Novel Compaction Processing of Ceramics with Spray-freeze Dried Granules

"AbstractionSpray freeze drying method was proposed to fabricate ·ceramic: powder granules for high performance ceramics. Obtained granules and their green compact were characterized by SEM and immersion liquid technique. Granules have a spherical shape of about l 00 µ m in diameter, ·and no binder segregation was found with the immersion liquid technique. The granule had sufficient strength for usual handling, while the strength was much lower than that of granules prepared by conventional spray-drying. Unlike the conventional green compacts, granule interfaces were not observed in the green body made with the spray-freeze dried granules.IntroductionIt was well kn9wn that spray-dried granules have binder segregation layer on their surfaces. The trace of this segregation layer survives in the later processes i.e. compaction and firing, and behaves as fracture origins in the sintered bodies. The origin of this problem is solvent drying process from slurry droplet surface in spray drying system. As alternative method we propose a freeze drying process for granule preparation, in which solvent is remove by sublimation though the process, binder segregation can be prevent.In this study, we applied spray freeze drying method to fabricate alumina powder granule, and characterized the obtained granules, and their green compacts and sintered bodies.Experimental procedure.Alumina powders and additives aqueous solution were mixed for 24 hours using a ball mill to· prepare the slurry for spray freeze drying. .The solid loading of the slurry was 30vo1%. Deflocculant (PAA-NH4 type) was added 0.5mass%, and the binder (PVA). 1.0, 2.0 or 3.0mass% of alumina. Obtained slurries were sprayed into liquid nitrogen to make frozen granules. The granules were freeze dried.For the characterization of the granules, immersion, liquid technique observation and single granule strength test were carried out. Strength of individual granule wa5 measured using micro compression testing machine (MCTM, SHIMADZU). Granule strength was calculated from following equation."