Evaluation of the Role of the Activating Application Method in the Cold Sintering Process of ZnO Ceramics Using Ammonium Chloride

Materials (Basel). 2023 Jan 1;16(1):408. doi: 10.3390/ma16010408.

Abstract

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.

Keywords: cold sintering; microstructure; oxide ceramics; thermo-vapor treatment; zinc oxide.

Grants and funding

The work of Andrey V. Smirnov, Maxim V. Kornyushin, Anastasia A. Kholodkova, and Yurii D. Ivakin was supported by RTU MIREA (initiative research “Ceramics Synthesis”). The work of Anton Smirnov was supported by the Ministry of Science and Higher Education of the Russian Federation under project 0707-2020-0034.