Effects of binary additives B2O3–Y2O3 on the microstructure and thermal conductivity of aluminum nitride ceramics

Aluminum nitride (AIN) ceramics, with binary additives B₂O₃-Y₂O₃, were sintered at temperatures from 1700 to 1850 °C. The microstructure and sintering characteristics were studied by XRD, HREM, SEM and TEM/EDS, which showed that Y₂O₃ gave different yttrium aluminates through the reaction with Al₂O₃ under different conditions. With the increase of sintering temperature, the yttrium-to-aluminum atomic ratio Y/Al decreased in the secondary phases of the sintered bodies. It was discovered that B₂O₃ could dissolve in the yttrium aluminates, forming some ordered structure with a superlattice. After sintering at 1850 °C for 4 h, a specimen with a fine microstructure and a thermal conductivity of 190 Wm^–1K^–1 was obtained.     

Microstructure and mechanical properties of B6O-B4C sintered composites prepared under high pressure

Sintered composites in the B₆O-xB₄C (x = 0–40 vol%) system were prepared under high pressure and high temperature conditions (3–5 GPa, 1500–1800°C) from the mixture of in-laboratory synthesized B₆O powder and commercially available B₄C powder. Relationship among the formed phases, microstructures and mechanical properties of the sintered composites was investigated as a function of sintering conditions and added B₄C content. Microhardness of the sintered composite was found to increase with treatment temperature up to 1800°C, while fracture toughness decreased slightly. Maximum microhardness of Hv 46 GPa was obtained from B₆O-30vol%B₄C sintered composite under the sintering conditions of 4 GPa, 1700°C and 20 min.     

Sintered iron-ceramic composites

In order to improve the strength and high-temperature properties of sintered iron, iron-ceramic composites have been studied. In the present investigation, iron powder with 0–8 vol % Al₂O₃ or SiC particles of different sizes were selected for the study. Powders were mixed, compacted and subsequently sintered at 1150°C under an endo gas atmosphere. Various properties of the sintered compacts, such as density and mechanical properties, were evaluated. Fractography, microstructural studies including EDAX, X-Ray image analysis were studied for selected specimens. It was established from the results that 4 vol % Al₂O₃ or SiC are optimum to obtain superior properties of the composites.     

Sintering behaviour of slip-cast Al2O3 – Y-TZP composites

The sintering behaviour of alumina–Y-TZP composites prepared by slip-casting technique were studied. Slip-cast samples containing varying amounts of Y-TZP ranging up to 90 vol% were prepared and evaluated. Sintering studies were carried out at 1450°C to 1600°C. Sintered samples were characterised where appropriate to determine phases present, grain sizes, bulk density and mechanical properties. Good correlation was obtained between the calculated prepared powder density and experimental results. The sintered bulk density of the composites was observed to increase with increasing Y-TZP content and sintering temperature up to 1550°C. Maximum hardness values (>14 GPa) were obtained for all samples containing <60 vol% Y-TZP and when sintered at 1550°C. It has been found that the additions of up to 50 vol% Y-TZP was effective in suppressing Al₂O₃ grain growth.     

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.     

Pressureless sintering and related reaction phenomena of Al2O3-doped B4C

The effects of alumina on the densification of boron carbide and related reaction phenomena in alumina-doped B₄C were studied. Pressureless sintering was conducted at various temperatures for 15 min in a flowing Ar atmosphere. The addition of alumina improved the densification of boron carbide. Maximum density of 96% theoretical was obtained with the 3 wt % alumina-doped B₄C sintered at 2150°C. Abnormal (or exaggerated) grain growth was observed in the specimen containing more than 4 wt % alumina. In the B₄C-Al₂O₃ reaction couples, good wetting of the liquid phase on the boron carbide grains was observed. X-ray diffraction and Auger electron spectra showed that the AlB₁₂C₂ phase was formed by the reaction between boron carbide and alumina. It is suggested that these phenomena promote the densification of boron carbide.     

