Pressureless sintered Al2O3–SiC nanocomposites

Al₂O₃ + 5 vol% SiC composite ceramics were prepared via a conventional powder processing route followed by pressureless sintering. Commercially available Al₂O₃ and SiC powders were milled together in an aqueous suspension. The slurry was freeze granulated, and green bodies were obtained by cold isostatic pressing of the granules. Pressureless sintering was carried out in a nitrogen atmosphere at 1750 and 1780 °C. Near full density (>99%) was achieved at 1780 °C. Densification at the lower sintering temperature was promoted by smaller additions of MgO. Vickers hardness and indentation fracture toughness varied around 18 GPa and 2.3 MPa m^1/2 after sintering at 1780 °C. Transmission electron microscopy revealed that the SiC particles were located predominantly to the interior of the matrix grains and well distributed throughout the composite microstructures. The intragranular particles had sizes in the range 50–200 nm while the intergranular particles were larger, typically 200–500 nm in diameter.     

Crystallographic characterization of silicon nitride ceramics sintered with Y2O3–Al2O3 or E2O3–Al2O3 additions

Silicon nitride ceramics were sintered using Y₂O₃–Al₂O₃ or E₂O₃–Al₂O₃ (E₂O₃ denotes a mixed oxide of Y₂O₃ and rare-earth oxides) as sintering additives. The intergranular phases formed after sintering was investigated using high-resolution X-ray diffraction (HRXRD). The use of synchrotron radiation enabled high angular resolution and a high signal to background ratio. Besides the appearance of β-Si₃N₄ phase the intergranular phases Y₃Al₅O₁₂ (YAG) and Y₂SiO₅ were identified in both samples. The refinement of the structural parameters by the Rietveld method indicated similar crystalline structure of β-Si₃N₄ for both systems used as sintering additive. On the other hand, the intergranular phases Y₃Al₅O₁₂ and Y₂SiO₅ shown a decrease of the lattice parameters, when E₂O₃ was used as additive, indicating the formation of solid solutions of E₃Al₅O₁₂ and E₂SiO₅, respectively.     

Crystallization behavior and properties of K2O–CaO–Al2O3–SiO2 glass-ceramics

In order to obtain high-strength anorthite glass-ceramics, K₂O–CaO–Al₂O₃–SiO₂ quaternary glass and relevant glass-ceramics were prepared and investigated. The results show that anorthite along with kalsilite or leucite was precipitated from the parent glass. Kalsilite crystals were formed firstly and then converted into leucite through reacting with SiO₂ in the glass phase. The morphology of the crystals was dependent on the heat-treatment temperature. Column crystals were transformed into fine granular grains when the sintering temperature changed from 900 °C to 1100 °C. The activation energy (E_α) and avrami constant (n) were also calculated as 463.81 KJ/mol and 3.74 respectively, indicating that bulk nucleation and three-dimensional crystal growth were the dominating mechanisms in the temperature range 1000–1100 °C. The maximum value of the flexural strength for the glass-ceramics containing leucite was 248 MPa and the coefficient of thermal expansion (CTE) was in the range 5.69~11.94×10⁻⁶ K⁻¹. The leucite is the main reason for the high CTEs and high flexural strength of glass-ceramics.     

Effect of the addition ZrO2–Al2O3 on nanocrystalline hydroxyapatite bending strength and fracture toughness

Nanocrystalline hydroxyapatite powder has been synthesized from a Ca(NO₃)₂·4H₂O and (NH₄)₂HPO₄ solution by the precipitation method. In the next step we prepared ZrO₂–Al₂O₃ powder. After preparation, the powder was dried at 80 °C and calcined at 1200 °C for 1 h. Various amounts (HAP–15 wt% ZA, HAP–30 wt% ZA) of powder were mixed with the hydroxyapatite by ball milling. The powder mixtures were pressed and sintered at 1000 °C, 1100 °C and 1200 °C for 1 h. In order to study the structural evolution, X-ray diffraction (XRD) was used. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used to estimate the particle size of the powder and observe fracture surfaces. Results show that the bending strength of pressed nanocrystalline HAP was improved significantly by the addition 15 wt% of ZrO₂–Al₂O₃ powders at 1200 °C, but the fracture toughness was not changed, however when 30 wt% of ZA powders were added to nanocrystalline HAP, the bending strength and fracture toughness of the specimens decreased at all sintering temperature.     

