Densification mechanism and microstructure characteristics of nano- and micro- crystalline alumina by high-pressure and low temperature sintering

Fully dense ceramics with retarded grain growth can be attained effectively at relatively low temperatures using a high-pressure sintering method. However, there is a paucity of in-depth research on the densification mechanism, grain growth process, grain boundary characterization, and residual stress. Using a strong, reliable die made from a carbon-fiber-reinforced carbon (C_f/C) composite for spark plasma sintering, two kinds of commercially pure α-Al₂O₃ powders, with average particle sizes of 220 nm and 3 μm, were sintered at relatively low temperatures and under high pressures of up to 200 MPa. The sintering densification temperature and the starting threshold temperature of grain growth (T_sg) were determined by the applied pressure and the surface energy relative to grain size, as they were both observed to increase with grain size and to decrease with applied pressure. Densification with limited grain coarsening occurred under an applied pressure of 200 MPa at 1050 °C for the 220 nm Al₂O₃ powder and 1400 °C for the 3 μm Al₂O₃ powder. The grain boundary energy, residual stress, and dislocation density of the ceramics sintered under high pressure and low temperature were higher than those of the samples sintered without additional pressure. Plastic deformation occurring at the contact area of the adjacent particles was proved to be the dominant mechanism for sintering under high pressure, and a mathematical model based on the plasticity mechanics and close packing of equal spheres was established. Based on the mathematical model, the predicted relative density of an Al₂O₃ compact can reach ～80 % via the plastic deformation mechanism, which fits well with experimental observations. The densification kinetics were investigated from the sintering parameters, i.e., the holding temperature, dwell time, and applied pressure. Diffusion, grain boundary sliding, and dislocation motion were assistant mechanisms in the final stage of sintering, as indicated by the stress exponent and the microstructural evolution. During the sintering of the 220 nm alumina at 1125 °C and 100 MPa, the deformation tends to increase defects and vacancies generation, both of which accelerate lattice diffusion and thus enhance grain growth.     

Achieving fabrication of highly transparent Y2O3 ceramics via air pre-sintering by deionization treatment of suspension

An easy albeit quite effective deionization suspension treatment was adopted to alleviate the detrimental effects related to the hydrolysis of Y₂O₃ in an aqueous medium. Fabrication of highly transparent Y₂O₃ ceramics with a fine grain size via air pre-sintering and post–hot isostatic pressing (HIP) treatment without using any sintering additive was achieved using the treated suspensions. The hydrolysis issue of Y₂O₃ powder in an aqueous medium was effectively alleviated by using deionization treatment, and a well-dispersed suspension with a low concentration of dissolved Y³⁺ species was obtained. The dispersed suspensions were consolidated by the centrifugal casting method, and the green bodies derived from the suspension of 35.0 vol% solid loading showed an improved homogeneity with a relative density of 52.1%. Fully dense Y₂O₃ transparent ceramic with high transparency was obtained by pre-sintering consolidated green compacts at a low temperature of 1400°C for 16 h in air followed by a post-HIP treatment at 1550°C for 2 h under 200 MPa pressure. The sample had a fine average grain size of 690 nm. The in-line transmittance of the sample reached 83.3% and 81.8% at 1100 nm and 800 nm, respectively, very close to the theoretical values of Y₂O₃.     

Highly oriented α-Al2O3 transparent ceramics shaped by shear force

Alumina platelets were arranged horizontally in submicron alumina particles by shear force in the flow of slurries during casting. The obtained alumina green bodies with platelets were pressureless-sintered in vacuum, producing ceramics with thoroughly oriented grains and high transmittance. The effects of sintering parameters on the densification, microstructure evolution, and orientation degree of alumina ceramics were investigated and discussed. The results showed that the densification, grain size, orientation degree, and in-line transmittance were increased with increasing sintering temperature. The enhancement of orientation degree was mainly coherent with grain growth. The grain-oriented samples exhibited a much higher in-line transmittance (at 600 nm) of 61 % than that of the grain random sample (29 %). Moreover, the transmission remained a high level in the ultraviolet range (<300 nm).     

