Atomic resolution transmission electron microscopy of the intergranular structure of aY2O3-containing silicon nitride ceramic

High-resolution transmission electron microscopy (HRTEM) employing focus-variation phase-reconstruction methods is used to image the atomic structure of grain boundaries in a silicon nitride ceramic at subangstrom resolution. Complementary energy-dispersive X-ray emission spectroscopy experiments revealed the presence of yttrium ions segregated to the 0.5-0.7-nm thin amorphous boundary layers that separate individual grains. Our objective here is probing if yttrium ions attach to the prismatic planes of the Si3N4 at the interface toward the amorphous layer, using Scherzer and phase-reconstruction imaging, as well as image simulation. Crystal structure images of grain boundaries in thin sample (<100 Angstrom) areas do not reveal the attachment of yttrium at these positions, although lattice images from thicker areas do suggest the presence of yttrium at these sites. It is concluded that most of the yttrium atoms are located in the amorphous phase and only a few atoms may attach to the terminating prism plane. In this case, the line concentrations of such yttrium in the latter location are estimated to be at most one yttrium atom every 17 Angstrom.