The effect of carbon coating of AIN powder on sintering behavior and thermal conductivity

High thermal conductive AlN ceramics doped with Y₂O₃ were produced by sintering the powders obtained after applying a carbon coating to the surface of AlN powder grains. During sintering at 1800°C for 1 hour, the carbon reacts with the surface of the AlN grains by carbothermal-reduction of Al₂O₃, and also with the Al₂Y₄O₉ intermediate phase to form AlN, Y₂O₃ and CO. By adding 0.56 mass% of carbon, almost all the Al₂Y₄O₉ is reacted and the thermal conductivity increases from 184 W/(m · K) to 224 W/(m · K). Further carbon addition decreases the thermal conductivity and also the final sintered density.     

Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

Phase separation and toughening of SiC-AIN solid-solution ceramics

SiC-AIN solid-solution ceramics were prepared by pressureless sintering using Al₂O₃ and Y₂O₃ as the sintering additives. The resulting ceramics were subjected to annealing treatments over a range of temperatures from 1400 °C to 1800 °C in the spinodal region. The fracture toughness of the annealed ceramics was examined, by the indentation method, in relation to the annealing temperature and annealing time. X-ray diffraction profiles revealed that phase separation occurred during annealing. In ceramics containing 50 mol % SiC annealed at 1800 °C, the morphology of the phase separation is the characteristic modulated stratiform structure. Energy-dispersive X-ray spectroscopy (EDS) showed that the structure consisted of alternations of silicon-rich and aluminium-rich composition. The fracture toughness of the annealed ceramics increased compared to the as-sintered solid-solution ceramics. The phase separation is expected to contribute to the toughening of ceramics with nanometre-scale texture.     

Effect of a small amount of liquid-forming additives on the microstructure of Al2O3 ceramics

Sintering behaviour and microstructure of Al₂O₃ ceramics without additives and with 0.02–0.25 mol% CaO + SiO₂ (CaO/SiO₂ = 1) were investigated. When Al₂O₃ bodies were sintered at 1400 °C, the sinterability and the grain size decreased as the content of CaO + Si₂ increased. When Al₂O₃ ceramics with 0.05 – 0.25 mol% CaO + SiO₂ were sintered at higher sintering temperature, both CaO and SiO₂ reacted with Al₂O₃ to produce the liquid phase along grain boundaries, and exaggerated platelet Al₂O₃ grains, with an aspect ratio of about 4.5, were formed. Because the size of platelet grains decreased as the content of CaO + SiO₂ increased, the distribution of either SiO₂ particles or this intergranular phase of CaO – Al₂O₃ – SiO₂ might control the microstructure.     

The effects of pre-oxidation on the sintering and mechanical property of powder injection moulded SiC material

Usually, injection moulded SiC green parts are debound in inert atmosphere or vacuum, which induces the residual carbon and increases forming cycle and production cost. In this paper, injection moulded SiC with Al₂O₃ and Y₂O₃ as sintering assistant was thermal debound in air and Ar, respectively. The paper investigates the effects of pre-oxidation during debinding stage on the sintering and mechanical property of SiC material. During sintering, the oxide SiO₂ is in favour of the shrinkage of debound samples at lower temperature. After sintering, the linear shrinkage of sintered samples with pre-oxidation is bigger than the sample without pre-oxidation. Test results by TEM and XRD indicate that SiO₂ disappear from the inside of the sintered samples. The loss of SiO₂ decreases the content of Al₂O₃, which affects the formation of YAG (Y₃Al₅O₁₂). Sintered Sic samples contain α-SiC phase and intergranular phase. There is no hetero-phase between the boundaries of α-SiC phase and intergranular phase. The bending and compression strength values of sintered samples with pre-oxidation reach to 537 MPa and 2.89 GPa, respectively. These values approach the strength of sintered samples without pre-oxidation (594 MPa and 3.0 GPa).     

Thermal stability and mechanical properties of yttria-doped tetragonal zirconia polycrystals with dispersed alumina and silicon carbide particles

Yttria-doped tetragonal zirconia polycrystals in which were dispersed various amounts of Al₂O₃ and SiC particles were sintered at 1500° C for 3 h, and the mechanical properties and the thermal stability of the sintered bodies were evaluated. Dispersion of Al₂O₃ caused no significant effect on sinterability, and increased the hardness and elasticity of the composites. Dispersion of SiC particles decreased the relative density and the grain size of composites. Elasticity and hardness increased by dispersing less than 10 vol% SiC, but decreased above 10 vol% SiC due to the decrease of relative density. Dispersion of both Al₂O₃ and SiC particles slightly increased the fracture toughness of ZrO₂-3 mol% Y₂O₃ ceramics but significantly decreased that of ZrO₂-2 mol% Y₂O₃ ceramics. The rate of the tetragonal-to-monoclinic phase transformation decreased by dispersing both Al₂O₃ and SiC particles. The transformation depth increased rapidly and then slowly with increasing the annealing time. The rate of increase in the transformation depth greatly decreased by dispersing Al₂O₃ particles.     

