Shimada Yusuke, Yoshida Kenta, Inoue Koji, Shiraishi Takahisa, Kiguchi Takanori, Nagai Yasuyoshi, Konno Toyohiko J
Institute for Materials Research, Tohoku University, Katahira, Aoba-ku, Sendai, Miyagi, Japan.
International Research Center for Nuclear Materials Science, Institute for Materials Research, Tohoku University, Oarai, Ibaraki, Japan.
Microscopy (Oxf). 2019 Jun 1;68(3):271-278. doi: 10.1093/jmicro/dfz010.
The in situ annealing observation in transmission electron microscope (TEM) is one of the effective methods for imaging thermally induced microstructural changes. For applying this dynamical characterization to bulk samples fabricated by ion-milling, electro-polishing or focused ion beam (FIB) mill, it is generally needed to use a heating-pot type system. We here report an initial trial to improve the spatial and temporal resolution during the in-situ annealing observation of bulk samples using a spherical aberration corrected (AC) TEM with a new thermal control unit. The information limit of 1.5 Å and the point resolution of 2.0 Å are achieved under isothermal annealing at 350°C, which is the same resolution at room temperature, and it is affected strongly of sample drift by the temperature variation. The sample is heated at a heating rate of +1.0°C/s, the drift distance observed by a TV readout speed CCD camera is less than 2.0 Å/s.
透射电子显微镜（TEM）中的原位退火观察是对热诱导微观结构变化进行成像的有效方法之一。对于通过离子铣削、电解抛光或聚焦离子束（FIB）铣削制备的块状样品应用这种动态表征，通常需要使用加热罐式系统。我们在此报告了一项初步试验，即使用配备新型热控单元的球差校正（AC）TEM，在块状样品的原位退火观察过程中提高空间和时间分辨率。在350°C等温退火条件下实现了1.5 Å的信息极限和2.0 Å的点分辨率，这与室温下的分辨率相同，并且温度变化对样品漂移有很大影响。样品以+1.0°C/s的加热速率加热，通过电视读出速度CCD相机观察到的漂移距离小于2.0 Å/s。
