Analysis of graphite orientation and crystallinity

A field emission electron probe microanalyzer (EPMA) equipped with hyperspectral soft X-ray emission (SXES) and cathodoluminescence (CL) spectrometry has been used to investigate a carbonaceous-rich geological deposit to understand the crystallinity and morphology of the carbon and the associated quartz.

The sample was sourced from the Epanko deposit Tanzania, located within the Mahenge Inlier in the Eastern Granulite terrane of the East African Orogen, where the host rocks consist of anorthosite basement and a sequence of sediments including shales, with a variable organic carbon content, and limestones that have been metamorphosed to high temperature and pressure as graphitic schists and marbles. The phases present in the sample were determined by clustering the X-ray hyperspectral map which was collected in parallel to the SEXS and CL datasets.

Mineral map showing quartz containing graphite

C Kα spectra from distinctively different carbon-rich grains, measured using the SXE spectrometer are shown to the right. The graphite spectra are equivalent to those observed on HOPG graphite and attributed to 2p(x+y) and 2pz orbitals. The C Kα second order peak at 281 eV is attributed to π bond, whereas the peak at 271 eV is attributed to σ bond. The presence of π and σ bonding indicates the highly crystalline graphitic nature of the carbon, as these would not be present if it was amorphous.

Second-order C Kα peak measured using the SXE spectrometer on the graphite grains showing the main two spectral forms of graphite within the mapped region. The C Kα spectrum (blue) is mainly the 2p(x+y), while the C Kα spectrum (red) is mainly the 2pz.

The differences in the spectral shapes are a reflection of the orientation of the individual grains, as the SXE spectrometer is sensitive to crystal orientation. The SXE spectrometer offers a spectral tool to measure both chemistry and bonding, and when combined with spectral CL, the complementary techniques enable new knowledge to be gained from mineral deposits. The relative ease of sample preparation compared to EBSD makes it an easier technique for the measurement of graphite grain orientations


Reference

MacRae, C. M., Pearce, M. A., Wilson, N. C., Torpy, A., Glenn, M. A., & Russo, S. P. (2020). Soft X-Ray and Cathodoluminescence Examination of a Tanzanian Graphite Deposit. Microscopy and Microanalysis, 26(4), 814-820. https://doi.org/10.1017/S1431927620001294