Densification behaviour and mechanical properties of pressureless-sintered B4C–CrB2 ceramics

B₄C based ceramics composites with 0–25 mol% CrB₂ were fabricated by pressureless sintering in the temperature range 1850°C to 2030°C. The CrB₂ addition enhanced the densification of B₄C due to the CrB₂–B₄C eutectic liquid phase formation. Both a high strength of 525 MPa and a modest fracture toughness of 3.7 MPa m^1/2 were obtained for the B₄C–20 mol% CrB₂ composite with a high-relative density of 98.1% after sintering at 2030°C. The improvement in fracture toughness is thought to result from the formation of microcracks and the deflection of propagating cracks resulting from the thermal expansion mismatch of CrB₂ and B₄C.     

Microstructure of cBN-diamond sintered compact prepared by reaction sintering

cBN-diamond composite sintered compacts (diamond content 15–70 wt %) were prepared by reaction sintering at 7–7.5 GPa and 1400–1700 °C for 10–30 min from the starting powder of the hBN-diamond system in the presence of 1 wt % NH₄NO₃ as a volatile catalyst. A fully dense sintered compact with 99% conversion from hBN to cBN was obtained at 7 GPa and 1700 °C after 30 min. An induced transformation from hBN to cBN seemed to occur on the surface of the added diamond seed crystals. Diamond seed crystals (about 30 wt %, grain size 0.2–1.5 m) were found to be well-dispersed in the reaction-bonded cBN matrix. The Vickers microhardness of the sintered compact was 5100 kg mm^–2. The contacts between diamond grains were observed in the sintered compacts containing diamond seed grains of more than 70 wt %. The toughness of the sintered compact tended to increase with decreasing diamond content and the grain size of seed crystals.     

Fabrication and mechanical properties of silicon carbide–silicon nitride nanocomposites

A powder mixture of ultrafine –SiC–35 wt% –Si₃N₄ containing 6 wt% Al₂O₃ and 4 wt% Y₂O₃ as sintering additives were liquid–phase sintered at 1800°C for 30 min by hot–pressing. The hot–pressed composites were subsequently annealed at 1920°C under nitrogen–gas–pressure to enhance grain growth. The average grain–size of the sintered bodies were ranged from 96 to 251 nm for SiC and from 202 to 407 nm for Si₃N₄, which were much finer than those of ordinary sintered SiC–Si₃N₄ composites. Both strength and fracture toughness of fine–grained SiC–Si₃N₄ composites increased with increasing grain size. Such results suggested that a small amount of grain growth in the fine–grained region (250 nm for SiC and 400 nm for Si₃N₄) was beneficial for mechanical properties of the composites. The room–temperature flexural strength and fracture toughness of the 8–h annealed composites were 698 MPa and 4.7 MPa · m^1/2, respectively.     

Spark plasma sintered tantalum carbide: Effect of pressure and nano-boron carbide addition on microstructure and mechanical properties

TaC and TaC-1 wt.% B₄C powders were consolidated using spark plasma sintering (SPS) at 1850 °C and varying pressure of 100, 255 and 363 MPa. The effect of pressure on the densification and grain size is evaluated. The role of nano-sized B₄C as sintering aid and grain growth inhibitor is studied by means of XRD, SEM and high resolution TEM. Fully dense TaC samples were produced at a pressure of 255 MPa and higher at 1850 °C. The increasing pressure also resulted in an increase in TaC grain size. Addition of B₄C leads to an increase in the density of 100 MPa sample from 89% to 97%. B₄C nano-powder resists grain growth even at high pressure of 363 MPa. The formation of TaB₂/Carbon at TaC grain boundaries helps in pinning the grain boundary and inhibiting grain growth. The effect of B₄C addition on hardness and elastic modulus measured by nanoindentation and the indentation fracture toughness has been studied. Relative fracture toughness increased by up to 93% on B₄C addition.     

