C. Omeara et J. Sjoberg, TRANSMISSION ELECTRON-MICROSCOPY INVESTIGATION OF THE OXIDATION OF HOT ISOSTATICALLY PRESSED SILICON-NITRIDE WITH AND WITHOUT SINTERING AIDS, Journal of the American Ceramic Society, 80(6), 1997, pp. 1491-1500
Analytical transmission electron microscopy of thin-foil cross section
s has been used to examine the oxidation behavior of hot isostatically
pressed silicon nitride (Si3N4) materials. The transmission electron
microscopy (TEM) cross sections are prepared by a special technique th
at provides electron transparency through the entire oxide, interfacia
l, subscalar, and matrix regions simultaneously. The materials are oxi
dized in an alumina furnace at 1250 degrees C for 100 h. TEM investiga
tion indicates that oxidation of Si3N4 occurs in an oxidation reaction
zone that is comprised of the scale, oxide/matrix interface, and subs
calar regions; therefore, the silica (SiO2)/Si3N4 interfacial surface
area that is available for oxidation is very large. The oxidative atta
ck on the Si3N4 grains is not uniform or sequential, and oxygen diffus
es into the matrix before the surface grains are consumed. Gas bubbles
, probably nitrogen gas, accumulate at all levels of the scale, and no
evidence is found for the existence of an ''oxynitride'' layer. Disin
tegration of the secondary phase, Y2Si2O7, in the subscalar region is
observed to occur, indicating that secondary, oxidation-related phenom
ena are occurring.