期刊
JOURNAL OF SYNCHROTRON RADIATION
卷 16, 期 -, 页码 83-96出版社
INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S0909049508030859
关键词
centring; diamond anvil cell; high pressure; X-ray diffraction; X-ray diffraction methods; rocking
资金
- Natural Science and Engineering Research Council of Canada
- NRC
- CIHR
- University of Saskatchewan
The distinct X-ray transmission profile obtained by scanning a sample in a diamond anvil cell across a collimated X-ray beam is used to monitor sample displacement brought about by rotation. This measured displacement can in turn be used to calculate, and subsequently correct, the sample position with respect to a centre of rotation. This centring method differs from others also based on transmission in that it does not require a 180 degrees sample rotation, nor does it require prior positioning of the rotation axis in the path of the X-ray beam. After a full description of the method, an example is presented together with an extended record of use to evaluate the method in a practical setting. The practice and benefits of rocking polycrystalline samples during X-ray exposure have also been quantitatively examined. Changing the orientation of the sample grains with respect to the incident beam yields the expected result of a more homogeneous intensity distribution along Debye rings. Interestingly, by limiting the amount of time large grains assume a particular orientation, rocking brings about the added effect of significantly reducing detector saturation. Sample rocking yields more reliable relative intensities, a more appropriate line shape and narrower line width. Data are presented for a calibration standard at ambient pressure as well as a research sample at high pressure.
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