Dumaresq Nicolas, Brodusch Nicolas, Bessette Stéphanie, Gauvin Raynald
Department of Materials Engineering, McGill University, Montreal, Quebec, Canada.
Department of Materials Engineering, McGill University, Montreal, Quebec, Canada.
Ultramicroscopy. 2024 Aug;262:113977. doi: 10.1016/j.ultramic.2024.113977. Epub 2024 Apr 23.
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, TiB and TiN compounds. All Ti L 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.
随着对新型束敏感材料(如用于锂离子电池的锂基化合物)表征需求的增加,电子显微镜中的电子束损伤在材料研究中变得越来越成问题。为了避免辐射分解损伤,使用低温电子显微镜(Cryo-EM)已成为常见做法,然而,在具有高加速电压(200 - 300 keV)的传统透射电子显微镜(TEM)/扫描透射电子显微镜(STEM)中仍可能发生撞击损伤。在这项工作中,使用h-BN、TiB和TiN化合物探索了加速电压为30 keV、20 keV和10 keV的电子能量损失谱。在低至10 keV的加速电压下成功观察到了所有Ti L、N K和B K边。使用多线性最小二乘法(MLLS)程序对所有三个样品进行了准确的元素定量分析,该程序给出的标准偏差最多为5%,这完全在用于定量分析的非弹性部分截面计算误差范围内。这些结果显示了使用低电压电子能量损失谱(EELS)的巨大潜力,这是朝着无撞击损伤分析迈出的又一步。