The present report explores the use of liquid-state nuclear magnetic r
esonance (NMR) spectroscopy for characterizing the methylhydridopolysi
lazane (MHPS) prepared by the Seyferth/Wiseman procedure and compares
the structure of this polymer with other ceramic precursors derived fr
om similar synthetic routes. X-ray diffraction, cross-polarization (CP
), and single-pulse magic angle spinning (MAS) solid-state NMR spectro
scopy were employed for characterizing temperature-induced short-range
bonding and phase evolution in MHPS precursors to SiC/Si3N4 ceramics.
The molecular weight and methyl substitution of the preceramic polyme
rs is shown to affect the ceramic yield and phase development of these
polysilazanes during pyrolysis. Ceramic yields approaching 90% are ob
served in these systems. CPMAS NMR is shown to be uniquely capable of
identifying the hydrogen-rich environments and the onset of short-rang
e SiC and Si3N4 phase development in these amorphous preceramic materi
als.