The influence of additives on microstrucutre of sub-micron alumina ceramics prepared by two-stage sintering

For various systems two-stage sintering has been reported as a successful way of suppressing the grain growth in the final stage of densification of polycrystalline ceramics. Our previous results on two-stage sintering of high purity submicrometre polycrystalline alumina indicate limited efficiency of the process with respect to suppression of grain growth. The present work deals with the influence of deliberate additions of various metal oxides (500 ppm of MgO, Y₂O₃ or ZrO₂) whose grain growth retarding effect in conventional sintering has been well documented, on two-stage sintering of submicrometre alumina ceramics. The addition of MgO was observed to enhance densification. Addition of yttria and zirconia impaired densification, but addition of all three dopants resulted in suppression of the grain growth and microstructure refinement in comparison to undoped alumina.     

Effect of hydroxyapatite and tricalcium phosphate addition on protein foaming-consolidation porous alumina

Porous alumina-hydroxyapatite (HA) and alumina-tricalcium phosphate (TCP) composites have been fabricated to investigate the effect of HA and ??-TCP addition on protein foaming-consolidation derived porous alumina. HA and ??-TCP loadings along with yolk content, starch content, and sintering temperature were varied to modulate performance of the porous composites. The rheological behavior of slurry shifted from pseudoplastic flow to a Newtonian fluid with increasing yolk concentration. The foaming capacity of slurry increased with yolk addition. The addition of starch into slurry resulted in bigger pore size and avoided the porous bodies from cracks. The shrinkage of sintered bodies increased with increasing HA loading, but decreased with increasing ??-TCP loading. The compressive strength of porous alumina-HA body was found 2.9?MPa at 45.8% porosity and 20.4?MPa at 36.8% porosity. The increasing porosity of porous alumina-TCP body from 56.1 to 61.6% improved the compressive strength from 3.1 to 4.2?MPa. Increasing sintering temperature resulted in large grain size among powder particles, thus improving the compressive strength of porous bodies. Preliminary results of DF-1 cells culture on the surface of porous alumina and alumina-TCP samples are also reported.     

泡沫陶瓷的研制

泡沫陶瓷是一种新型的功能陶瓷材料。它具有独特的结构和性能，在工业中有着广泛的应用前景。泡沫陶瓷具有密度小、透气性高、耐高温、抗化学腐蚀等特性。本研究对用颗粒强化的氧化铝骨架合成泡沫陶瓷进行了分析。这种材料比其它多孔陶瓷材料具有更好的热化学性质。这种材料可以用有机海绵浸浆获得，然后烧去海绵，留下多孔陶瓷网。这种方法的优点是它包含了过程参数和陶瓷结构，同时合成物的烧结情况及其它条件的影响在文中也有阐述。     

Hot-Pressing Alumina—Mechanisms of Material Transport

The effect of load on initial neck growth between alumina single-crystal spheres has been measured at 1530°C. The neck areas are larger than those observed in pressureless sintering and constant for all times between 10 and 480 minutes. The neck areas are proportional to the loads; i.e. they equilibrate at equal stresses (50,000 psi). It is shown quantitatively that the initial enhanced neck growth observed cannot be attributed to enhanced sintering by diffusion under the influence of stress. The plastic flow contribution to densification during hot-pressing is calculated from the stress inferred from the foregoing measurements, from the applied load in hot-pressing, and from geometric relations between particles. It is shown that for aluminum oxide the contribution of plastic flow to densification at the pressures normally used in hot-pressing is small. It is concluded that the final stage of densification of alumina during hot-pressing occurs by enhanced diffusion under the influence of stress.     

活性炭掺杂对多孔氧化铝陶瓷支撑体结构及性能的影响

以平均粒径为4μm的a-Al2O3为起始原料、活性炭为成孔剂,通过干压成型法制备片状多孔Al2O3支撑体。研究了活性炭含量对多孔氧化铝支撑体结构和性能的影响。结果表明：活性炭在高温烧成过程中的氧化可显著提高支撑体的孔隙率,进而提高其渗透性能。当活性炭添加量为17％（质量分数）、烧成温度为1450℃时,支撑体的孔隙率、平均孔径、三点抗弯强度和纯水渗透通量分别达到45．8％,2．1μm,44．6MPa和88m3／（m^2·h·MPa）。经过80℃、10％NaOH溶液腐蚀20d后,支撑体的三点抗弯强度仍可以维持在23．4MPa,表明支撑体具有较好的耐碱腐蚀性能。     

