Depletion of Grain-Boundary Phase and Elastic Creep Deformation Upon Ultra-Long Flexural Stress Rupture Experiments of NC-132 Silicon Nitride

A unique grain-boundary structure evolution was observed in two MgO-doped silicon nitride specimens (Norton, NC-132) that were tested in ultra-long flexure stress rupture experiments with an applied stress of 266 MPa and fractured at 14 941 and 17 376 h. Transmission electron microscopy showed that, although the starting material had a secondary glass phase both at multi-grain junctions and along grain boundaries, the tested specimens contained no residual glass phase. Concurrent with the elimination of the secondary glass phase, a continuous network of cracked grain boundaries was observed after long-term flexure testing consistent with the concept of elastic creep. It is, therefore, concluded that at ultra-long annealing times, this material is affected by creep deformation via microcrack nucleation and growth due to the depletion of the amorphous siliceous grain-boundary phase, which is seen as a truly transient, fugitive secondary phase.