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.     

Sintering,microstructure, and mechanical properties of vitrified bond diamond composite

The demand for high-performance grinding wheels is gradually increasing due to rapid industrial development. Vitrified bond diamond composite is a versatile material for grinding wheels used in the backside grinding step of Si wafer production. However, the properties of the vitrified bond diamond composite are controlled by the characteristics of the diamond particles, the vitrified bond, and pores and are very complicated. The main objective of this study was to investigate the effects of SiO₂–Na₂O–B₂O₃–Al₂O₃–Li₂O–K₂O–CaO–MgO–ZrO₂–TiO₂–Bi₂O₃ glass powder on the sintering, microstructure, and mechanical properties of the vitrified bond diamond composite. The elemental distributions of the composite were analyzed using electron probe micro-analysis (EPMA) to clarify the diffusion behaviors of various elements during sintering.The results showed that the relative density and transverse rupture strength of the composite sintered at 620 °C were 91.7% and 126 MPa, respectively. After sintering at 680 °C, the glass powder used in this study exhibited a superior forming ability without an additional pore foaming agent. The relative density and transverse rupture strength of the composite decreased to 48.2% and 49 MPa, respectively. Moreover, the low sintering temperature of this glass powder protected the diamond particles from graphitization during sintering, as determined by X-ray diffraction and Raman spectrum. Furthermore, the EPMA results indicate that Na diffused and segregated at the interface between the diamond particles and vitrified bond, contributing to the improved bonding. The diamond particles can remain effectively bonded by the vitrified bond even after fracture.     

Low-temperature constrained sintering of YSZ electrolyte with Bi2O3 sintering sacrificial layer for anode-supported solid oxide fuel cells

Solid oxide fuel cells (SOFCs) have strong potential for next-generation energy conversion systems. However, their high processing temperature due to multi-layer ceramic components has been a major challenge for commercialization. In particular, the constrained sintering effect due to the rigid substrate in the fabrication process is a main reason to increase the sintering temperature of ceramic electrolyte. Herein, we develop a bi-layer sintering method composed of a Bi₂O₃ sintering sacrificial layer and YSZ main electrolyte layer to effectively lower the sintering temperature of the YSZ electrolyte even under the constrained sintering conditions. The Bi₂O₃ sintering functional layer applied on the YSZ electrolyte is designed to facilitate the densification of YSZ electrolyte at the significantly lowered sintering temperature and is removed after the sintering process to prevent the detrimental effects of residual sintering aids. Subsequent sublimation of Bi₂O₃ was confirmed after the sintering process and a dense YSZ monolayer was formed as a result of the sintering functional layer-assisted sintering process. The sintering behavior of the Bi₂O₃/YSZ bi-layer system was systematically analyzed, and material properties including the microstructure, crystallinity, and ionic conductivity were analyzed. The developed bi-layer sintered YSZ electrolyte was employed to fabricate anode-supported SOFCs, and a cell performance comparable to a conventional high temperature sintered (1400 °C) YSZ electrolyte was successfully demonstrated with significantly reduced sintering temperature (<1200 °C).     

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.     

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.     

Investigation on the anti-reduction mechanism of Ti4+ in high dielectric constant system Ca0.9La0.067TiO3 by doping with Al2O3

Ca_0.9La_0.067TiO₃ (abbreviated as CLT) ceramics doped with different amount of Al₂O₃ were prepared via the solid state reaction method. The anti-reduction mechanism of Ti⁴⁺ in CLT ceramics was carefully investigated. X-ray diffraction (XRD) was used to analyze the phase composition and lattice structure. Meanwhile, the Rietveld method was taken to calculate the lattice parameters. X-ray photoelectron spectroscopy (XPS) was employed to study the valence variation of Ti ions in CLT ceramics without and with Al₂O₃. The results showed that Al³⁺ substituted for Ti⁴⁺ to form solid solution and the solid solubility limit of Al³⁺ is near 1.11 mol%. Furthermore, the reduction of Ti⁴⁺ in CLT ceramics was restrained by acceptor doping process and the Q × f values of CLT ceramics were improved significantly. The CLT ceramic doped with 1.11 mol% Al₂O₃ exhibited good microwave dielectric properties: ε_r = 141, Q × f = 6848 GHz, τ_f = 576 ppm/°C.     

Effect of polyethyleneimine-fatty acid complex type dispersant structure on the overall processing chain of Si3N4 ceramics using multicomponent non-aqueous slurries

The effect of fatty acid structure of polyethyleneimine (PEI)-fatty acid complex, which was designed as a polymer dispersant for multi-component non-aqueous slurries, on the overall processing chain of Si₃N₄ ceramics involving slurry stabilization, spray drying, compaction, and liquid sintering was investigated using PEI-oleic acid (PEI-OA) and PEI-isostearic (PEI-ISA) complexes. Si₃N₄-Y₂O₃-Al₂O₃-AlN-TiO₂/toluene slurries were selected as a real model for Si₃N₄-based multicomponent slurries. It was observed that both PEI-OA and PEI-ISA can stabilize Si₃N₄-Y₂O₃-Al₂O₃-AlN-TiO₂/toluene slurries; however, the PEI-ISA system tended to have slightly higher slurry viscosity, which was suspected to be due to the interactions between protruded PEI segments among short ISA chains. The spray-dried granules from PEI-ISA-stabilized slurry were observed to have filled structures with higher surface roughness whereas those prepared from PEI-OA-stabilized slurry were observed to have hollow-structured granules. The granules prepared from PEI-OA slurry had improved flow and compaction properties with higher relative density of green compacts compared with those prepared from PEI-ISA-stabilized slurry, whereas the relative density and microstructural homogeneity of S₃N₄ ceramics sintered at 1600?°C for 2?h were observed to be higher for the PEI-ISA system. It is suspected that PEI-OA effectively improved the dispersion stability of multicomponent slurries and flow/compaction properties of granules; however, the inhomogeneous microstructures of green compacts induced by the hollow-structured granules had an adverse effect on the sintering of Si₃N₄ ceramics.     

High performance multi-layer varistor (MLV) from doped ZnO nanopowders by water based tape casting: Rheology,sintering, microstructure and properties

In this work, we report the fabrication of a high performance multi-layer varistor (MLV) via water based tape casting method using novel compositions of nanomaterials. Bi₂O₃, CaO and Co₃O₄ doped ZnO nanopowders were prepared by solution combustion synthesis (SCS) route, calcined at different temperatures (550, 650, 750 and 850?°C) and characterized by TEM, XRD, SEM and AFM. The nanopowder (crystallite size ~30?nm) calcined at 650?°C for 1?h was used as the starting material for MLV fabrication. Compositions of the slurry containing doped ZnO nanopowders, binder and plasticizer in water solvent were optimized for the fabrication of thick film. The rheological properties of the slurries having different solid loadings were analysed and thick films of various thicknesses (50–500?µm) were prepared by varying the feeding rate of tape casting. The film roughness of 38.3?nm for the thick film made from 40?wt% solid slurry was found to be superior compared to other samples due to the presence of reduced crack and shrinkage. MLV fired at 950?°C for 1.5?h exhibited a coefficient of nonlinearity of 18 and breakdown voltage of 291.5?V that yields superior properties compared to commercial MLVs.