The Effect of Applied Stress on the Densification of a Low-Temperature Cofired Ceramic-Filled Glass System Under Constrained Sintering

The effect of uniaxial stress on the mechanical response and densification behavior of a low-fire borosilicate glass (BSG)+alumina system during constrained sintering of a multilayer BSG+alumina/alumina laminate has been investigated. Compared with free sintering, the pressure-less constrained sintering of BSG+alumina exhibits poorer densification, and larger porous bulk viscosity at a given temperature. This is caused by the in-plane tensile stress and anisotropic development generated in the transverse directions of the laminate during constrained sintering. The applied uniaxial stress required in the thickness direction to densify BSG+alumina under constrained sintering varies in the range of 50–400 kPa at 700°–800°C. The above results are in agreement with those calculated using the viscous analogy for the constitutive relationships of a porous sintering compact.     

Transient liquid phase sintering of high-purity mullite for high-temperature structural ceramics

High-purity mullite ceramics, promising engineering ceramics for high-temperature applications, were fabricated using transient liquid phase sintering to improve their high-temperature mechanical properties. Small amounts of ultrafine alumina or silica powders were uniformly mixed with the mullite precursor depending on the silica-alumina ratio of the resulting ceramics to allow for the formation of a transient liquid phase during sintering, thus, enhancing densification at the early stage of sintering and mullite formation by the reaction between additional alumina and the residual glassy phase (mullitization) at the final stage of sintering. The addition of alumina powder to the silica-rich mullite precursor resulted in a reaction between the glassy silica and alumina phases during sintering, thereby forming a mullite phase without inhibiting densification. The addition of fine silica powder to the mullite single-phase precursor led to densification with an abnormal grain growth of mullite, whereas some of the added silica remained as a glassy phase after sintering. The resulting mullite ceramics prepared using different powder compositions showed different sintering behaviors, depending on the amount of alumina added. Upon selecting an optimum process and the amount of alumina to be added, the pure mullite ceramics obtained via transient liquid phase sintering exhibited high density (approximately 99%) and excellent high-temperature flexural strength (approximately 320 MPa) at 1500 °C in air. These results clearly demonstrate that pure mullite ceramics fabricated via transient liquid phase sintering with compositions close to those of stoichiometric mullite could be a promising process for the fabrication of high-temperature structural ceramics used in an ambient atmosphere. The transient liquid phase sintering process proposed in this study could be a powerful processing tool that allows for the preparation of superior high-temperature structural ceramics used in the ambient processing atmosphere.     

Fabrication and characterisation of porous silicon nitride ceramics using Yb2O3 as sintering additive

Porous Si₃N₄ ceramics were fabricated by liquid-phase sintering with a Yb₂O₃ sintering additive, and the microstructure and mechanical properties of the ceramics were investigated, as a function of porosity. Low densification was achieved using a lower Yb₂O₃ additive content. Fibrous β-Si₃N₄ grains developed in the porous microstructure, and the grain morphology and size were affected by different sintering conditions. A high porosity, ∼40–60%, with β-Si₃N₄ grain development, was obtained by adjusting the additive content. Superior mechanical properties, as well as strain tolerance, were obtained for porous ceramics with a microstructure of fine, fibrous grains of a bimodal size distribution.     

Porous Mullite Preforms via Fused Deposition

Nonrandom porous mullite ceramic preforms were fabricated by the indirect fused deposition process. MgO was added to commercial mullite powders as a sintering aid. The influence of porosity and the amount of MgO on the densification and mechanical properties was studied. The shrinkage and compressive strength of the porous samples were found to increase with increasing MgO content. At constant MgO concentration, shrinkage was found to decrease linearly as the volume fraction of porosity increased. The compressive strength of porous samples decreased with an increase in the volume fraction of porosity at constant MgO content.     

