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.

本研究的目的是通过原位透射电子显微镜定量表征陶瓷界面中的原子和电子结构。今年，我们最终设计了原位TEM支架来表征界面功能，并将该技术应用于多个领域。我们与东京大学、日本精细陶瓷中心和拓普康 EM 服务有限公司合作，在以下几点上开发了该项目。(1)原位 TEM 系统的开发我们开发了新设计的原位 TEM 系统。通过结合三个研究所实验制作的部件来表征界面功能的 TEM 支架，对电压施加组件、温度测量组件和真空室附件进行了优化，并定量确认了电压和温度的准确性。此外，将开发的 TEM 支架引入 TEMP 的高分辨率极片中，并通过优化测量条件构建了能够同时表征 EDS 和 EELS 的系统。在1300℃下分辨率达到O.2Onm，高温下EELS能量分辨率达到0.8eV，并构建了获得高质量动态图像的CCD系统，并对其漂移量进行了研究。系统被证实在2nm/min之内。(2)演示实验新开发的用于表征界面功能的原位TEM支架被应用于多种材料系统。成功测量了氧化铝、氧化锆、钛酸盐、氧化锌等的晶界和位错处的微观结构和电子结构的行为以及高温下晶格缺陷的行为。

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)