Pressureless sintering of SiC-TiC composites with improved fracture toughness

Composites of SiC-TiC containing up to 45 wt% of dispersed TiC particles were pressureless sintered to 97% of theoretical density at temperatures between 1850°C and 1950°C with Al₂O₃ and Y₂O₃ additions. An in situ-toughened microstructure, consisted of uniformly distributed elongated -SiC grains, matrixlike TiC grains, and yttrium aluminum garnet (YAG) as a grain boundary phase, was developed via pressureless sintering route in the composites sintered at 1900°C. The fracture toughness of SiC-30 wt% TiC composites sintered at 1900°C for 2 h was as high as 7.8 MPa·m^1/2, owing to the bridging and crack deflection by the elongated -SiC grains.     

Crystallization of the glassy phase in an Si3N4 material by post-sintering heat treatments

It is shown that post-sintering heat treatments in air in the temperature range 1100 to 1400° C result in substantial crystallization of the glassy phase in an Si₃N₄ material which was produced by the nitridation pressureless sintering (NPS) method using Y₂O₃ and Al₂O₃ as sintering aids. X-ray diffraction combined with analytical electron microscopy showed that the secondary crystalline phases which form are strongly dependent upon time and temperature of heat treatment as well @S depth below the oxide scale. This effect is primarily due to the outward diffusion of cations (yttrium, aluminium and impurities) as well as the inward diffusion of oxygen. Small glassy pockets and thin amorphous intergranular films remain in the microstructure after heat treatment.     

Effect of CuO additives on the reversibility of zirconia crystalline phase transitions

We have studied the influence of the differents atmospheres on the sintering of CuO-doped-zirconia ceramics. After an annealing treatment in a reducing atmosphere, we have found nanoparticles of metallic copper in triple points and in the grains of the sintered zirconia. Furthermore, the influence of the intergranular Y₂Cu₂O₅ phase on the tetragonal to monoclinic phase transition and the crystalline structure of zirconia is discussed with respect to results obtained from X-ray diffraction, differential thermal analysis, Raman spectroscopy and High Resolution Transmission Electron Microscopy.     

Study on microstructures and mechanical properties of short-carbon-fiber-reinforced SiC composites prepared by hot-pressing

Short-carbon-fiber-reinforced silicon carbide composites were prepared by hot-pressing with SiC powder, Polycarbosilane as precursor polymer and MgO–Al₂O₃–Y₂O₃ as sintering additives. The phase composition, microstructure and mechanical properties of the composites with different Polycarbosilane content were investigated. The results showed that, dense composites could be prepared at a relatively low temperature of 1800 °C via the liquid-phase-sintering mechanism and the highest mechanical property was obtained for the composites with 20 wt.% PCS and 8 wt.% sintering additives. The amorphous interphase formed during sintering process in the composites not only contributed to the densification of the composites, but also improved the fiber–matrix bonding. The nano-silicon carbide derived from Polycarbosilane, could also play a role of improving the relative density of the composites.     

Effects of oxidation on intergranular phases in silicon nitride ceramics

The effects of oxidation on changes in the secondary phases of two Si₃N₄ ceramics were investigated by transmission electron microscopy. The Si₃N₄ materials were oxidized at 1400 °C for 168 h in laboratory air. One material, sintered with 5 vol% Yb₂O₃+0.5 vol% Al₂O₃, containing a Yb₂Si₂O₇ crystalline secondary phase, displayed no gross changes following oxidation. However, the thickness of the amorphous intergranular film was observed to have decreased by 20% from its initial thickness of 1.0 nm. The second Si₃N₄ material, sintered with 5 wt% Y₂O₃+1 wt% MgO, had a completely amorphous secondary phase. Devitrification of the secondary phase at multiple-grain junctions to -Y₂Si₂O₇ accompanied the outward diffusion of additive and impurity cations occurring in the residual amorphous intergranulàr films during oxidation. Substantial cavitation and intergranular phase depletion was observed at both multiple-grain junctions and two-grain boundaries. The equilibrium thickness of the amorphous intergranular film consequently decreased from 1.2 to 0.9 nm following oxidation. Purification of the amorphous intergranular films by diffusion of cations to the surface led to a reduction in impurity concentration, resulting in the observed thinning of grain-boundary films.     

