Development of TEM in-situ system for interface structure in ceramic material

本研究的目的是利用原位透射电镜定量表征陶瓷界面的原子和电子结构。在这一年里，我们最终设计了原位TEM支架来表征界面功能，并将该技术应用于几个模型系统。我们与东京大学，日本精细陶瓷中心和Topcon EM服务公司合作，在以下几点上开发了这个项目。(1)原位TEM系统的研制我们将三所研究所实验制作的零件结合在一起，开发了一种新型的原位TEM支架来表征界面功能。在这种情况下，电压施加组件，温度测量组件和。对真空弧面附件进行了优化，定量地确定了电压和温度的精度。此外，在TEMP的高分辨率极片中引入了开发的TEM支架，并通过优化测量条件构建了能够同时表征EDS和EELS的系统。结果表明，在1300℃时，EELS的点-点分辨率可达0.2 μ m，在高温下，EELS的能量分辨率可达0.8eV。构建了获得高质量动态图像的CCD系统，并确定了该系统的漂移量在2nm/min以内。(2)验证实验：新开发的原位TEM holder用于表征界面功能，并应用于几种材料体系。结果，成功地测量了氧化铝、氧化锆、锶在晶界和位错处的微观和电子结构的动态行为，以及晶格缺陷在高温下的行为。钛酸盐，氧化锌等。

The purpose of this study is to quantitatively characterize the atomic and electronic structures in ceramic interface by in-situ transmission electron microscopy. In this year, we finally designed the in-situ TEM holder to characterize the interfacial function, and applied this technique to several model systems. We developed this project on the following points with the collaboration between University of Tokyo, Japan Fine Ceramic Center and Topcon EM service Co..(1)Development of in-situ TEM systemWe developed newly designed in-situ TEM holder to characterize the interfacial function by combining the parts which were made experimentally at three institutes. In this case, the voltage applied components, the temperature measurement components and. vacuum camber attachments were optimized, and the accuracy for voltage and temperature were quantitatively confirmed. In addition, the developed TEM holder was introduced inside the high-resolution pole-piece in TEMP and the systems to be able to simultaneously characterize EDS and EELS were constructed by optimizing the measurement conditions. As the result, the point-point resolution was attained to O.2Onm at 1300℃, and the energy resolution of EELS was got up to 0.8eV at the high temperature. Furthermore, the CCD system to obtain high quality dynamic images was constructed, and the amount of the drift in this system was confirmed to be within 2nm/min..(2)Demonstration ExperimentsThe newly developed in-situ TEM holder to characterize the interfacial function was applied for several material systems. As the result, the dynamic behavior of micro and electronic structures at grain boundaries and dislocations, the behavior of lattice defects at high-temperatures were successfully measured for alumina, zirconia, strontium. titanate, zinc oxide and so on.