Uemura Naoki, Egoshi Tomoya, Murakami Koichi, Kizuka Tokushi
Department of Materials Science, Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1, Tennoudai, Tsukuba, Ibaraki 305-8573, Japan.
Department of Materials Science, Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1, Tennoudai, Tsukuba, Ibaraki 305-8573, Japan.
Micron. 2022 Jun;157:103244. doi: 10.1016/j.micron.2022.103244. Epub 2022 Mar 16.
We developed high temperature in situ transmission electron microscopy using a high-density laser irradiation device (nominal maximum laser density ~9.4 GW/m) and a corresponding heat shielding sample mount device. The spatial line resolution of the microscope was maintained to be 0.14 nm at ambient temperatures after the installation of the laser irradiation device. The system was applied to the investigation of high temperature structural variation in tungsten plates. When the laser power was increased up to irradiation densities of approximately 61-280 MW/m (laser source output: 130-590 mW) to degrade tungsten plates, the microscope was undamaged. The surface dynamics was observed in situ by lattice imaging at irradiation densities of approximately 61-75 MW/m (laser source output: 130-160 mW); the spatial line resolution of the microscope was maintained to be 0.23 nm at high temperatures. It was expected that high temperature observation is realized using this heating system, which can be applied to the investigation of various advanced heat-resistant materials. We found using this heating system that degradation in tungsten plates started from surfaces and progressed through the preferential generation of characteristic defects, such as atomistic and nanometer holes and rods, and their subsequent evolution in thinner regions during the heating. It was demonstrated that the holes and rod were truncated with {110} sidewalls, i.e., these surfaces were stable in tungsten at high temperatures.
我们使用高密度激光辐照装置(标称最大激光密度约为9.4 GW/m)和相应的隔热样品台装置开发了高温原位透射电子显微镜。安装激光辐照装置后,显微镜在环境温度下的空间线分辨率保持为0.14 nm。该系统被应用于研究钨板的高温结构变化。当激光功率增加到约61 - 280 MW/m的辐照密度(激光源输出:130 - 590 mW)以降解钨板时,显微镜未受损。在约61 - 75 MW/m的辐照密度(激光源输出:130 - 160 mW)下通过晶格成像原位观察表面动力学;显微镜在高温下的空间线分辨率保持为0.23 nm。预计使用这种加热系统可以实现高温观察,该系统可应用于研究各种先进的耐热材料。我们使用这种加热系统发现,钨板的降解从表面开始,并通过优先产生特征缺陷(如原子级和纳米级的孔洞和棒状物)以及它们在加热过程中在较薄区域的后续演变而进行。结果表明,孔洞和棒状物具有{110}侧壁截断,即这些表面在高温下的钨中是稳定的。