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进动技术和电子衍射测量法作为晶体结构分析和化学键测定的新工具。

Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination.

作者信息

Avilov A, Kuligin K, Nicolopoulos S, Nickolskiy M, Boulahya K, Portillo J, Lepeshov G, Sobolev B, Collette J P, Martin N, Robins A C, Fischione P

机构信息

Institute of Crystallography of Russian Academy of Sciences, Leninsky prosp. 59, Moscow 119333, Russian Federation.

出版信息

Ultramicroscopy. 2007 Jun-Jul;107(6-7):431-44. doi: 10.1016/j.ultramic.2006.09.006. Epub 2006 Dec 20.

Abstract

We have developed a new fast electron diffractometer working with high dynamic range and linearity for crystal structure determinations. Electron diffraction (ED) patterns can be scanned serially in front of a Faraday cage detector; the total measurement time for several hundred ED reflections can be tens of seconds having high statistical accuracy for all measured intensities (1-2%). This new tool can be installed to any type of TEM without any column modification and is linked to a specially developed electron beam precession "Spinning Star" system. Precession of the electron beam (Vincent-Midgley technique) reduces dynamical effects allowing also use of accurate intensities for crystal structure analysis. We describe the technical characteristics of this new tool together with the first experimental results. Accurate measurement of electron diffraction intensities by electron diffractometer opens new possibilities not only for revealing unknown structures, but also for electrostatic potential determination and chemical bonding investigation. As an example, we present detailed atomic bonding information of CaF(2) as revealed for the first time by precise electron diffractometry.

摘要

我们开发了一种新型快速电子衍射仪,用于晶体结构测定,具有高动态范围和线性度。电子衍射(ED)图案可在法拉第笼探测器前进行连续扫描;几百个ED反射的总测量时间可为几十秒,对所有测量强度具有较高的统计精度(1-2%)。这种新工具可安装到任何类型的透射电子显微镜(TEM)上,无需对镜筒进行任何修改,并与专门开发的电子束进动“旋转星”系统相连。电子束进动(文森特-米德格利技术)减少了动力学效应,也使得能够使用精确强度进行晶体结构分析。我们描述了这种新工具的技术特性以及首批实验结果。通过电子衍射仪精确测量电子衍射强度不仅为揭示未知结构,也为静电势测定和化学键研究开辟了新的可能性。作为一个例子,我们展示了首次通过精确电子衍射法揭示的CaF₂的详细原子键合信息。

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