Apparatus for rapid analysis of wide-angle X-ray diffraction patterns at high temperatures

高温下广角 X 射线衍射图样快速分析装置

• 批准号: 59880007
• 负责人: HASHIZUME Hiroo
• 金额: $ 4.67万
• 依托单位: Tokyo Institute of Technology
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Developmental Scientific Research
• 财政年份: 1984
• 资助国家: 日本
• 起止时间: 1984 至 1985
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-59880007/
• 关键词: X-ray position detector; powder crystal; high-temperature; structure analysis

An apparatus has been developed which permits rapid recording of Xray diffraction patterns from inorganic powder crystals at high temperatures. The apparatus is built on a newly designed cylindrical position sensitive gas detector with an angular coverage of 120 degree of arc. The detector uses a thin metal blade in the anode and is operated in the selfquenching streamer mode. The anode radius is as large as 250mm to be compatible with most high-temperature specimen chambers. A delay line reads out the position signal from the strip cathodes to give an angular resolution of 0.05 degree of arc. The detector is mounted on a two-axis goniometer to detect a diffraction pattern from a stationary powder specimen. To suppress the broadening of reflection lines in the detected pattern, a slit system limits the angular divergence of X-rays incident on the planar specimen. The data, collected in a multi-channel analyzer memory, is read into a computer for analysis by a pattern fitting program. A test made with a standard corundom specimen demonstrates the speed and precision of the apparatus: a diffraction pattern substantially better in resolution has been obtained in a recording time of 1/80 as compared with a standard theta-two theta scanning method. The experimental pattern has been fitted well with the calculated one to give structural parameters in good agreement with the published data for this material. The usefulness of the apparatus in high-temperature works has been shown in an application, where the structure of the delta phase in bismuth oxide is refined at 784 degree Celsius.

已经开发了一种设备，该设备允许在高温下从无机粉末晶体中快速记录X射线衍射图。该设备建立在新设计的圆柱位置敏感气体探测器上，其角度覆盖率为120度。检测器在阳极中使用薄金属刀片，并在自Quenching流媒体模式下操作。阳极半径高达250mm，可与大多数高温标本室兼容。延迟线读取了从带状阴极的位置信号，得出的角度分辨率为0.05度。将检测器安装在两轴的角度计上，以检测固定粉末样本的衍射图。为了抑制检测到的模式中反射线的扩展，狭缝系统限制了在平面样品上入射X射线的角度差异。收集在多通道分析仪内存中的数据被读取到计算机中，以通过模式拟合程序进行分析。用标准的圆锥形标本进行的测试证明了设备的速度和精度：与标准的Theta-Two-Two-Two Theta扫描方法相比，在记录时间为1/80的衍射模式中，分辨率的分辨率要好得多。实验模式与计算出的模式非常适合，以使结构参数与该材料的已发布数据吻合。设备在高温作品中的有用性已在一个应用中显示，在该应用中，在784度摄氏二碳中，氧化物中三角洲相的结构进行了完善。