Silicon carbide fibers of different generation/processing routes (NLM-Nicalon and Tyranno SA3) were thermally treated to trigger the growth of nanocrystals, which were analyzed using Raman spectroscopy and transmission electron microscopy (TEM). The nanocrystals were also aged in molten sodium nitrate to investigate their reactivity. The spatial correlation model has been used to model the Raman spectra and extract accurate and statistical information on the nanocrystallites' structure and dimension. For the NLM fibers, an average size of 2.5 to 7.0 nm was calculated, which was in good agreement with TEM observations. For the Tyranno SA3 fiber, despite the heavily faulted stacking sequence, the Raman peaks remained sharp, indicating that the crystallite dimension calculated from the Raman spectra is only dependent on the actual size of the nanocrystals and is not affected by the sequence of the stacking faults.

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