An Byeong-Seon, Kwon Yena, Cha Hyun-Woo, Kang Min-Chul, Oh Jin-Su, Yang Cheol-Woong
School of Advanced Materials Science and Engineering, Sungkyunkwan University, Suwon, 16419, Korea.
Microsc Res Tech. 2019 Jan;82(1):39-46. doi: 10.1002/jemt.23065. Epub 2018 Oct 8.
The quantity of the crystalline phases present in a nanomaterial is an important parameter that governs the correlation between its properties and microstructure. However, quantification of crystallinity in nanoscale-level applications by conventional methods (Raman spectroscopy and X-ray diffraction) is difficult because of the spatial limitations of sampling. Therefore, we propose a technique that involves using energy-filtered electron diffraction in transmission electron microscopy which offers improved spatial resolution. The degree of crystallinity (DOC) was calculated by separating the crystalline and amorphous intensities from the total intensity histogram acquired by the azimuthal averaging of the zero-loss filtered signals from electron diffraction. In order to validate the method, it was demonstrated that the DOC calculated by zero-loss filtered electron diffraction was consistent with the DOC measured by the area ratio using an amorphous silicon on crystalline silicon standard sample. In addition, the results obtained from zero-loss filtered and conventional electron diffractions were compared. The zero-loss filtered electron diffraction successfully provided the reliable results of the crystallinity quantification. In contrast, the DOC measured using conventional electron diffraction yielded extremely variable results. Therefore, our results provide a crystallinity quantification technique that can extract quantitative information about crystallinity of nanoscale devices by using zero-loss filtered electron diffraction with better reliability than conventional electron diffraction. RESEARCH HIGHLIGHTS: The degree of crystallinity can be measured by separating the crystalline and amorphous intensities from the total intensity histogram acquired by the azimuthal averaging of the zero-loss filtered signals from selected area electron diffraction.
纳米材料中存在的晶相数量是一个重要参数,它决定了材料性能与其微观结构之间的相关性。然而,由于采样的空间限制,用传统方法(拉曼光谱和X射线衍射)对纳米级应用中的结晶度进行量化很困难。因此,我们提出了一种技术,该技术涉及在透射电子显微镜中使用能量过滤电子衍射,它具有更高的空间分辨率。结晶度(DOC)通过从电子衍射的零损失过滤信号的方位角平均获得的总强度直方图中分离出结晶和非晶强度来计算。为了验证该方法,通过使用晶体硅上的非晶硅标准样品,证明了通过零损失过滤电子衍射计算的DOC与通过面积比测量的DOC一致。此外,还比较了零损失过滤电子衍射和传统电子衍射获得的结果。零损失过滤电子衍射成功地提供了可靠的结晶度量化结果。相比之下,使用传统电子衍射测量的DOC产生的结果变化极大。因此,我们的结果提供了一种结晶度量化技术,该技术可以通过使用零损失过滤电子衍射来提取关于纳米级器件结晶度的定量信息,其可靠性优于传统电子衍射。研究亮点:结晶度可以通过从选定区域电子衍射的零损失过滤信号的方位角平均获得的总强度直方图中分离出结晶和非晶强度来测量。