A developing energy-saving approach of cold sintering in a pure aqueous medium was applied to the preparation of α-Al2O3 ceramics and performed on spark plasma sintering equipment. The initial γ-Al(OH)3 and γ-AlOOH powders and the cold-sintered ceramics were studied by X-ray diffraction analysis, infrared spectroscopy, thermal analysis, and scanning electron microscopy to reveal the chemical and structural transformations they experienced during the cold sintering. At 450 °C and 70 MPa, initially γ-AlOOH transformed into a fragile α-Al2O3 material. Porous α-Al2O3 ceramics with about 60% porosity were obtained after cold sintering of γ-Al(OH)3 in the same conditions combined with subsequent annealing at 1250 °C for 3 h. The role of water molecules in the studied processes was considered as the enhancement of structural mobility in the cold-sintered material due to its reversible hydroxylation similar to earlier investigated supercritical water actions on the precursors during α-Al2O3 formation. Further improvement of the cold sintering setup and regimens would open prospects in α-Al2O3 ceramics manufacturing by an ecologically benign route.
Although the activating effect of an acetate medium in the cold sintering process of zinc oxide ceramics is well known, some problems need to be solved on the effect of process conditions and the initial powder’s preparation methods on the ceramic’s density and microstructure. This article describes an effect of the zinc acetate introduction method, its concentration in zinc oxide powder as well as that of the die sealing configuration on the density and microstructure of zinc oxide ceramics obtained by the cold sintering process at 244 °C. The activating additive of zinc acetate was applied in two ways: (1) impregnation in aqueous solution and (2) impregnation with subsequent treatment in water vapor. Zinc oxide powders and ceramics were analyzed using SEM, TGA/DSC/MS and XRD to reveal the effect of powder pre-treatment and sintering conditions on the material microstructure. Cold sintered ZnO ceramics samples with a relative density up to 0.99 and with average grain sizes from 0.28 to 1.71 μm were obtained. The die sealing by two Teflon sealing rings appeared to be the most effective.
The influence of the method of applying the activating additive ammonium chloride and its concentration on the density and microstructure of zinc oxide ceramic obtained by cold sintering at 244 °C was investigated. The activating agent was applied by two methods: impregnation and subsequent autoclave treatment. When the powder was activated by the impregnation method, the crystal sizes remained at the initial level of 0.17–0.19 μm. After the autoclave treatment, the crystal sizes increased to 0.31–0.53 μm. Samples of cold sintering ZnO with relative density up to 0.96 and average grain sizes 0.29–0.86 μm were obtained. ZnO powders and ceramic samples were analyzed using SEM, TGA/DSC, and XRD to reveal the effect of the powder activation method and cold sintering conditions on the material microstructure. The effect of ammonium chloride concentration on grain growth and microstructure of ceramic samples is shown. It was found that the average grain size of ceramic samples with an increase in additive concentration passes through a minimum. In cold sintering of the autoclave activated powder, the effect of reducing the average grain size was observed. The results of this work are discussed on the basis of the idea of the solid-phase mobility of the crystal structure arising when interacting with an aqueous medium.
The influence of the following factors on the surface roughness of steel workpieces after burnishing is studied experimentally: the method of attaching the polyhedral insert, the...