Micro X-ray diffraction (µXRD): a versatile technique for characterization of Earth and planetary materials

Abstract

Recent developments in laboratory-based micro X-ray diffraction (µXRD) have extended X-ray examination of geomaterials to the microscopic level (50–500 µm), greatly expanding the applicability of XRD to mineralogy, petrology, materials, environmental, and planetary sciences. Laboratory-based µXRD has been accomplished using a Bruker™ D8 Discover diffractometer, having a sealed-tube Cu source, theta–theta geometry, Gobel mirror parallel optics with 50–500 µm collimation, and general area detector diffraction system (GADDS). A wide range of samples, including polished thin sections, electron probe microanalysis (EPMA) mounts, rock slabs, whole rocks, and powders have been examined with µXRD using a remote-controlled XYZ sample stage, with imaging by optical microscope monitor and charge-coupled device (CCD) camera. Individual grains in heterogeneous samples have been examined in situ, with little or no sample preparation. The two-dimensional GADDS preserves textural and crystallinity information (e.g., bioapatite) and easily discriminates between multiple phases of utility for synthetic or natural samples (e.g., mine tailings). In situ µXRD of minerals preserves spatial relationships, enabling study of orientational phenomena, such as strain-related mosaicity (giving “streaked” diffraction lines). Examples include strained quartz (La Malbaie quartzite, Quebec) and shocked clinopyroxenes (Shergottite NWA 3171). Mineral mapping has been demonstrated by reproducing exsolution textures of kamacite from taenite (Widmanstätten pattern) in the Toluca iron meteorite. Diffraction data obtained from single crystals (by the omega scan method) have enabled grain-by-grain correlation between unit cell (µXRD) and chemical composition (EPMA), as demonstrated by kimberlite indicator garnets. The examples shown herein demonstrate the breadth of information that can be obtained by µXRD of Earth and planetary materials.