Susceptor-assisted fast microwave sintering of TiN reinforced SiAlON composites in a single mode cavity

In the present study, 17 wt % TiN reinforced α-β SiAlON composites were sintered at low temperature by susceptor-assisted microwave heating. The effect of TiN addition on dielectrical properties of starting powders, as well as the influence of sintering temperature on phase evolution, microstructure development and mechanical properties of α/β-SiAlON-TiN composites were investigated. The obtained results showed that TiN addition increased the microwave absorbing properties which is reflected in the peak sintering temperature. Thus, the α:β ratio decreased and mechanical properties were improved, especially the fracture toughness of the composites. Furthermore, an estimate of energy consumption during microwave assisted sintering at the laboratory scale is presented. As a result, the highest values for relative density (97.1%), Vickers hardness (13.35 ± 0.47 GPa), and fracture toughness (7.52 ± 0.54 MPa m^1/2) were obtained by microwave sintering for 30 min at 1300 °C.     

Effect of microwave sintering on the microstructure and mechanical properties of AA7075/B4C/ZrC hybrid nano composite fabricated by powder metallurgy techniques

AA7075 + 6%B4C+3%ZrC nano hybrid composite was successfully fabricated, with nano reinforcements composition in AA7075 alloy selected based on previous investigation, to achieve better mechanical performance. Two different sintering techniques, namely conventional and microwave, were implemented to determine the effect on microstructural and mechanical properties. Microstructural investigation was performed with the help of W-SEM. Tensile, compression, and hardness were measured with the help of UTM and Vickers microhardness machine. Porosity was calculated by using Archimedes principle. It was observed that the added nano ZrC particles formed agglomerates and the B₄C particles were distributed homogenously. Composites processed by microwave sintering showed excellent mechanical properties compared to the conventionally sintered composites. No intermetallic compounds were detected in microwave sintered composites through XRD analysis, indicating strong and clean interface bonds between matrix and reinforcement particles. High strain to fracture value of 12.24% was noted in microwave sintered nano hybrid composite, while it was 6.12% for conventional sintered one. Fractography revealed no peeling action of reinforcements from the matrix material, and the mode of failure was brittle. It was concluded that, while fabricating nano range hybrid composites, the implementation of advanced sintering technique (microwave sintering) with low sintering temperatures and low sintering times with internal heat generations, helps in eliminating defects that may develop because of high surface energies of nano range reinforcements.     

A thermal perspective of flash sintering: The effect of AC current ramp rate on microstructure evolution

In flash sintering experiments, the thermal history of the sample is key to understanding the mechanisms underlying densification rate and final properties. By combining robust temperature measurements with current-ramp-rate control, this study examined the effects of the thermal profile on the flash sintering of yttria-stabilized zirconia, with experiments ranging from a few seconds to several hours. The final density was maximized at slower heating rates, although processes slower than a certain threshold led to grain growth. The amount of grain growth observed was comparable to a similar conventional thermal process. The bulk electrical conductivity correlated with the maximum temperature and cooling rate. The only property that exhibited behavior that could not be attributed to solely the thermal profile was the grain boundary conductivity, which was consistently higher than conventional in flash sintered samples. These results suggest that, during flash sintering, athermal electric field effects are relegated to the grain boundary.     

