A compact high-resolution X-ray powder diffractometer

摘要

A new powder diffractometer operating in transmission mode is described. It can work as a rapid very compact instrument or as a high-resolution instrument, and the sample preparation is simplified. The incident beam optics create pure Cu Kα1 radiation, giving rise to peak widths of ∼0.1° in 2θ in compact form with a sample-to-detector minimum radius of 55 mm, reducing to peak widths of <0.05° in high-resolution mode by increasing the detector radius to 240 mm. The resolution of the diffractometer is shown to be governed by a complex mixture of angular divergence, sample size, diffraction effects and the dimensions of the detector pixels. The data can be collected instantaneously, which combined with trivial sample preparation and no sample alignment, makes it a suitable method for very rapid phase identification. As the detector is moved further from the sample, the angular step from the pixel dimension is reduced and the resolution improves significantly for very detailed studies, including structure determination and analysis of the microstructure. The advantage of this geometry is that the resolution of the diffractometer can be calculated precisely and the instrumental artefacts can be analysed easily without a sample present. The performance is demonstrated with LaB6 and paracetamol, and a critical appraisal of the uncertainties in the measurements is presented. The instantaneous data collection offers possibilities in dynamic experiments.