Thin foils of fully dense, but only partially transformed, hot-pressed
silicon nitride materials have been examined by high-resolution trans
mission electron microscopy. Large untransformed grains are seen to co
ntain high densities of nanometer dimension, round or oval, textural f
eatures. Examination at high magnification shows these to be clusters
of dislocation loops, which are concentrated towards grain centers. Th
e loops occur most commonly in grains of materials with a high proport
ion (almost-equal-to 70%) of unconverted alpha-Si3N4, as shown by quan
titative X-ray diffraction analysis. They are seen less often in mater
ial more fully converted to the bets-Si3N4 phase (almost-equal-to 5% a
lpha-Si3N4). The loops are believed to form by condensation from super
saturated concentrations of vacancies during rapid cooling from densif
ication temperature. The loops are confined exclusively to the grain i
nteriors, and in consequence an estimate of the nitrogen vacancy diffu
sion coefficient can be made.