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Trial production of single-crystal X-ray diffractometer with 2D detector for high-pressure crystallography

高压晶体学用二维探测器单晶X射线衍射仪的试制

基本信息

批准号：
12354008
负责人：
MATSUSHITA Nobuyuki
金额：
$ 27.57万
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 (A)
财政年份：
2000
资助国家：
日本
起止时间：
2000 至 2003
项目状态：
已结题

项目摘要

A single-crystal X-ray diffractometer with Imaging Plate(IP) as a two dimensional detector was assessed suitable for structure analysis of metal complexes. X-ray diffraction data were measured for a number of single-crystals of various metal complexes using the IP X-ray diffractometer, and their structure analyses were performed To compare with these results, ten of their metal complexes were also measured by using a 4-circle X-ray diffractometer, which is a typical one for the single-crystal structure analysis. The results of the analyses from the IP X-ray diffractometer were satisfactory.A diamond-anvil-cell (DAC) being able to be mount with the IP X-ray diffractometer was developed as a high-pressure apparatus. That is a 40 mmφ DAC, which is lather than a typical DAC for single-crystal diffraction. A goniometer-head was also developed suitable for the 40 mmφDAC and the IP X-ray diffractometer.A high precise drilling machine for gasket hole and various jigs were manufactured to precisely manipulate very small single crystals in the DAC.A lighting system, a beam-stopper, and collimaters around the goniometer were rebuilt to mount the DAC on the IP X-my diffractometer.Movement of the goniometer with DAC was checked It is confirmed that the collision and any other trouble were not happened in the movement As a torsion of the goniometer-head was, however, observed due to the weight of the DAC in the check process, the goniometer-head was rebuilt to strengthen it.Measurement procedures and technique were studied and developed for the single crystal in the DAC on the IP X-ray diffractometer.

用成像板(IP)作为二维探测器的单晶X射线衍射仪适用于金属络合物的结构分析。用IP-X-射线衍射仪测量了几种不同金属络合物单晶的X射线衍射数据，并对它们的结构进行了分析，与这些结果相比较，还用四圆X-射线衍射仪测量了它们的10种金属络合物的结构，这是单晶结构分析的典型仪器。IP-X-射线衍射仪的分析结果令人满意。研制了一种可与IP-X-射线衍射仪一起安装的钻石压腔(DAC)高压装置。这是一个40 mm的φ数模转换器，它比用于单晶衍射的典型数模转换器起泡。还研制了适用于40 mmφ数模转换器和激电X射线衍射仪的测角头。研制了一台高精度的垫片孔钻床和各种夹具，以精确操作DAC中的微小单晶。改造了测角仪周围的照明系统、挡光器和准直器，将数模转换器安装在IP X-My衍射仪上。检查了测角仪与数模转换器的移动情况，确认在移动过程中没有发生碰撞和任何其他故障，但由于检查过程中观察到数模转换器的重量，对测角头进行了加固改造，研究开发了IP-X-射线衍射仪上DAC中单晶的测量方法和技术。