High temperature mechanical properties of structural ceramics Si3N4 are controlled by ∼1 nm thick silicate amorphous films covering all grain boundaries. The composition of the film dictates the equilibrium film thickness resulted from a force balance at grain boundary. Many efforts arc brought to alter film chemistry and thickness, and this system offers ideal model materials to understand grain boundary and property relationship. Using a dedicated STEM (VG HB601) with high spatial resolution EELS analysis and high resolution Z-contrast imaging, various novel quantification data of the grain boundary in Si3N4 can be obtained. The methods described here can also be applied to other types of grain boundaries.

EELS profiling was performed to acquire a full spectrum from each position at a lateral increment of 1Å across a boundary in a pure Si3N4 sample with only SiO2 impurities from surface oxidation. It gives directly elemental distributions near the boundary such as Si, N and O profiles shown in Fig. 1.