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.

本研究的目的是用原位电子显微镜对陶瓷界面的原子和电子结构进行定量表征。在这一年里，我们终于设计了用于表征界面功能的原位瞬变电磁场保持器，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，在以下几个方面开发了本项目。(1)原位透射电子显微镜系统的开发我们结合三个研究所的实验零件，开发了新设计的原位透射电子显微镜夹持器，用于表征界面功能。在这种情况下，电压施加组件、温度测量组件和。对真空度进行了优化，并定量验证了电压和温度测量的准确性。此外，在TEMP的高分辨率极片中引入了所研制的瞬变电磁波保持器，并通过优化测量条件，构建了能同时表征EDS和EELS的系统。结果表明，在1300℃下，点-点分辨率达到0.2 nm，高温下能量分辨率达到0.8 eV。此外，还建立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2 nm/min以内。(2)演示实验新研制的用于表征界面功能的原位透射电子显微镜夹持器已应用于多种材料体系。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，以及高温下晶格缺陷的行为。钛酸盐、氧化锌等。

项目成果

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)

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)

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)

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)