Fabrication and properties of pressure-sintered reaction-bonded Si3N4 ceramics with addition of Eu2O3–MgO–Y2O3

Dense pressure-sintered reaction-bonded Si₃N₄ (PSRBSN) ceramics were obtained by a hot-press sintering method. Precursor Si powders were prepared with Eu₂O₃–MgO–Y₂O₃ sintering additive. The addition of Eu₂O₃–MgO–Y₂O₃ was shown to promote full nitridation of the Si powder. The nitrided Si₃N₄ particles had an equiaxial morphology, without whisker formation, after the Si powders doped with Eu₂O₃–MgO–Y₂O₃ were nitrided at 1400 °C for 2 h. After hot pressing, the relative density, Vickers hardness, flexural strength, and fracture toughness of the PSRBSN ceramics, with 5 wt% Eu₂O₃ doping, were 98.3 ± 0.2%, 17.8 ± 0.8 GPa, 697.0 ± 67.0 MPa, and 7.3 ± 0.3 MPa m^1/2, respectively. The thermal conductivity was 73.6 ± 0.2 W m^?1 K^?1, significantly higher than the counterpart without Eu₂O₃ doping, or with ZrO₂ doping by conventional methods.     

Dual effect synergistically triggered Ce:(Y,Tb)3(Al,Mn)5O12 transparent ceramics enabling a high color-rendering index and excellent thermal stability for white LEDs

Ce:Y₃Al₅O₁₂ transparent ceramics (TCs) with appropriate emission light proportion and high thermal stability are significant to construct white light emitting diode devices with excellent chromaticity parameters. In this work, strategies of controlling crystal-field splitting around Ce³⁺ ion and doping orange-red emitting ion, were adopted to fabricate Ce:(Y,Tb)₃(Al,Mn)₅O₁₂ TCs via vacuum sintering technique. Notably, 85.4 % of the room-temperature luminescence intensity of the TC was retained at 150 °C, and the color rendering index was as high as 79.8. Furthermore, a 12 nm red shift and a 16.2 % increase of full width at half maximum were achieved owing to the synergistic effects of Tb³⁺ and Mn²⁺ ions. By combining TCs with a 460 nm blue chip, a warm white light with a low correlated color temperature of 4155 K was acquired. Meanwhile, the action mechanism of Tb³⁺ ion and the energy transfer between Ce³⁺ and Mn²⁺ ions were verified in prepared TCs.     

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.     

Mechanical properties and thermal shock in thin ZrO2–Y2O3–Al2O3 films obtained by the sol-gel method

Thin multilayer coatings of ZrO₂–Y₂O₃–Al₂O₃ were prepared using the sol-gel method and dip-coating technique in order to advance in the study of what influence the incorporation of Al₂O₃ has on films of Y₂O₃-doped ZrO₂, investigating its role in the synthesis of the solutions and in the characteristics and properties of the coatings. After the characterization of the solutions used in the process, the microstructure of the films was studied and their mechanical behaviour and resistance to thermal shock were determined so as to optimize the characteristics and functionality of these coatings. With increased alumina content, 3YSZ-Al₂O₃ (20 mol%), the cubic phase of the zirconia disappeared completely at the sintering temperature used (700 °C), resulting in the tetragonal phase with Al in solution. There was also a decrease in the coatings' hardness and Young's modulus, and an increase in toughness and resistance to thermal shock. These results allow guidelines to be established for the design of multilayer structures that are, tougher, more resistant, and have improved surface properties.     

Performance of Al2O3 particle reinforced glass-based seals in planar solid oxide fuel cells

Glass-based materials are usually considered as excellent seals for jointing adjacent components in planar solid oxide fuel cells, but the uncontrollable crystallization in the glass may cause delamination and micro-cracks in such seals. To solve this problem, Al2O3 ceramic particles were added to a BaO–CaO–Al2O3–B2O3–SiO2 glass system to reduce negative effects caused by crystalline phase on the gas tightness and the joint strength in the seals. At an operating temperature of 750 °C, the glass-based seals with 20 wt% Al2O3 addition (GA80) exhibited extremely low leakage rates (~0.002 sccm/cm under an input gas pressure of 13.6 kPa) and higher shear strength (3.31 MPa). The Al2O3 ceramic addition and the crystalline phase BaAl2Si2O8 reinforced the glass matrix. Further thermal cycle analyses indicated that leakage rates for the GA80 seals remained at around 0.0025 sccm/cm after 10 thermal cycles, which was consistent with minor microstructural change and good interface bonding. Single cell testing with of GA80 seals was performed and the results demonstrated stable electrochemical performance through 6 thermal cycles at an open circuit voltage of 1.16–1.18 V, as well as a power density above 546 mW/cm2 at a current density of 925 mA/cm2. These results showed the high thermal cycle stability of the glass/Al2O3 composite seals in intermediate temperature planar solid oxide fuel cells.     

