A benzoate coprecipitation route for synthesizing nanocrystalline GDC powder with lowered sintering temperature

Electrolyte powders with low sintering temperature and high-ionic conductivity can considerably facilitate the fabrication and performance of solid oxide fuel cells (SOFCs). Gadolinia-doped ceria (GDC) is a promising electrolyte for developing intermediate- and low-temperature (IT and LT) SOFCs. However, the conventional sintering temperature for GDC is usually above 1200 °C unless additives are used. In this work, a nanocrystalline powder of GDC, (10 mol% Gd dopant, Gd_0.1Ce_0.9O_1.95) with low-sintering temperature has been synthesized using ammonium benzoate as a novel, environmentally friendly and cost-effective precursor/precipitant. The synthesized benzoate powders (termed washed- and non-washed samples) were calcined at a relatively low temperature of 500 °C for 6 h. Physicochemical characteristics were determined using thermal analysis (TG/DTA), Raman spectroscopy, FT-IR, SEM/EDX, XRD, nitrogen absorptiometry, and dilatometry. Dilatometry showed that the newly synthesized GDC samples (washed and non-washed routes) start to shrink at temperatures of 500 and 600 °C (respectively), reaching their maximum sintering rate at 650 and 750 °C. Sintering of pelletized electrolyte substrates at the sintering onset temperature for commercial GDC powder (950 °C) for 6 h, showed densification of washed- and non-washed samples, obtaining 97.48 and 98.43% respectively, relative to theoretical density. The electrochemical impedance spectroscopy (EIS) analysis for the electrolyte pellets sintered at 950 °C showed a total electrical conductivity of 3.83 × 10^?2 and 5.90 × 10^?2 S cm^?1 (under air atmosphere at 750 °C) for washed- and non-washed samples, respectively. This is the first report of a GDC synthesis, where a considerable improvement in sinterability and electrical conductivity of the product GDC is observed at 950 °C without additives addition.     

Sintering of WC-Ni nanocomposite powder: Experimental and artificial neural networks modeling study

The sintering behavior of WC-Ni nanocomposite powder was evaluated through experimental and statistical approaches to study the contribution of involving parameters of chemical composition (Ni wt. %) and sintering temperature on sinterability of system by assessing the resulted densification and microhardness. The experimental process was designed based on factorial experimental design for independent effective parameters of Ni percentage (12, 18 and 23 wt %), and sintering temperature (8 different values within 1350–1485 °C). The resulted products of experimental testing after compaction and sintering were analyzed by FESEM and EDX to image the microstructure and evaluate the chemical composition and elemental distribution. The density and microhardness were measured as well. An artificial neural network (ANN) was applied to describe the corresponding individual and mutual impacts on sintering. The ANN model was developed by feed-forward back propagation network including topology 2:5:2 and trainlm algorithm to model and predict density and microhardness. A great agreement was observed between the predicted values by the ANN model and the experimental data for density and microhardness (regression coefficients (R²) of 0.9983 and 0.9924 for target functions of relative density and microhardness, respectively). Results showed that the relative importance of operating parameters on target functions (relative density and microhardness) was found to be 62% and 38% for sintering temperature and Ni percentage, respectively. Also, ANN model exhibited relatively high predictive ability and accuracy in describing nonlinear behavior of the sintering of WC-Ni nanocomposite powder. The experimental results confirmed that the appropriate sintering temperature was influenced by Ni content. The optimum parameters were found to be 12 wt % Ni sintered at 1460 °C with the highest microhardness and relative density.     

