Microstructure of Gilsocarbon graphite revealed by a correlative study of optical texture and FIB-TEM

Abstract

Transmission Electron Microscopy (TEM) alongside Polarized Optical Microscopy (POM), is used to investigate the microstructure of nuclear graphite, specifically Gilsocarbon coke, fillers, binders, and flour. Detailed analyses revealed domain structures, domain boundaries, sub-domains and two types of microcracks: intra-domain and inter-domain cracks. Analysis of TEM images, from samples prepared via Focused Ion Beam (FIB), showed domain sizes in coke filler and flour regions ranged from 1 to 3 μm, whereas binder regions had larger domains of up to tens of micrometers, with correspondingly longer Mrozowski cracks. Within these domains, sub-domain boundaries further constrained Mrozowski cracks, resulting in crack lengths significantly shorter than the domain size. Domain boundaries were classified into small-angle and large-angle boundaries based on orientation differences, with large-angle boundaries arising from multiple small-angle transformations facilitated by polygonal microcracks. This microstructural data obtained from virgin Gilsocarbon graphite provides essential inputs for an experimentally informed model predicting the deformation and fracture properties of this material at the micrometer length scale, which may offer improved insights to enhance our understanding of how these properties may evolve under reactor operating conditions.