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

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 Role of the Activator Additives Introduction Method in the Cold Sintering Process of ZnO Ceramics: CSP/SPS Approach.

The great prospects for introducing the cold sintering process (CSP) into industry determine the importance of finding approaches to reduce the processing time and mechanical pressure required to obtain dense ceramics using CSP. The introducing zinc acetate into the initial ZnO powder of methods, such as impregnation, thermovapor autoclave treatment (TVT), and direct injection of an aqueous solution into a die followed by cold sintering process using a spark plasma sintering unit, was studied. The effect of the introduction methods on the density and grain size of sintered ceramics was analyzed using SEM, dynamic light scattering, IR spectroscopy, and XRD. The impregnation method provides sintered samples with high relative density (over 0.90) and significant grain growth when sintered at 250 °C with a high heating rate of 100 °C/min, under a uniaxial pressure of 80 MPa in a vacuum, and a short isothermic dwell time (5 min). The TVT and aqueous solution direct injection methods showed lower relative densities (0.87 and 0.76, respectively) of CSP ZnO samples. Finally, the development of ideas about the processes occurring in an aqueous medium with CSP and TVT, which are subject to mechanical pressure, is presented.