Processing of Silicon Nitride Ceramics Produced by Spark Plasma Sintering

Four silicon nitride powder blends vary in starting powder characteristics, glass chemistry, and phase composition. This work focuses on how these properties influence densification behavior, microstructural development, and the resulting mechanical performance of dense ceramics. Previous work completed on alpha-rich, low oxide containing (8 wt%), and fine silicon nitride powder (GS-44) showed high hardness equiaxed with grained ceramic. GS-44 served as an excellent precursor for the matrix phase material in graphene reinforced composites, which resulted in 235% increase in toughness and high hardness retention [1] with the addition of 1.5 vol% graphene. As the GS-44 powder is no longer in production, investigative work into other commercial powders and customization of powder blends was initiated. Commercial blends were selected based on availability, high alpha content, fine particle size, and additive chemistry (Al2O3, MgO, and Y2O3). The objective was to understand which powder characteristics led to a ceramic design that contained high hardness, strength, and toughness properties in order to increase the use of silicon nitride in extreme temperature environments. One such example is aerospace and structural applications that require a high-performance material that is lightweight and good thermal stability. Strong covalent bonding in silicon nitride make densification of powders extremely difficult; thereby, sintering additives are necessary to promote liquid phase sintering processes. Compaction of ceramic powders was carried out using a spark plasma sintering (SPS) furnace by utilizing a pulsed direct current through a conductive graphite die that encapsulates the sample powder. SPS was preferred over other conventional sintering methods owing to its high heating rate and short dwell times at the sintering target temperature. Thus, SPS provides superior control for tailoring the final silicon nitride properties by producing a hard alpha-phase and tough beta-phase microstructures. The custom blend developed had an appreciable amount of media wear included during the milling process that increased the additive content. Development of the custom blend was used to understand the effect of a larger additive content. Commercial GS-44 blend was used as the control to track the effect of adjusting specific surface area and oxide content in silicon nitride powder systems (HCS-M, C-R3, and UA-SN). The mechanical results for the four matrix systems, showed that toughness increased with grain coarsening and minimization of alumina content in beta silicon nitride. Based on these findings it is important to determine tradeoffs (i.e. balance of high hardness, toughness, and strength) to engineer an optimal ceramic that can be used for structural and aerospace applications.Dissertation not available (per author's request