Construction of a very low temperature specimen stage for the 400kV Analytical Atom Resolution Eletron Microscope.

为 400kV 分析原子分辨率电子显微镜构建极低温样品台。

• 批准号: 60850006
• 负责人: HASHIMOTO Hatsujirou
• 金额: $ 10.88万
• 依托单位: Okayama University of Science (1986)Osaka University (1985)
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Developmental Scientific Research
• 财政年份: 1985
• 资助国家: 日本
• 起止时间: 1985 至 1986
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-60850006/
• 关键词: High resolution electron microscopy; Atomic structure; Herium stage; Low temperature specimen stage; 超伝導材料; 原子直視電子顕微鏡法; 極低温試料ホルダー; 照射損傷

The present research aimed to construct the very low temperature specimen stage adaptable to 400kV Analytical Atom Resolution Electron Microscope (AARM). The low temperature stage has been made by paying the careful attention which enable every performance of the 400kV AARM to be preserved. For this aim, Both the 400kV AARM in Osaka University and in JEOL Ltd. has been used for testing the capabilities of the present very low temperature specimen stage.Specimens can be tilted in both X and Y axes with +10 , which is useful to study the crystalline specimens. In order to detect the characteristic X-ray to analyze the materials and secondary electrons to see the SEM images, the present low temperature specimen stage has the side entry goniometer style. However,this style of the goniometer is very weak for mechanical vibration and rather difficult to obtain high resolution images. Though elimination of the vibration is not impossible, since the fund is limited, it was aimed and succeeded … More that the resolution is 2.5 nm and the lowest temperature of a specimen is 30 K.Since it is clear that the electron microscope must have the resolution of 0.2 -0.3 nm in order to see the images of atoms directly, another specimen holder with high resolution and very low temperature ( the temperature of the liquid helium ) adaptable to the specimen stage in the superconducting electron lens (SCEL) has been made for reference. Though this specimen stage can reveal the atomic structure of the specimen in liquid helium temperature, the characteristic X-ray cannot be detected and also no temperature variation can be carried out. However element analysis can be carried out using the electron energy loss spectrometer fabricated at the bottom of the microscope. Movement of atoms and their clusters can also be observed by TV-camera and recorded in video tape recorder (VTR).Using the side entry very low temperature specimen stage to the AARM together with the low temperature stage in the SCEL, some observations of images of a superconducting material <Nb_3> Sn at various temperatures from room temperature to 30 K, atom resolution images of Th-pyromeritate at 5 K and the variation of Th-pyromeritate by electron irradiation at 5 K have been carried out. Some variation of the images were recorded in VTR.After the present research, it was known that the performance of the low temperature specimen stage can be improved. After some improvements, the temperature of the present low temperature specimen stage was lowered to be 20 K but the mechanical vibration becomes as large as 20 nm in the specimen position. The origin of the vibration is now under studying, but the results obtained so far are reported.The present investigations are now applying to the Okayama University of Science and the Ministry of Education , science and Culture to install 400 kV AARM in Okayama University of Science and planning to carry out the extensive low temperature research in atomic scale together with low temperature research group. Less

本研究旨在构建适用于400kV分析原子分辨率电子显微镜（AARM）的极低温样品台。低温阶段经过精心设计，使 400kV AARM 的各项性能得以保留。为此，大阪大学和 JEOL 有限公司的 400kV AARM 已用于测试当前极低温样品台的能力。样品可以在 X 和 Y 轴上倾斜 +10°，这对于研究晶体样品非常有用。为了检测特征X射线以分析材料和二次电子以查看SEM图像，目前的低温样品台具有侧入式测角仪样式。然而，这种测角仪的机械振动能力很弱，很难获得高分辨率图像。虽然消除振动并非不可能，但由于资金有限，我们的目标是分辨率为2.5 nm，样品最低温度为30 K。显然，电子显微镜必须具有0.2 -0.3 nm的分辨率才能直接看到原子图像，因此需要另一种高分辨率和极低温度（液氦温度）的样品架来适应样品 超导电子透镜（SCEL）阶段已被提出以供参考。该样品台虽然可以揭示液氦温度下样品的原子结构，但无法检测到特征X射线，也无法进行温度变化。然而，可以使用安装在显微镜底部的电子能量损失光谱仪进行元素分析。原子及其团簇的运动也可以通过电视摄像机观察并记录在磁带录像机（VTR）中。利用AARM的侧入式极低温样品台和SCEL中的低温台，对超导材料<Nb_3> Sn在室温至30 K的不同温度下的图像进行了一些观察，Th-焦炭酸在5 K下的原子分辨率图像以及Th-焦炭酸的变化 进行了5K电子辐照。 VTR中记录的图像发生了一些变化。经过目前的研究，我们知道低温样品台的性能可以得到改善。经过一些改进，现有低温样品台的温度降低至20 K，但样品位置的机械振动却达到20 nm。目前正在研究振动的起源，但目前已报告了目前获得的结果。目前的研究正在向冈山理科大学和日本文部科学省申请在冈山理科大学安装400 kV AARM，并计划与低温研究小组一起在原子尺度上进行广泛的低温研究。较少的

项目成果

M. Takeda, H. Yoshida, H. Endoh and H. Hashimoto: "High - resolution electron microscopy of microstructures in <Nb_3> X (A15) superconductors" Proc. 11th International Congress on Electron Microscopy. 863-864 (1986 ( Kyoto ))

M. Takeda、H. Yoshida、H. Endoh 和 H. Hashimoto：“<Nb_3> X (A15) 超导体微观结构的高分辨率电子显微镜”Proc。

H.Yoshida;M.Takeda;H.Hashimoto;H.Endoh: In-situ experiments with high voltage electron microscopes. 229-232 (1986)

H.Yoshida;M.Takeda;H.Hashimoto;H.Endoh：高压电子显微镜的原位实验。

H.Hashimoto;H.Endoh;M.Kuwabara;M.Tomita;Y.Yokota: In-situ experiments with high voltage electron microscopes. 295-310 (1986)

H.Hashimoto;H.Endoh;M.Kuwabara;M.Tomita;Y.Yokota：高压电子显微镜的原位实验。

H. Yoshida, M. Takeda, H. Hashimoto and H. Endoh: "Atomic lattice imperfections in <Nb_3> Sn, <Nb_3> Al and <Nb_3> (Al,Ge) superconductors" In - situ experiments with high voltage electron microscopes. 1. 229-232 (1986 ( Osaka ))

H. Yoshida、M. Takeda、H. Hashimoto 和 H. Endoh：“<Nb_3> Sn、<Nb_3> Al 和 <Nb_3> (Al,Ge) 超导体中的原子晶格缺陷”高压电子显微镜原位实验

H.Yoshida;H.Hashimoto;Y.Yokota;Y.Harada: Proceeding of 18th International Conference on Low Temperature Physics. (1987)

H.Yoshida；H.Hashimoto；Y.Yokota；Y.Harada：第 18 届国际低温物理会议论文集。