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

陶瓷材料界面结构TEM原位系统的开发

• 批准号: 13555169
• 负责人: IKUHARA Yuichi
• 金额: $ 8.06万
• 依托单位: The University of Tokyo
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 2001
• 资助国家: 日本
• 起止时间: 2001 至 2003
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-13555169/
• 关键词: Side entry holder; Finite element method; High resolution electron microscopy; In-situ Observation; Stress; Voltage; Current; 電流; 高分解能電子顕微鏡法; 電圧

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.

这项研究的目的是通过原位透射电子显微镜定量地表征陶瓷界面中原子和电子结构。在今年，我们最终设计了原位固定器来表征界面功能，并将此技术应用于多个模型系统。我们在以下几点开发了该项目，日本东京大学优质陶瓷中心和Topcon EM Service Co.（1）开发新设计的现场tem持有者开发了界面功能，通过结合在三个机构实验实验制造的零件来开发新设计的界面功能。在这种情况下，电压施加的组件，温度测量组件和。优化了真空凹凸附着，并定量确认电压和温度的精度。此外，发达的TEM持有器是在温度中的高分辨率杆件中引入的，并且能够通过优化测量条件来构建了能够同时表征ED和EEL的系统。结果，在1300℃时达到了点点分辨率，在高温下，鳗鱼的能量分辨率达到0.8EV。此外，构建了获得高质量动态图像的CCD系统，并确认该系统中的漂移量在2nm/min之内。结果，在晶界和错位上，微观和电子结构的动态行为成功地测量了高温下的晶格缺陷的行为，用于氧化铝，氧化氧化氧化氧化氧基。钛酸，氧化锌等。

项目成果

Katsuyuki Matsunaga 他: "First-principles calculations of intrinsic defects in Al_2O_3"Physical Review B. 68. 085110-1-085110-9 (2003)

Katsuyuki Matsunaga 等：“Al_2O_3 固有缺陷的第一原理计算”Physical Review B. 68. 085110-1-085110-9 (2003)

C.Iwamoto, X.Q..Shen, H.Okumura, H.Matsuhata, Y.Ikuhara: "Structure Analysis of GaN Thin Film with Inversion Domains by High Voltage Atomic Resolution Microscopy"Mater.Trans.. 43. 1542-1546 (2002)

C.Iwamoto、X.Q..Shen、H.Okumura、H.Matsuhata、Y.Ikuhara：“通过高压原子分辨率显微镜对具有反转域的 GaN 薄膜进行结构分析”Mater.Trans.. 43. 1542-1546 (2002)

Atsutomo Nakamura 他: "Conducting nanowires in insulating ceramics"Nature Materials. 2. 453-456 (2003)

Atsutomo Nakamura 等人：“绝缘陶瓷中的导电纳米线”《自然材料》2. 453-456 (2003)。

Yuichi Ikuhara: "Towards New Transmission Electron Microscopy in Advanced Ceramics"J.Ceram.Soc.Jpn.. 110. 139-145 (2002)

Yuichi Ikuhara：“迈向先进陶瓷中的新型透射电子显微镜”J.Ceram.Soc.Jpn.. 110. 139-145 (2002)

K.Matsunaga, T.Tanaka, T.Yamamoto, Y.Ikuhara: "First-principles calculations of intrinsic defects in Al_2O_3"Physical.Review B. 68. 085110-1-085110-9 (2003)

K.Matsunaga、T.Tanaka、T.Yamamoto、Y.Ikuhara：“Al_2O_3 中固有缺陷的第一原理计算”Physical.Review B. 68. 085110-1-085110-9 (2003)