Characteristics of translucent alumina produced by slip casting method using gypsum mold

Translucent Al₂O₃ ceramics were successfully produced by slip casting using a gypsum mold, provided that CaSO₄ impurities, which had penetrated into the green bodies from the gypsum mold, were removed by the wash of HCl aqueous solution. Some of the calcined Al₂O₃ compacts were washed with HCl aqueous solution before sintering the compacts and the others were not washed with HCl aqueous solution. The relative densities of the sintered Al₂O₃ ceramics with HCl treatment were higher than those of the untreated samples. Grains in the HCl-treated samples, which sintered at 1350°C, grew homogeneously with about 1 m in diameter. When the sintering temperature was higher, the grains grew homogeneously. The sintered Al₂O₃ ceramics with the HCl treatment were translucent. The transmittance value increased from 0 to 12% with increasing wavelength from 300 to 900 nm. The Al₂O₃ ceramics with the HCl treatment did not have the transmittance when the solid contents of slurry were low. The transmittance was influenced by the solid contents of slurry. On the other hand, grains in the HCl-untreated samples, which sintered at 1350°C, grew heterogeneously with the range from 0.2 to 2 m. The Al₂O₃ ceramics did not have the transmittance.     

Effects of sintering aids on the microstructure and mechanical properties of laminated Si3N4/BN ceramics

Laminated Si₃N₄/BN ceramics with two types of sintering aids, MgO–Y₂O₃–Al₂O₃ (MYA) and La₂O₃–Y₂O₃–Al₂O₃ (LYA), were fabricated through roll compaction and hot-pressing. Sintering aids influence evidently the microstructure and mechanical properties of laminated Si₃N₄/BN ceramics. In comparison with La₂O₃–Y₂O₃–Al₂O₃, MgO–Y₂O₃–Al₂O₃ sintering aid is easier to form a glassy phase with lower viscosity and lower eutectic temperature, which is much easier to migrate into BN interlayers. This results in the denser interlayer microstructure and good bending strength of laminated Si₃N₄/BN ceramics at room temperature, but poor work of fracture (WOF) at room temperature, low strength and work of fracture at elevated temperature. In addition, the LYA sintering aid is good for forming elongated and interlocked β-Si₃N₄ grains and beneficial to the mechanical properties of the laminated Si₃N₄/BN ceramics.     

Effect of grain width and aspect ratio on mechanical properties of Si<Subscript>3</Subscript>N<Subscript>4</Subscript> ceramics

Sintering additives Y₂O₃ and Al₂O₃ with different ratios ((Y₂O₃/Al₂O₃) from 1 to 4) were used to sinter Si₃N₄ to high density and to induce microstructural changes suitable for raising mechanical properties of the resultant ceramics. The sintered Si₃N₄ ceramics have bi-modal microstructures with elongated β-Si₃N₄ grains uniformly distributed in a matrix of equiaxed or slightly elongated grains. Pores were found within the grain boundary phase at the junction regions of Si₃N₄ grains. The highest average aspect ratio (length/width of the grains) of ∼4.92 was found for Y₂O₃/Al₂O₃ ratio of 2.33 with fracture toughness and strength values of ∼7 MPam^1/2 and 800 MPa, respectively. The effect of microstructure, specifically grain morphology, on mechanical properties of sintered Si₃N₄ were investigated and found that the aspect ratio of the elongated grains is the most important microstructural feature which controls mechanical properties of these ceramics.     

Cost-effective fabrication of porous α-SiAlON bonded β-SiAlON ceramics

Porous sialon ceramics have been cost-effectively prepared by pressureless sintering from a mixture of elongated SHS β-sialon powders with an α-sialon precursor composition composed of α-Si₃N₄, AlN, Y₂O₃ and Al₂O₃. The obtained porous sialon ceramics exhibited low shrinkage and homogeneous pore size distribution. The results of X-ray diffraction and scanning electron microscopy showed that a uniform microstructure with elongated and intermingled β-SiAlON grains, which were strongly connected by α-SiAlON phase, has been obtained.     

Preparation and properties of mullite-bonded porous SiC ceramics using porous alumina as oxide

Mullite-bonded porous silicon carbide ceramics were prepared by an in situ reaction bonding technique and sintering in air with SiC, porous Al₂O₃, and graphite as starting materials. The pores in the ceramics were formed by burning graphite and by stacking particles of SiC and Al₂O₃. The surface of SiC was oxidized to SiO₂ at high temperature. With a further increase in temperature, SiO₂ reacted with Al₂O₃ to form mullite. The reaction-bonding characteristics, phase composition, open porosity, mechanical strength as well as the microstructure of porous SiC ceramics were investigated.     