Additive Manufacturing of Stable Energy Storage Devices Using a Multinozzle Printing System

The development of the Internet of things has prompted an exponential increase in the demand for flexible, wearable devices, thereby posing new challenges to their integration and conformalization. Additive manufacturing facilitates the fabrication of complex parts via a single integrated process. Herein, the development of a multinozzle, multimaterial printing device is reported. This device accommodates the various characteristics of printing materials, ensures high-capacity printing, and can accommodate a wide range of material viscosities from 0 to 1000 Cp. Complete capacitors, inclusive of the current collector, electrode, and electrolyte, can be printed without repeated clamping to complete the preheating, printing, and sintering processes. This method addresses the poor stability issue associated with printed electrode materials. Furthermore, after the intercalation of LiFePO₄ with Na ions, X-ray photoelectron spectroscopy and X-ray diffraction results reveal that the Na ions permeate the interlayer structure of LiFePO₄, enhancing the ion migration channels by increasing the ion transmission rate. A current rate of 2.5 mAh ensures >2000 charge/discharge cycles, while retaining a charge/discharge efficiency of 96% and a discharge capacity of 91.3 mAh g⁻¹. This manufacturing process can provide conformal power modules for a diverse range of portable devices with various shapes, improving space utilization.     

Microstructural,mechanical, and thermal properties of microwave-sintered KLS-1 lunar regolith simulant

KLS-1 Lunar regolith simulant was microwave sintered to explore its potential applicability in future lunar construction. The effects of sintering temperature on linear shrinkage, density, porosity, and microstructural, mechanical, and thermal properties were investigated. As the sintering temperature increased, linear shrinkage and density increased and porosity decreased. Structural evolution in the sintered samples was characterized by scanning electron microscopy and X-ray diffraction. Unconfined compressive strength testing showed that mechanical strength increased significantly with increasing sintering temperature, with 1120 °C giving the highest strength of 37.0 ± 4.8 MPa. The sintered samples exhibited a coefficient of thermal expansion of approximately 5 × 10⁻⁶ °C⁻¹, which was well-maintained even after cyclic temperature stress between −100 and 200 °C. Therefore, this microwave processing appears promising for the fabrication of building material with sufficient mechanical strength and thermal durability for lunar construction.     

Fabrication and upconversion luminescence properties of Er:SrF2 transparent ceramics compared with Er:CaF2

SrF₂ transparent ceramic is a promising upconversion material due to the low phonon energy. The effect of different sintering temperatures on Er:SrF₂ transparent ceramics was investigated. The suitable sintering temperature for Er:SrF₂ transparent ceramics was 900 °C by hot-pressed sintering in this study. High quality of Er:SrF₂ transparent ceramics with different doping concentrations were obtained. The upconversion luminescence spectra and decay behavior were compared between Er:SrF₂ and Er:CaF₂ transparent ceramics with different Er³⁺ doping concentration. The green emission of 5 at.% Er:SrF₂ ceramic was much stronger than that of 5 at.% Er:CaF₂ ceramic, while the red emission of Er:SrF₂ ceramic was almost the same as that of Er:CaF₂ ceramic. The upconversion luminescence lifetime of Er:SrF₂ transparent ceramics was longer than that of Er:CaF₂.All the results indicated Er:SrF₂ transparent ceramics was a candidate for green fluorescent upconversion materials.     

Moderate temperature sintering of BaZr0.8Y0.2O3-δ protonic ceramics by A novel cold sintering pretreatment

The state-of-the-art protonic ceramic conductor BaZr_0.8Y_0.2O_3-δ (BZY20) requires an extremely high sintering temperature (≥1700 °C) to achieve the desired relative density and microstructure necessary to function as a proton conducting electrolyte. In this work, we developed a cold sintering pretreatment assisted moderate-temperature sintering method for the fabrication of high-quality pure BZY20 pellets. BZY20 pellets with high relative density of ~94% were fabricated with a final sintering temperature of 1500 °C (200 °C lower than the traditional sintering temperature). A comparison with BZY20 control samples indicated that the proper amount of BaCO₃ introduced on the BZY20 particle surface and the high green density achieved by cold sintering pretreatment were the main drivers for lowering the sintering temperature. The electrical conductivity measurement by electrochemical impedance spectroscopy showed that the as-prepared BZY20 pellets have a proton conductivity comparable to the state-of-the-art values. The cold sintering pretreatment outlined in this work has the potential to lower the sintering temperatures for similar types of protonic ceramic materials under consideration for a wide range of energy conversion and storage applications.