Sutter John P, Boada Roberto, Bowron Daniel T, Stepanov Sergey A, Díaz-Moreno Sofía
Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot, Oxfordshire OX11 0DE, UK.
ISIS Neutron and Muon Source, Rutherford Appleton Laboratory, Didcot, Oxfordshire OX11 0QX, UK.
J Appl Crystallogr. 2016 Jul 6;49(Pt 4):1209-1222. doi: 10.1107/S1600576716009183. eCollection 2016 Aug 1.
EXAFS studies on dilute samples are usually carried out by collecting the fluorescence yield using a large-area multi-element detector. This method is susceptible to the 'glitches' produced by all single-crystal monochromators. Glitches are sharp dips or spikes in the diffracted intensity at specific crystal orientations. If incorrectly compensated, they degrade the spectroscopic data. Normalization of the fluorescence signal by the incident flux alone is sometimes insufficient to compensate for the glitches. Measurements performed at the state-of-the-art wiggler beamline I20-scanning at Diamond Light Source have shown that the glitches alter the spatial distribution of the sample's quasi-elastic X-ray scattering. Because glitches result from additional Bragg reflections, multiple-beam dynamical diffraction theory is necessary to understand their effects. Here, the glitches of the Si(111) four-bounce monochromator of I20-scanning just above the Ni edge are associated with their Bragg reflections. A fitting procedure that treats coherent and Compton scattering is developed and applied to a sample of an extremely dilute (100 micromolal) aqueous solution of Ni(NO). The depolarization of the wiggler X-ray beam out of the electron orbit is modeled. The fits achieve good agreement with the sample's quasi-elastic scattering with just a few parameters. The X-ray polarization is rotated up to ±4.3° within the glitches, as predicted by dynamical diffraction. These results will help users normalize EXAFS data at glitches.
对稀释样品的扩展X射线吸收精细结构(EXAFS)研究通常通过使用大面积多元素探测器收集荧光产率来进行。这种方法容易受到所有单晶单色仪产生的“毛刺”影响。毛刺是在特定晶体取向的衍射强度中的尖锐下降或尖峰。如果补偿不当,它们会降低光谱数据质量。仅通过入射通量对荧光信号进行归一化有时不足以补偿毛刺。在钻石光源的最先进摆动器光束线I20 - 扫描上进行的测量表明,毛刺会改变样品准弹性X射线散射的空间分布。由于毛刺是由额外的布拉格反射引起的,因此需要多光束动态衍射理论来理解它们的影响。在此,I20 - 扫描的Si(111)四反射单色仪在镍边缘上方的毛刺与其布拉格反射相关。开发了一种处理相干散射和康普顿散射的拟合程序,并将其应用于极稀(100微摩尔)硝酸镍水溶液样品。对摆动器X射线束在电子轨道外的去极化进行了建模。仅用几个参数,拟合结果就与样品的准弹性散射取得了良好的一致性。如动态衍射所预测的,在毛刺范围内X射线偏振旋转高达±4.3°。这些结果将有助于用户在存在毛刺的情况下对EXAFS数据进行归一化。