CaO-Y2O3添加剂对AlN陶瓷显微结构及性能的影响

研究了掺杂ＣａＯ－Ｙ２Ｏ３热压烧结和常压烧结ＡｌＮ陶瓷的性能和显微结构．结果表明：热压烧结ＡｌＮ陶瓷的第二相为Ｙ３Ａｌ５Ｏ１２，常压烧结ＡｌＮ陶瓷的第二相为Ｙ３Ａｌ５Ｏ１２和Ｃａ３Ｙ２Ｏ６；热压烧结ＡｌＮ的第二相体积百分数和晶格氧含量均低于常压烧结；热压烧结ＡｌＮ陶瓷的微观结构良好，其热导率达到２００Ｗ／ｍ·Ｋ．     

Sintering and dielectric properties of 0.88Al2O3-0.12TiO2 microwave ceramics by glass addition

The microwave characteristics and the microstructures of 0.88Al₂O₃-0.12TiO₂ with various amounts of MgO-CaO-SiO₂-Al₂O₃ (MCAS) glass sintered at different temperatures have been investigated. The sintering temperature can be lowered to 1300 °C by the addition of MCAS glass. The densities, dielectric constants (ε_r) and quality values (Q×f) of the MCAS-added 0.88Al₂O₃-0.12TiO₂ ceramics decrease with the increase of MCAS glass content. The temperature coefficients of the resonant frequency (τ_f) are shifted to more negative values as the MCAS content or the sintering temperatures increase. The change of the crystalline phases of Al₂TiO₅ phase and rutile-TiO₂ phase has profound effects on the microwave dielectric properties of the MCAS-added Al₂O₃-TiO₂ ceramics. As sintered at 1250 °C, 0.88Al₂O₃-0.12TiO₂ ceramics with 2 wt.% MCAS glass addition exists a ε_r value of 8.63, a Q×f value of 9578 and a τ_f value of +5 ppm/°C.     

Sintering and characterization of Bi4Ti3O12 ceramics

Polycrystalline ferroelectric Bi₄Ti₃O₁₂ ceramics have been prepared by the method of reactive liquid phase sintering. The sintering behaviour of the Bi₂O₃-TiO₂ composite was examined by plotting the isothermal densification curves. The results indicate that the starting oxides are involved in the reaction even at temperatures lower than or equal to 800°C, but the reaction advances at a very slow rate. Above solidus, the liquid phase promotes an extended reaction. Saturation observed in two densification curves, at 875 and 1100°C demonstrate that the reaction proceeds by two steps. A completion of the Bi₄Ti₃O₁₂ formation occurs after 60 min of sintering at 1100°C. Optical micrographs of sintered bismuth titanate ceramics show randomly oriented ferroelectric grains separated by a paraelectric intergranular layer. The Bi₄Ti₃O₁₂ crystallites exhibit a platelike morphology, similar in the appearance to mica, as evidenced by scanning electron micrographs. Isothermal annealing (750 to 950°C) does not affect the microstructure and electric properties of sintered bismuth titanate. The considerable value of dielectric permittivity and the appearance of hysteresis have been correlated to the presence of oxygen vacancies within the pseudotetragonal structure of Bi₄Ti₃O₁₂. The oxygen vacancies are preferentially sited in the vicinity of bismuth ions as evidenced by X-ray photoemission data. XPS and AES measurements confirm that the surface concentration of cations comprising the Bi₄Ti₃O₁₂ ceramics does not deviate from the nominal bulk composition.     

A novel spray co-precipitation method to prepare nanocrystalline Y<Subscript>2</Subscript>O<Subscript>3</Subscript> powders for transparent ceramics

A novel spray co-precipitation method was adopted to synthesize well dispersed nanocrystalline Y₂O₃ powders for transparent ceramics. Several analytic techniques such as XRD, SEM, BET and UV–Vis–NIR spectrophotometer were used to determine the properties of coprecipitated powders, and the microstructure and optical properties of as-fabricated ceramics. The influences of the aging time on powders and ceramics were systematically investigated. Precursors were completely reached to yield the Y₂O₃ phase after being calcined at 1250 °C in air. The calcined Y₂O₃ powders exhibited an approximately spherical morphology with narrow size distribution and weak agglomeration, with mean particle size of ~140 nm. The co-precipitated nanopowders with an aging time of 12 h exhibited the best sintering activity due to the low agglomeration, and the in-line transmittance of Y₂O₃ ceramic sintered at 1800 °C for 8 h in vacuum reached to 77.2% at 1064 nm (1 mm thickness).