Effect of temperature on the structure and mechanical properties of SiC–TiB2 composite ceramics by solid-phase spark plasma sintering

SiC composite ceramics have good mechanical properties. In this study, the effect of temperature on the microstructure and mechanical properties of SiC–TiB₂ composite ceramics by solid-phase spark plasma sintering (SPS) was investigated. SiC–TiB₂ composite ceramics were prepared by SPS method with graphite powder as sintering additive and kept at 1700 °C, 1750 °C, 1800 °C and 50 MPa for 10min.The experimental results show that the proper TiB₂ addition can obviously increase the mechanical properties of SiC–TiB₂ composite ceramics. Higher sintering temperature results in the aggregation and growth of second-phase TiB₂ grains, which decreases the mechanical properties of SiC–TiB₂ composite ceramics. Good mechanical properties were obtained at 1750 °C, with a density of 97.3%, Vickers hardness of 26.68 GPa, bending strength of 380 MPa and fracture toughness of 5.16 MPa m^1/2.     

Fabrication and properties of diatomite ceramics with hierarchical pores based on direct stereolithography

Porous diatomite ceramics with hierarchical pores and high apparent porosity (50.29–56%) were successfully fabricated via direct stereolithography. The pre-ball-milling time, dispersant type and dispersant concentration were systematically investigated to prepare diatomite pastes with high solid loading, low viscosity and a self-supporting effect. The results showed that a pre-ball-milling time of 24 h was more suitable to prepare diatomite pastes with high solid loading, and Span80 at 2 wt% was the optimal dispersant to obtain 40 vol% diatomite paste with a low viscosity and a self-supporting effect. To restrain the formation of defects, a heating rate as low as 0.2 °C/min was allowed to control the pyrolysis rate in the multistage debinding process. At sintering temperatures ranging from 900 °C to 1000 °C, porous diatomite ceramics exhibited a typical bimodal porosity, high apparent porosity and great flexural strength.     

Fabrication method,dielectric properties,and electromagnetic absorption performance of high alumina fly ash-based ceramic composites

Mullite-Al₂O₃-SiC composites were in-situ synthesized through carbothermal reduction reaction of fly ash (FA) with a high alumina content and activated carbon (AC). The effects of sintering temperature, holding time, and amount of AC on the β-SiC yield, microstructure, dielectric properties, and electromagnetic (EM) absorption performance of the composites in the 2–18 GHz frequency range were studied. The results show that increasing the AC improves the porosities of the composites, with the highest porosity of 56.17% observed. The β-SiC yield varies considerably as the sintering parameters were altered, with a maximum yield of 23% achieved under conditions of 12 wt% AC, 1400 °C sintering temperature, and 3 h holding time. With a thickness of 3.5 mm, this composite has excellent EM absorption performance, exhibiting a minimum reflection loss (RL_min) of -51.55 dB at 7.60 GHz. Significantly, the maximum effective absorption bandwidth (EAB) reaches 3.39 GHz when the thickness is 3.0 mm. These results demonstrate that the composite prepared under ideal conditions can absorb 99.99% of the waves passing through it. Because of the interfacial polarization, conductive loss, and impedance matching of the heterostructure, the synthesized mullite-Al₂O₃-SiC composites with densities ranging from 1.43 g/cm³ to 1.62 g/cm³ demonstrate outstanding EM attenuation capabilities. Therefore, this study presents a remarkable way of utilizing fly ash to fabricate inexpensive, functional ceramic materials for EM absorption applications.     

Effects of particle size distribution and sintering temperature on properties of alumina mold material prepared by stereolithography

Alumina mold materials prepared by stereolithography usually have considerable sintering shrinkage, and their properties related to casting have been rarely studied. In this study, alumina molds materials were prepared by stereolithography, and the effects of particle size distribution and sintering temperature on the properties of the materials were investigated. Results show that the viscosity of the slurries decreases as the fraction of fine powder increases, and the particle size distribution affects the curing behaviors slightly. Sintering shrinkage increases as the fraction of fine powder or the sintering temperature increases. Although lower sintering shrinkage can be achieved by sintering at 1350 °C or 1450 °C, the mold materials sintered at lower temperatures would continue to shrink under the service temperature of 1550 °C, and thus 1550 °C is determined as the optimal sintering temperature. As the fraction of fine powder increases, the creep resistance first increases and then decreases, and specimens prepared with 0.1 fraction of fine powder exhibit the best creep resistance with the droop distance of 4.44 ± 0.45 mm. Specimens prepared with 0.1 fraction of fine powder and sintered at 1550 °C exhibit linear shrinkage of 6.36% along the X/Y direction and 11.39% along the Z direction, and have a flexural strength of 78.15 ± 3.50 MPa and porosity of 30.12 ± 0.08%. The resulting material possesses relatively low sintering shrinkage, proper mechanical strength, porosity and high-temperature properties that meet the requirements for casting purposes.     