Fabrication of mullite-bonded porous SiC ceramics via a sol–gel assisted in situ reaction bonding

In the present work, mullite-bonded porous SiC ceramics were fabricated using reaction bonding techniques. The morphologies, phase composition, open porosity, pore size distribution and mechanical strength of porous ceramics were examined as a function of alumina sources (calcined nano-sized alumina powder and alumina sol prepared from hydrolysis of aluminum isopropoxide) and contents. It was found that the addition of alumina in powder form effectively enhanced the strength and decreased the porosity. In contrast, when alumina was added in sol form, a reverse effect was observed. Moreover, it was revealed that when a portion of calcined alumina was replaced by alumina sol, the mechanical properties improved significantly (more than 30%) as well as porosity compared to the traditional method. Pore size distribution analysis showed that the dispersion of nanosize alumina powder and SiC micro-particles in alumina sol is strongly improved compared to mixing in ethanol.     

Transient liquid phase diffusion process for porous mullite ceramics with excellent mechanical properties

Porous mullite ceramics were fabricated by the transient liquid phase diffusion process, using quartz and fly-ash floating bead (FABA) particles and corundum fines as starting materials. The effects of sintering temperatures on the evolution of phase composition and microstructure, linear shrinkage, porosity and compressive strength of ceramics were investigated. It is found that a large amount of quartz and FABA particles can be transformed into SiO₂-rich liquid phase during the sintering process, and the liquid phase is transient in the Al₂O₃-SiO₂ system, which can accelerate the mullitization rate and promote the growth of mullite grains. A large number of closed pores in the mullite ceramics are formed due to the transient liquid phase diffusion at elevated temperatures. The porous mullite ceramics with high closed porosity (about 30%) and excellent compressive strength (maximum 105?MPa) have been obtained after fried at 1700?°C.     

Flash Spark Plasma Sintering of 3YSZ: Modified sintering pathway and impact on grain boundary formation

Yttria stabilized zirconia (3 mol% YSZ) ceramics were prepared by Flash-SPS, while allowing high heating rates up to 200 °C/s, which led to the extremely fast densification within a few seconds. The high heating rates had strong impact on sintering mechanisms, in terms of densification and grain growth. While the specimens ended with 5–15 vol% porosity and limited grain growth (< 350 nm), their hardness is higher than fully dense counterpart SPSed ceramics. Using the sintering trajectories, microstructural observations, and impedance spectroscopy, we highlight altered sintering mechanism which resulted in very thin grain boundaries compared to SPS. It appears that densification is largely advanced at grain boundary interfaces, with no residual nano-pores at the grain junctions, where some pores with size comparable to grain size were present. This opens up opportunities for the fabrication of porous lightweight ceramics with good mechanical properties.     

Effects of microwave sintering on the properties of porous hydroxyapatite scaffolds

Microwave sintering was used to process porous hydroxyapatite scaffolds fabricated by the extrusion deposition technique. The effects of microwave sintering on the microstructure, phase composition, degradation, compressive strength and biological properties of the scaffolds were investigated. After rapid sintering, scaffolds with controlled structure, high densification and fine grains were obtained. A significant increase in mechanical strength was observed relative to conventional sintering. The scaffolds (55–60% porosity) microwave sintered at 1200 °C for 30 min exhibited the highest average compressive strength (45.57 MPa). The degradation was determined by immersing the scaffolds in physiological saline and monitoring the Ca²⁺concentration. The results indicated that the microwave-sintered scaffolds possessed higher solubility than conventionally sintered scaffolds, as it released more Ca²⁺ at the same temperature. Furthermore, an in vitro MC3T3-E1 cell culturing study showed significant cell adhesion, distribution, and proliferation in the microwave-sintered scaffolds. These results confirm that microwave sintering has a positive effect on the properties of porous hydroxyapatite scaffolds for bone tissue engineering applications.     

Constrained Densification Kinetics of Alumina/Borosilicate Glass + Alumina/Alumina Sandwich Structure

The densification kinetics and mechanism of a low-temperature cofirable borosilicate glass (BSG) + alumina during the constrained sintering of a sandwich structure of alumina/(BSG + alumina)/alumina has been studied. The densification kinetics becomes slower when the BSG + alumina tape is constrained during firing. However, a viscous flow-controlling mechanism of the BSG also is still operative during free and constrained sintering. The densification behavior of constrained sintering can be mathematically described by free sintering, using the viscous analogy for the constitutive equations of a porous sintering glass.     

