Extended X-ray absorption fine structure (EXAFS) study of secondary phases in Yb2O3-doped Si3N4 ceramics

Liquid-phase sintered Si3N4 doped with Yb2O3 as a sintering aid was characterized by both transmission electron microscopy and extended X-ray absorption fine structure (EXAFS) measurements. Structural information about the secondary phases was obtained with an emphasis being placed on the evaluation of EXAFS data. Two Si3N4 samples were processed which contained either 5 vol% or 10 vol% Yb2O3 as sintering additive. After sintering, only an amorphous secondary phase was observed in the material doped with 5 vol% Yb2O3. The material with the higher Yb2O3 volume fraction underwent a further heat treatment after the densification, in order to crystallize pockets of the secondary phase. This heat treatment resulted in the formation of Yb2Si2O7 at multi-grain junctions, with however, amorphous phases remaining along the grain and phase boundaries. The EXAFS data obtained from the two doped Si3N4 materials were compared with reference spectra obtained on pure Yb2O3 and synthetic Yb2Si2O7. No residual Yb2O3 was determined in the doped Si3N4 materials, independent of the Yb2O3 volume fraction. Compared to synthetic Yb2Si2O7, the secondary phase formed in the 10 vol% Yb2O3 containing material showed only subtle changes in the EXAFS data. A clear distinction between purely amorphous and a combination of crystalline plus amorphous Yb secondary phases was possible, when both doped Si3N4 materials were compared. However, no distinction between the glass phase present at triple junctions and the amorphous residue along grain/phase boundaries was feasible, since a full numerical data evaluation could not be performed.