Magnard Nicolas P L, Sørensen Daniel R, Kantor Innokenty, Jensen Kirsten M Ø, Jørgensen Mads R V
Department of Chemistry and Nano-Science Center, University of Copenhagen, Copenhagen 2100, Denmark.
Department of Chemistry & iNANO, Aarhus University, Aarhus 8000, Denmark.
J Appl Crystallogr. 2023 May 31;56(Pt 3):825-833. doi: 10.1107/S1600576723004016. eCollection 2023 Jun 1.
Here the use of a broad energy bandwidth monochromator, a pair of BC/W multilayer mirrors (MLMs), is demonstrated for X-ray total scattering (TS) measurements and pair distribution function (PDF) analysis. Data are collected both on powder samples and from metal oxo clusters in aqueous solution at various concentrations. A comparison between the MLM PDFs and those obtained using a standard Si(111) double-crystal monochromator shows that the measurements yield MLM PDFs of high quality which are suitable for structure refinement. Moreover, the effects of time resolution and concentration on the quality of the resulting PDFs of the metal oxo clusters are investigated. PDFs of heptamolybdate clusters and tungsten α-Keggin clusters from X-ray TS data were obtained with a time resolution down to 3 ms and still showed a similar level of Fourier ripples to PDFs obtained from 1 s measurements. This type of measurement could thus open up faster time-resolved TS and PDF studies.
在此展示了使用一种宽能量带宽单色仪，即一对BC/W多层镜（MLM），用于X射线全散射（TS）测量和对分布函数（PDF）分析。在不同浓度下，对粉末样品以及水溶液中的金属氧簇均进行了数据收集。将MLM的PDF与使用标准Si(111)双晶单色仪获得的PDF进行比较，结果表明测量得到的高质量MLM的PDF适用于结构精修。此外，还研究了时间分辨率和浓度对所得金属氧簇PDF质量的影响。从X射线TS数据中获得的七钼酸簇和钨α-凯gin簇的PDF，其时间分辨率低至3 ms，并且与从1 s测量中获得的PDF相比，仍显示出相似水平的傅里叶波纹。因此，这种类型的测量可以开展更快的时间分辨TS和PDF研究。
