X-射线衍射仪中样品架对物相分析的影响  

Influence of sample holder on phase analysis in X-ray diffractometer

作　　者：李丹 林丽萍 胡准 LI Dan;LIN Liping;HU Zhun(Instrumental Analysis Center,School of Chemical Engineering and Technology,Xi'an Jiaotong University,Xi'an 710049,China)

机构地区：[1]西安交通大学化学工程与技术学院,公共分析测试中心,陕西西安710049

出　　处：《实验技术与管理》2021年第1期36-39,共4页Experimental Technology and Management

基　　金：陕西省自然科学基金青年项目(2017JQ2016)。

摘　　要：由于X-射线衍射分析仪具有操作简单、无损样品、信息全面等优点,是目前进行物相分析的重要方法之一。但在实际操作过程中,样品架自身的衍射信号会影响样品结构的解析,因此X-射线衍射仪中样品架的选择是快速准确得到样品晶体结构及物相分析的关键。该文基于岛津XRD-6100衍射仪,通过对比铝样品架、树脂样品架、无反射样品架、载玻片及自制凹槽样品架,研究样品架对样品衍射信号的影响。结果表明:不同样品架因其性质不同有各自明确的背景峰。若样品量充足,晶型好的样品对于样品架的选择并无特殊的要求,为了得到更高的峰强度,建议使用常规的铝制或树脂样品架;若样品量少且多为非晶态馒头峰的样品,需考虑样品架对其X-射线衍射峰的影响,建议使用无反射样品板,或者以35°为界,特征峰在35°之前建议使用铝制样品架,35°之后建议使用树脂样品架;载玻片和凹槽样品架主要用于特殊形状规格样品的测试。X-ray diffraction analyzer is one of the important methods for phase analysis because of its advantages of simple operation, non-destructive sample and comprehensive information. However, the sample holder with distinct materials can affect the diffraction of the sample in real operation. Therefore, the proper selection of sample holders is important to get the precise information on the fine structure of samples–crystallite size, crystallite type and chemical composition, etc. In this paper, the sample holders with various materials, i.e., aluminum, resin, non-reflecting material, slide glass and self-made groove, are applied to investigate the effect of materials on the diffraction of samples. The results show that different sample frames have their own clear back-view peaks due to their different properties. If the sample quantity is sufficient, it is recommended to use conventional aluminum or resin sample holders in order to obtain higher peak strength. If the sample quantity is small and most samples are of amorphous steamed bread peak, the influence of sample rack on X-ray diffraction peak should be considered. It is suggested to use non reflective sample plate or take 35° as the boundary. Aluminum sample holder is recommended before 35° and resin sample holder is recommended after 35° for characteristic peak. Slide and groove sample holders are mainly used for testing samples with special shape and specification.

关 键 词：精密仪器 X-射线衍射分析 样品架 

分 类 号：G312[文化科学] O632[理学—高分子化学]