Microstructure and properties of the sintered composite prepared by hot pressing of TiN-coated alumina powder

Alumina powders (average grain size: 50 m) coated with TiN film of thickness 0.5 and 1.2 m were prepared by rotary powder-bed chemical vapour deposition for 15 and 90 min, respectively. These Al₂O₃-TiN composite powders were hot-pressed at 1800 °C and 40 MPa for 30 min. The microstructure of the Al₂O₃-TiN sintered composite was composed of a TiN network homogeneously distributed on the grain boundaries of alumina. The mechanical properties (hardness, bending strength and fractured toughness) and thermal conductivity of the sintered composite were found to depend on the composition and microstructure of the sintered composite, even with a small content (3–7 wt%) of TiN. The resistivity of the sintered composite was 10^–1-10^–3 cm. The relatively high electrical conductivity of the Al₂O₃-TiN composite was caused by the grain boundary conduction of TiN.     

High pressure consolidation of B6O-diamond mixtures

Sintered composites in the B₆O-xdiamond (x= 0–80 vol%) system were prepared under high pressure and high temperature conditions (3–5 GPa, 1400–1800°C) from the mixture of in-laboratory synthesized B₆O powder and commercially available diamond powder with various grain sizes (<0.25, 0.5–3, and 5–10 m). Relationship among the formed phases, microstructures, and mechanical properties of the sintered composites was investigated as a function of sintering conditions, added diamond content, and grain size of diamond. Sintered composites were obtained as the B₆O-diamond mixed phases when using diamond with grain sizes greater than 0.5 m, while the partial formation of the diamond-like carbon was observed when using diamond grain sizes less than 0.25 m. Microhardness of the sintered composite was found to increase with treatment temperature and pressure, and the fracture toughness slightly decreased. A maximum microhardness of H _v57 GPa was measured in the B₆O-60 vol% diamond (grain size < 0.25 m) sintered composite under the sintering conditions of 5 GPa, 1700°C and 20 min.     

Transparent Lu2O3:Eu ceramics by sinter and HIP optimization

Evolution of porosity and microstructure was observed during densification of lutetium oxide ceramics doped with europium (Lu₂O₃:Eu) fabricated via vacuum sintering and hot isostatic pressing (HIP’ing). Nano-scale starting powder was uniaxially pressed and sintered under high vacuum at temperatures between 1575 and 1850 °C to obtain densities ranging between 94% and 99%, respectively. Sintered compacts were then subjected to 200 MPa argon gas at 1850 °C to reach full density. Vacuum sintering above 1650 °C led to rapid grain growth prior to densification, rendering the pores immobile. Sintering between 1600 and 1650 °C resulted in closed porosity yet a fine grain size to allow the pores to remain mobile during the subsequent HIP’ing step, resulting in a fully-dense highly transparent ceramic without the need for subsequent air anneal. Light yield performance was measured and Lu₂O₃:Eu showed ∼4 times higher light yield than commercially used scintillating glass indicating that this material has the potential to improve the performance of high energy radiography devices.     

Abnormal grain growth in alumina-doped hafnia ceramics

Hafnia (HfO₂) ceramics containing 0.0, 5.0, and 10.0 vol% Al₂O₃, respectively, were sintered at 1600°C for various periods from 2–24 h. Abnormal grain growth was found to occur in the Al₂O₃-containing compositions. Hafnia containing 5.0 vol% Al₂O₃ exhibits an average grain size of almost double that of the Al₂O₃-free hafnia matrix, coupled with a much wider grain-size distribution. The material containing 10.0 vol% Al₂O₃ shows a smaller average grain size than the composition containing 5.0 vol% Al₂O₃. However, its average grain size is still larger than that of the Al₂O₃-free hafnia on sintering at 1600°C for more than 8 h. Microstructural characterization, carried out using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) equipped with an energy dispersive analysis facility (EDX), indicated that there existed a continuous segregant layer at the grain boundaries and grain junctions in the Al₂O₃-free hafnia. Hafnia exhibits a low solubility in the segregant layer phase which inhibits the growth of the hafnia grains. The Al₂O₃ particles act as a scavenger for the silicon-rich glassy phase, damaging the continuous nature of the boundary segregant layer and promoting grain growth in the Al₂O₃-doped hafnia ceramics. The microstructural development at the sintering temperature is an overall result of the concurrent scavenger effect and grain pinning by the Al₂O₃ particles.     

