Specimen Plate Preparation for a Little Amount Specimen in X-ray Powder Diffraction
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摘 要
从对参与衍射的试样体积(宽度)、入射X射线在试样表面的总光量和亮度及X射线被试样吸收三个方面在扫描过程中的变化的分析出发,讨论了在试样量少到不能以薄层填满整个试样槽时,如何制作试样板以得到衍射强度高的高质量衍射谱的方法。在固定发散狭缝宽度的条件下,为使参与衍射的试样面积大,使长度方向的试样尺寸与X射线管中线焦点的长度相同比试样宽度等于试样槽宽度更有利于得到较高的衍射强度。但参与衍射的试样体积会在高θ角时随θ增加而减少。如用可变狭缝,则在全扫描过程中,全部试样始终参与衍射,衍射强度更高,但入射光光通量随θ增加而增加。如改用细条状试样及不需扫描的德拜-谢乐或纪尼叶衍射几何,则入射光光通量和参与衍射的试样体积均不随θ角变化。
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Abstract
For getting a high quality X-ray powder diffraction pattern having higher diffraction intensity when there is only a little specimen which is not enough to spread a film in a specimen groove on a specimen plate, the preparation of a specimen plate was discussed. The discussion was based on the analysis of the change of specimen volume (width) taken part in diffraction, X-ray flux and brilliance on specimen surface, X-ray absorption by specimen in scanning. Under the condition of the width of divergence slit (DS) is fixed,for getting the largest specimen area taken part in the diffraction that the specimen size on the direction of length equals the length of the line focus in X-ray tube is better than that the specimen size on the direction of width is equal to the width of the specimen groove. But in this case the specimen volume (width) taken part in diffraction decrease with the increase of θin the range of highθ. If the slit is adjustable, the whole of the specimen in the specimen groove always take part in the diffraction. Therefore the diffraction intensity is higher. But the flux of incident X-ray is increased with the increase ofθ. If the specimen is filled in a capillary,the diffraction geometry change to Debye-Scherrer geometry or Guinier geometry which do not scanning, the flux of incident X-ray and the specimen volume (width) taken part in diffraction does not change with θ.
中图分类号 O434.1
所属栏目 试验技术与方法
基金项目
收稿日期 2010/3/2
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备注马礼敦(1935-),男,教授。
引用该论文: MA Li-dun. Specimen Plate Preparation for a Little Amount Specimen in X-ray Powder Diffraction[J]. Physical Testing and Chemical Analysis part A:Physical Testing, 2011, 47(3): 146~150
马礼敦. X射线粉末衍射少量试样的试样板制作[J]. 理化检验-物理分册, 2011, 47(3): 146~150
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参考文献
【1】程利芳,杨传铮.多晶X射线衍射仪中填样宽度效应的研究[C]//理学中国用户论文集.长春:[s.n.],2008(2):82-87.
【2】张杰.多晶X射线衍射测量结果的一些影响因素[C]//第十届全国X射线衍射学术大会论文摘要集.上海:[s.n.],2009:300-303.
【3】马礼敦.近代X射线多晶体衍射———实验技术与数据分析[M].北京:化学工业出版社,2004:411-413,260-265.
【2】张杰.多晶X射线衍射测量结果的一些影响因素[C]//第十届全国X射线衍射学术大会论文摘要集.上海:[s.n.],2009:300-303.
【3】马礼敦.近代X射线多晶体衍射———实验技术与数据分析[M].北京:化学工业出版社,2004:411-413,260-265.
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