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Silicon carbide polytype characterisation in coated fuel particles by Raman spectroscopy and 29Si magic angle spinning NMR

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The silicon carbide layer of a batch of intact TRISO (tristructural isotropic) coated fuel particles with zirconia kernels was characterised by Raman spectroscopy and magic angle spinning nuclear magnetic resonance (MAS-NMR). The techniques were evaluated as a probe for the evolution of SiC local structure as a function of chemical vapour deposition processing. NMR resolved 29Si resonances consistent with multiple α-polytypes: a mixture of 6H, 15R and 4H within a majority (36%) 3C-SiC target structure. Polarised Raman spectroscopy by contrast, showed some evidence of hexagonal and cubic local environments but no evidence for clearly defined hexagonal or orthorhombic polytypes. It was clear from the Raman that there was significant scattering from q >0 regions of the Brillouin zone, consistent with a loss of translational symmetry associated with stacking faults. Simulation and TEM images suggested that the signals observed in Raman and NMR correspond closer to a random arrangement of SiC layers in which structures similar to the various polytypes occur over short distances. As NMR is a probe of local environment, the signals obtained were similar to those that would come from a mixture of crystallites, each of a well-defined polytype. The NMR data was analysed quantitatively by fitting the spectra of known polytypes and by using a simple model to represent the random arrangement of layers in a heavily faulted crystal.
2012-11-28
ELSEVIER SCIENCE BV
JRC68914
0022-3115,   
https://publications.jrc.ec.europa.eu/repository/handle/JRC68914,   
10.1016/j.jnucmat.2012.08.047,   
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