Effect of sintering process on the microstructures of Bi2O3-doped yttria stabilized zirconia

Variations of microstructures in Bi₂O₃-doped yttria stabilized zirconia (YSZ) with conventional furnace and microwave sintering were investigated in this work. The results demonstrated that a small amount of addition of Bi₂O₃ was effective in reducing the sintering temperature of YSZ from 1500 °C to 1200 °C and promoting the densification rate of the ceramics. It is interesting that microwave sintering is found to suppress the evaporation rate of Bi₂O₃ and formation of the monoclinic-ZrO₂ or other amorphous phases. Compared to conventional furnace sintering, significant improvement in density of Bi₂O₃-doped YSZ at lower sintering temperatures with microwave sintering was observed. Rapid heating rate and short sintering time for restricting serious segregation at grain boundary were observed as well. Employing microwave sintering at the same sintered condition, the density of a specimen was evidently increased by 4.59% in comparison to the specimen sintered with a conventional furnace sintering.     

Sintering characteristics and crystallization for sol–gel-derived powders for low-dielectric and low-temperature sintering ceramics

Samples in the MgO–Al₂O₃–SiO₂ system were prepared by the sol–gel technique. The coalescence, sintering characteristics, and crystallization were investigated by X-ray diffraction, thermal analysis, and scanning electron microscopy. The dielectric properties and density were measured with an impedance analyzer. Results demonstrated that the obtained cordierite powders synthesized with the sol–gel method distribute uniformly and its effective size is 474 nm. The glass powder could be sintered at 950 °C, and the polymorphic modification cordierite detected in the sintered sample was only stable hexagonal -phase. The sintering densification process was performed mainly in the temperature range from 800 °C to 930 °C, and follows the viscous floating principle. The dielectric constant of the sintered body is 4.2 and its dielectric loss is lower than 0.001 at high frequency (1.5 GHz).     

Effect of sintering temperature on the microstructure and high-frequency magnetic properties of Ni0.467Zn0.07Co0.015Fe0.511O4 ferrite

In this work, an attempt is made to study the effects of sintering temperature on the microstructure and high-frequency (HF) magnetic properties of a nickel zinc ferrite compound of very low ZnO content of Ni_0.467Zn_0.07Co_0.015Fe_0.511O₄ composition. Samples were prepared by a conventional ceramic route and sintered for 2 h at 1150, 1200, 1250, and 1300 °C. It was shown that the higher the sintering temperature the higher the saturation magnetization and the measured initial permeabilities, and the lower was the H _c of the samples. This was related to the increased sintered densities and grain sizes. The magnitudes of the electrical resistivity of the samples sintered at 1300 °C compared to those of the samples sintered at 1150 °C and 1200 °C showed four orders decrease. This is thought to be due to the grain-size increase and possibly the formation of higher Fe²⁺/Fe³⁺ concentration. The lowest measured quality factor (Q-factor) obtained in the range of 60–210 MHz, corresponds to the samples sintered at 1300 °C. The highest Q-value in the frequency range of 125–210 MHz was obtained for the samples sintered at 1150 °C, which has also shown the highest electrical resistivity.     

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.     

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.     

Sintering temperature, microstructure and resistivity of polycrystalline Sm0.2Ce0.8O1.9 as SOFC's electrolyte

In this work, near-completely soft-agglomerated Sm_0.2Ce_0.8O_1.9 powders have been prepared. The pellets were formed and sintered at various sintering conditions of temperature and time. It was found that the sintering conditions have significant effects on the pellet resistivity. By the measurements with the DC four-probe method, it was found that the overall resistivity of the polycrystalline Sm_0.2Ce_0.8O_1.9 material sintered at 1500°C increases linearly with the reciprocal of the average grain size. The AC impedance spectroscopy has been used to distinguish the grain resistivity and the apparent grain boundary resistivity. The brick layer microstructural model has been used to provide an estimate of the apparent grain boundary resistivity and to relate the electrical properties to the microstructural parameters. By lowering the sintering temperature to 1100–1200°C, the true grain boundary resistivity was nearly two orders lower than that sintered at 1500°C, and thus the overall resistivity decreases to about 31 ohm-cm at 700°C measurement. This makes the Sm_0.2Ce_0.8O_1.9 material capable of working as SOFC's electrolyte at temperatures lower than 700°C.