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

本文介绍了一种适合于金属配合物结构分析的X射线单晶衍射仪。使用IP X射线衍射仪测量了许多不同金属配合物的单晶的X射线衍射数据，并进行了它们的结构分析。为了与这些结果进行比较，还使用四圆X射线衍射仪测量了它们的十个金属配合物，这是单晶结构分析的典型仪器。研制了一种可与IP X射线衍射仪配套使用的金刚石压砧（DAC）高压装置。这是一个40 mmφ DAC，比用于单晶衍射的典型DAC更宽。研制了适用于40 mmφDAC和IP X射线衍射仪的测角头，研制了高精度垫片孔钻削机和各种夹具，实现了DAC中微小单晶的精密加工，并设计了照明系统、光束阻挡器、和准直器周围的测角仪被重建，安装在IP X的DAC-我的衍射仪。检查了带有DAC的测角仪的运动，确认在运动中没有发生碰撞和任何其他故障。然而，由于检查过程中DAC的重量，观察到测角仪头的扭转，对测角头进行了改造，对测角头进行了加固，研究和开发了在IP X射线衍射仪上对DAC中单晶进行测量的方法和技术。

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.