Analysis of scanning electron microscopy images was used to study the changes in the crystal size distribution of ZnO, which occurred during its processing in an aqueous medium at 220–255 °C and an equilibrium vapor pressure in an autoclave. The results were compared with those of ZnO placed in a die for treatment under similar conditions supplemented with mechanical pressure application in the cold sintering process. In both cases, ZnO was treated in the presence of an activating additive: either zinc acetate or ammonium chloride. During autoclaving, a powder consisting of fine ZnO monocrystals was obtained, while the cold sintering process led to ceramics formation. Under vapor pressure and mechanical pressure, the aqueous medium affected ZnO transformation by the same mechanism of solid-phase mobility activation due to the additives’ influence. The higher the content of additives in the medium, and the higher the mechanical pressure, the more pronounced activating effect was observed. Mass transfer during the cold sintering process occurred mainly by the coalescence of crystals, while without mechanical pressure, the predominance of surface spreading was revealed. In the initial ZnO powder, the average crystal size was 0.193 μm. It grew up to 0.316–0.386 μm in a fine-crystalline powder formed in the autoclave and to an average grain size of 0.244–0.799 μm in the ceramics, which relative density reached 0.82–0.96. A scheme explaining the influence of an aqueous medium on the solid-phase mobility of ZnO structure was proposed. It was found that the addition of 7.6 mol% ammonium chloride to the reaction medium causes the processes of compaction and grain growth similar to those observed in ZnO Cold Sintering Process with the addition of 0.925 mol% zinc acetate.
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.
Porous α-Al2O3 ceramics are a highly sought-after material with a multitude of applications; for example, they are used as filters, substrates, biomedicine materials, etc. Despite the availability of raw materials, a challenge associated with this technology is the high energy budget caused by sintering above 1500 °C. For the cold sintering processing (CSP) of ceramics, lowering the α-Al2O3 sintering temperature is one of the most urgent challenges in the background of its rapid development. This paper is the first to demonstrate a solution to this problem using the CSP of α-alumina ceramics in the presence of pure water as a transient liquid. The manufactured materials were examined using XRD analysis; the evolution of their microstructures during CSP was revealed by SEM; and the porosity was evaluated using the Archimedes method. Ceramics with an open porosity up to 36% were produced at 380–450 °C and 220 MPa in 30 min. An increase in the pressure was found to impede α-Al2O3 formation from γ-AlOOH. The development of the microstructure was discussed within the framework of the dissolution–precipitation model and homogenous nucleation. The results of the SEM study pointed to the coalescence of γ-AlOOH grains during CSP.
1 May 2015 in Russian Journal of General Chemistry
Objectives and achievements of the production of disperse composite materials (DCMs) which consist of particles with a metal coating are represented. The prospects of the DCM production by the dusty...
Objectives. To examine the general principles and recent advances in the synthesis of high-purity and high-homogeneity barium titanate powders in the manufacture of electronic components.Results. The main publications regarding the synthesis of barium titanate powder, including the works of recent years, were analyzed. The technological advantages and disadvantages of various synthesis methods were identified. Groups of methods based on solid-state interaction of reagents and methods of “wet chemistry” were also considered. The possibilities of producing barium titanate particles of non-isometric shapes for creating textured ceramics were discussed separately.Conclusions. Barium titanate is a well-known ferroelectric with a high dielectric constant and low dielectric loss. It is used as a component in ceramic electronic products, for example, capacitors, memory devices, optoelectronic devices, and piezoelectric transducers. The possibilities of producing functional ceramics based on barium titanate powder largely depend on its state and morphological characteristics, determined during the synthesis stage. The most important factors affecting the functional characteristics of ceramics are the purity and morphology of the powder raw materials used.