Three series of SiC/AlN samples were prepared by pyrolysis of “poly(aluminosilazane)”, the product of the reaction between hexamethylcyclotrisilazane and triethylaluminum. The Si/Al ratio was varied for one series (with constant pyrolysis temperature) and the pyrolysis temperature was varied for the other two series, with Si/Al = 1 and 3. 27Al and 29Si magic angle spinning NMR were used to analyze these samples in terms of coordination number, nearest neighbor atoms, and crystallinity. NMR results indicate that higher crystallinity and phase separation into discrete SiC and AlN crystallites accompany an increase in pyrolysis temperature. Disorder and increased heterogeneity in connectivity are observed with increasing Si/Al ratio of the initial reactants.

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