Microstructure and mechanical properties of B4C matrix composites prepared via hot-pressing sintering with Pr6O11 as additive

High-performance B₄C-PrB₆ composites were prepared via hot-pressing sintering with matrix phase B₄C and with 2–5 wt% Pr₆O₁₁ as additive. The effects of different sintering processes and Pr₆O₁₁ content on the microstructure and mechanical properties of the composites were studied in detail. It is found that increasing sintering temperature and pressure will contribute to the densification of B₄C-PrB₆ composites. Coarse grains are formed in B₄C without additives at high temperature conditions, resulting in the decrease of the densification. Pr₆O₁₁ can effectively hinder the formation of coarse grains and finally promote the densification of the composites. The main toughening mechanisms of composites was crack deflection. The composites with 4 wt% Pr₆O₁₁ prepared at 2050 °C and 25 MPa had the best comprehensive mechanical properties. The relative density, hardness, flexural strength and fracture toughness reached to 98.9%, 37.6 GPa, 339 MPa and 4.4 MP am^1/2, respectively.     

Microstructure and thermal expansion behavior of diamond/SiC/(Si) composites fabricated by reactive vapor infiltration

Diamond/SiC/(Si) composites were fabricated by Si vapor vacuum reactive infiltration. The coefficient of thermal expansion (CTE) of composites have been measured from 50 to 400 °C. With the diamond content increasing, CTE of composite decreased, simultaneously, the microstructure of the composites changed from core–shell particles embedded in the Si matrix to an interpenetrating network with the matrix. The CTEs of composites versus temperature matched well with those of Si. The Kerner model was modified according to the structural features of the composites, which exhibited more accurate predictions due to considering the core–shell structure of the composites. The thermal expansion behavior of the matrix was constrained by diamond/SiC network during heating.     

Microwave versus conventional sintering: Estimate of the apparent activation energy for densification of α-alumina and zinc oxide

A comparative study between the conventional and 2.45 GHz microwave multimode sintering behavior of insulator (α-Al₂O₃) and semi-conductive ceramic (ZnO) was systematically investigated. The apparent activation energy of nonisothermal sintering was determined by way of the Arrhenius plot of densification data at constant heating rates (CHR) and the concepts of Master Sintering Curves (MSCs), respectively. During microwave densification process, the apparent activation energy was about 90 kJ/mol less than the value for conventional sintering of Al₂O₃ applying these two estimation methods. However, an opposite result was obtained in the case of ZnO, although its densification process had been also accelerated by microwave as well as Al₂O₃. The significant differences in activation energy give a good proof of the difference in diffusion mechanism induced by the electromagnetic field underlying microwave sintering.     

High-strength AlN ceramics by low-temperature sintering with CaZrO3–Y2O3 co-additives

Aluminum nitride (AlN) ceramics with the concurrent addition of CaZrO₃ and Y₂O₃ were sintered at 1450-1700 °C. The degree of densification, microstructure, flexural strength, and thermal conductivity of the resulting ceramics were evaluated with respect to their composition and sintering temperature. Specimens prepared using both additives could be sintered to almost full density at relatively low temperature (3 h at 1550 °C under nitrogen at ambient pressure); grain growth was suppressed by grain-boundary pinning, and high flexural strength over 630 MPa could be obtained. With two-step sintering process, the morphology of second phase was changed from interconnected structure to isolated structure; this two-step process limited grain growth and increased thermal conductivity. The highest thermal conductivity (156 Wm⁻¹ K⁻¹) was achieved by two-step sintering, and the ceramic showed moderate flexural strength (560 MPa).