Processing of Porous SiC by Aluminum‐Derived Binders and Sacrificial Porogen Leaching Method

Porous SiC was successfully fabricated by a facile and energy efficient sacrificial porogen leaching method using in situ synthesized aluminum‐based binders by reaction bonding at low sintering temperatures of 600–1000°C. Porous SiC ceramics with porosity in the range of 30–58% and compressive strength of 1–33 MPa were obtained. Interconnected bimodal pores were produced by both stacking of SiC particles and leach out of salt. During sintering, the aluminum binder experienced metal to ceramic transformations forming various alumina polymorphs (γ, δ, θ and α‐Al₂O₃). The porogen content and sintering temperatures significantly influence the properties of porous SiC.     

High-Temperature Young's Modulus of Alumina During Sintering

High-temperature Young's modulus of a partially sintered alumina ceramic has been studied dynamically during the sintering process. Comparative, room-temperature Young's modulus data were obtained for a suite of partially sintered alumina compacts with different porosities. The dynamic Young's modulus of a 1200°C partially sintered material was observed to decrease linearly with temperature, but then above 1200°C it increased sharply as sintering and densification of the alumina became dominant. The evolution of the Young's modulus due purely to sintering exhibited an exponential relationship with porosity in excellent agreement with room-temperature measurements of equivalent porous alumina ceramics.     

Design and preparation of high permeability porous mullite support for membranes by in-situ reaction

The natural mineral kaolin combined with alumina additives Al(OH)₃,α-Al₂O₃ and AlF₃ was used to prepare porous mullite ceramic membrane supports using an in-situ reaction. The effects of composition and sintering temperature on the sintering behavior, pore structure, permeability and microstructure of the resulting porous mullite supports were extensively investigated. The experimental results showed that excess SiO₂ in kaolin can be consumed by adding alumina precursors, which resulted in a stiff skeleton of interlinked needle-like mullite crystals in-situ during the sintering. The needle-like mullite crystals touched each other and formed a short network, which acted as a porous skeletal network structure. This network resulted in a highly permeable porous structure. The resulting support is suitable for the preparation of asymmetric ceramic membranes. The densification and pore structure of the support can be effectively adjusted by control of the quantity of alumina precursors in the composition and the sintering temperature. Sintering the subject mullite compositions at 1500 °C for two hours resulted in support structures with an average porosity of 45.9%, an average pore size of 1.3 µm and a penetrating porosity of 35.9%.     

Enhanced mechanical properties for porous ceramics with an in situ formation of anorthite crystals during vitrification

Porous anorthite ceramics are widely applied as catalysis supports, separation membranes, and thermal insulations at high temperatures. In situ formation of anorthite crystals during vitrification is herein employed to improve mechanical properties of porous anorthite with modulated grain sizes on pore walls. Sintering parameters of shrinkage (5%–30%), open porosity (31.0%–58.3%), density (1.18–1.71 g/cm³), and mass loss (12.20%–18.26%) are estimated to investigate the influences of sintering aids of calcite, fused mullite, and silicon carbide or talcum on the densification processes of porous anorthite. The Kissinger equation is used to determine the activation energy of 783 kJ/mol for the crystallization of anorthite, which is significantly low for the formation of anorthite crystals through surface nucleation mechanism in present flux-rich melt. In situ crystallization and simultaneous densification under liquid drainages are favored for whiskers-reinforced mechanism to enhance flexural strengths (6.9–19.4 MPa) for porous anorthite with the porosity of 49.6%–58.3% through the formation of hierarchical nano- and microscale structures during vitrification.     

Sintering of Ultra-High-Purity Alumina Doped Simultaneously with MgO and FeO

The use of ultra-high-purity powder processing and multiple solid-solution additive doping has been evaluated as an effective approach for the fabrication of alumina ceramics. MgO was found to inhibit grain growth more strongly in very pure powders because of its stronger solute drag effect. The degree of inhibition was severe enough to render grain growth insensitive to porosity. By diminishing the dragging influence of pores on grain-boundary motion, MgO guards against abnormal grain growth due to inhomogeneous densification. FeO acted singly in alumina to promote grain growth more than densification. FeO was not, therefore, an effective sintering additive for undoped alumina. FeO did, however, Ceramic benefit the sintering of MgO-doped alumina.