loss spectroscopy with an accelerating voltage of 30,20 and 10 keV was explored with h-BN, TiB2 and TiN compounds. All Ti L2,3, N K and B K edges were successfully observed with an accelerating voltage as low as 10 keV. An accurate elemental quantification for all three samples was obtained using a multi-linear least square (MLLS) procedure which gives at most a 5 % of standard deviation which is well within the error of the computation of the inelastic partial-cross section used for the quantification. These results show the great potential of using low-voltage EELS which is another step towards a knock-on damage free analysis.
期刊介绍:
Ultramicroscopy is an established journal that provides a forum for the publication of original research papers, invited reviews and rapid communications. The scope of Ultramicroscopy is to describe advances in instrumentation, methods and theory related to all modes of microscopical imaging, diffraction and spectroscopy in the life and physical sciences.