The effect of slurry flocculation on the characteristics of silicon nitride granules prepared by the spray drying process is investigated. The flocculation state of an aqueous silicon nitride slurry is controlled by adding nitric acid and evaluated as a function of pH. Dense and hard silicon nitride granules result from a well‐dispersed slurry having a high pH (e.g., 10.8). These hard granules retain their shape in green compacts and form detrimental defects. Lowering the pH of the slurry to a certain value (e.g., pH 7.9) results in slurry flocculation. Granules prepared from this flocculated slurry have low density and low diametral compression strength and contribute to the elimination of large pores in green compacts.
The effect of spray‐dried granule strength on the micro‐structure of green compacts obtained by isostatic pressing was quantitatively analyzed. The fracture strength of single granules of Si3N4 powder made with ultrafine A12O3 and Y2O3 powders was measured directly by diametral compression. It was found that fracture strength increased notably with the increasing relative density of the granule and the decreasing size of agglomerates in suspension before spray‐drying. Even when green bodies were prepared at an isostatic pressure of 200 MPa, intergranular pores, which negatively affected densification of the sintered bodies, occurred between unfractured granules. The volume and size of these pores in the green compacts increased with the increasing fracture strength of the granules. In the case of closely packed granules, an isostatic pressure of 800 MPa was required to completely collapse the intergranular pores. A simple equation was derived to calculate the isostatic pressure necessary for complete collapse of intergranular pores in the green compacts, and it was determined that granule strength must be kept as low as possible to obtain uniform green compacts.
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