An ultrasonic study on ternary xPbO–(45-x)CuO–55B2O3 glasses

A series of xPbO–(45-x)CuO–55B₂O₃ glasses (5 ≤ x ≥ 40 mol %) were prepared by the melt-quenching technique. The X-ray diffraction (XRD) patterns of the prepared glasses are found to have amorphous structure. An extensive ultrasonic study has been made to explore the structural role of PbO and CuO in the borate network. Various elastic properties were calculated from the measured data of density and ultrasonic velocity. Ultrasonic velocity and elastic moduli revealed broad humps at about 20 mol % PbO, which are attributed to the borate anomaly. Below 20 mol % PbO, all Pb²⁺ ions are considered to be entering the borate network as a glass modifier. This results in the transforms the borate network from an open structure to a denser three-dimensional structure due to BO₃ → BO₄ conversion. Beyond 20 mol, addition of PbO results in the formation of metaborate, pyroborate, and orthoborate units with NBOs. This weakness the glass structure and decrease both ultrasonic velocity and elastic moduli. The elastic properties were predicted and quantitatively analyzed by taking into account the effect of boron coordination number on the compositional and structural parameters involved in Makishima–Mackenzie's theory, ring deformation model and bond compression model. An excellent agreement between the computed theoretical and experimental elastic moduli, micro-harness and Poisson's ratio was achieved for majority of samples.     

LCD-SLA 3D printing of BaTiO3 piezoelectric ceramics

Stereolithography-based 3D printing is a promising method to produce complex shapes from piezoceramic materials. In this study, LCD-SLA 3D printing was used to create lead-free piezoceramics based on barium titanate (BaTiO₃, BT). Three types of BT powders (micron, submicron and nanoscale) were tested in LCD-SLA 3D printing, and a technique for the preparation of a ceramic slurry suitable for LCD-SLA printing has been developed. Using TGA-DSC analysis, the thermal debinding parameters to obtain crack-free samples were determined, followed by further sintering and the study of the piezoelectric properties (ε_r = 1965, d₃₃ = 200 pC/N, tan = 1,7 %). The results of the study demonstrate high potential for the production of complex piezoceramic elements that can be used in aviation, in particular, aviation radio equipment; in the marine industry for transceiver modules of hydroacoustic antennas; and in the nuclear industry for pressure control sensors in the steam–water path.     

Low thermal conductivity in porous SiC–SiO2–Al2O3–TiO2 ceramics induced by multiphase thermal resistance

The introduction of multiple heterogeneous interfaces in a ceramic is an efficient way to increase its thermal resistance. Novel porous SiC–SiO₂–Al₂O₃–TiO₂ (SSAT) ceramics were fabricated to achieve multiple heterogeneous interfaces by sintering equal volumes of SiC, SiO₂, Al₂O₃, and TiO₂ compacted powders with polysiloxane as a bonding phase and carbon as a template at 600 °C in air. The porosity could be controlled between 66% and 74% by adjusting the amounts of polysiloxane and the carbon template. The lowest thermal conductivity (0.059 W/(m·K) at 74% porosity) obtained in this study is an order of magnitude lower than those (0.2–1.3 W/(m·K)) of porous monolithic SiC, SiO₂, Al₂O₃, and TiO₂ ceramics at an equivalent porosity. The typical specific compressive strength value of the porous SSAT ceramics at 74% porosity was 3.2 MPa cm³/g.     

Enhanced thermal shrinkage behavior of phenolic-derived carbon aerogel-reinforced by HNTs with superior compressive strength performance

A novel carbon/m-HNTs composite aerogel was synthesized by introducing the modified halloysite nanotubes (m-HNTs) into phenolic (PR) aerogels through chemical grafting, followed with carbonization treatment. In order to explore the best proportion of HNTs to phenolic, the micromorphology of PR/m-HNTs were investigated by SEM before carbonization, confirming 10 wt% of m-HNTs is most beneficial to the porous network of aerogels. The interaction between PR and HNTs was studied by FTIR spectra, and microstructure evolution of the target product-carbon/m-HNTs composite aerogel were illustrated by SEM and TEM techniques. SEM patterns indicated that the carbon/m-HNTs aerogels maintain a stable porous structure at 1000 °C (carbonization temperature), while a ~20 nm carbon layer was formed around m-HNTs generating an integral unit through TEM analysis. Specific surface area and pore size distribution of composite aerogels were analyzed based on mercury intrusion porosimetry and N₂ adsorption–desorption method, the obtained results stayed around 500 m²g^?1 and 1.00 cm³g^?1 (pore volume) without significant discrepancy, compared with pure aerogel, showing the uniformity of pore size. The weight loss rate (26.76%) decreased greatly compared with pure aerogel, at the same time, the best volumetric shrinkage rate was only 30.83%, contributed by the existence of HNTs supporting the neighbor structure to avoid over-shrinking. The highest compressive strength reached to 4.43 MPa, while the data of pure aerogel was only 1.52 MPa, demonstrating the excellent mechanical property of carbon/m-HNTs aerogels.