Eutectic crystallization in the UO2–Al2O3–HfO2 ceramic phase diagram

In the frame of the Generation IV Sodium Fast Reactor (SFR) safety studies, a core catcher with a sacrificial material could be placed at the bottom of the nuclear reactor. Its role is to dilute the (U, Pu)O₂ molten fuel in case of a hypothetical core meltdown accident. A Al₂O₃–HfO₂ ceramic is a candidate for the sacrificial material. To understand how the molten fuel would mix with this sacrificial material, the UO₂–Al₂O₃–HfO₂ system was investigated at CEA Cadarache PLINIUS corium platform. The eutectic position of the UO₂–Al₂O₃–HfO₂ was determined: the eutectic temperature is 1728±22 °C (2001±22 K) and the eutectic composition is 30 wt% UO₂–35 wt% Al₂O₃–35 wt% HfO₂. Then, the pseudo-binary UO₂–(50 wt% Al₂O₃–50 wt% HfO₂) phase diagram has been proposed.     

Influence of Al2O3 whisker concentration on flexural strength of Al2O3(w)–ZrO2 (TZ-3Y) composite

On investigating the possibility of using alumina whisker reinforced 3 mol% Yttria stabilized Tetragonal Zirconia (TZ-3Y) composite for bioceramic applications, presented here is the influence of varying whisker concentration (2, 5, 10, 15 and 20 wt%) on flexural strength of the composite. Whiskers of hydrothermally synthesized Ammonium Aluminum Carbonate Hydroxide (AACH) were used for composite synthesis. These whiskers transformed in situ into alumina during sintering. It was found that with addition of alumina whiskers, strength was increased and reached a maximum value of 1212±60 MPa and 1325±65 MPa, in pure and 1 wt% CTAB added samples respectively, at a concentration of 10 wt% Al₂O₃ whiskers. The strength values of the synthesized composite can compete well with commercially available materials for dental applications.     

The reaction between the magnesia–chrome brick and the molten slag of MgO–Al2O3–SiO2–CaO–FetO and the resulting microstructure

The reaction and microstructure at the interface of MgO–Cr₂O₃ brick and the molten slag of MgO–Al₂O₃–SiO₂–CaO–Fe_tO after static slag corrosion at 1823–1923 K for various times and the resulting microstructure were investigated and characterized. After the static slag corrosion at 1923 K for 4 h, the XRD results show the major phases of periclase MgO, MgCr₂O₄ spinel, and CaMgSiO₄ as the minor phase. MgCr₂O₄ phase causes MgO to form a discontinuous phase in MgO–Cr₂O₄ brick. After static slag corrosion at 1923 K for 4 h, SEM micrographs show that brick interior cracks, MgO and dissolved MgO. MgO dissolved due to the molten plag penetrated into the brick interior and reaction with it, leading to a localized dissolution of brick slag. TEM micrographs and ED patterns demonstrate that the minor phase of (Mg, Fe)(Al, Cr)₂O₄ precipitates in the MgCr₂O₄ matrix.     

Bi2O3对K2O–B2O3–SrO–Al2O3–Nb2O5–SiO2玻璃陶瓷介电储能性能的影响

随着电力电子系统的不断发展,高功率脉冲电容器的需求增多。电介质电容器因具有放电功率大、充放电速度快及性能稳定等优点,在电力系统、电子器件、脉冲电源等方面发挥着重要作用,广泛应用于民用领域及军事领域。通过熔融压延制备玻璃基体,采用可控结晶工艺研究了不同含量的Bi₂O₃ (x=0.0%、1.0%、2.0%、4.0%,摩尔分数)对K₂O–B₂O₃–Sr O–Al₂O₃–Nb₂O₅–SiO₂玻璃陶瓷物相演化、微观结构、介电和储能性能的影响。在该玻璃陶瓷中,KSr₂Nb₅O₁₅为主要析出晶相,当Bi₂O₃的加入量为x=2.0%(摩尔分数)时,热处理温度为950℃时,玻璃陶瓷样品的储能密度最大可达到1.27 J/cm³,室温下介电常数可达342,是热处...     

Effect of different nucleation catalysts on the crystallization of Li2O–ZnO–MgO–Al2O3–SiO2 glasses

Based on local raw materials, a range of LiZnMg aluminosilicate glasses were prepared to investigate the influence of TiO₂, Cr₂O_3, and ZrO₂ on the crystallization behaviour and thermal expansion characteristics. Differential thermal analysis showed that the crystallization propensity increases in the order TiO₂ > Cr₂O₃ > ZrO₂. Virgilite, β-spodumene ss, gahnite, enstatite and cristobalite were formed in the prepared glass-ceramics. The microstructure of glass-ceramic samples showed growths of rounded and subrounded grains in the base sample, whereas, somewhat rod-like and accumulated growths appeared in samples containing ZrO₂. However, a rather homogeneous texture of accumulated growths was developed in glass-ceramics containing TiO₂ and Cr₂O₃. The coefficient of thermal expansion of parent glasses was sensitive to the type of nucleating agent added (Cr₂O₃ > TiO₂ > ZrO₂) varying from 24.8 × 10⁻⁷ to 65.1 × 10⁻⁷ °C⁻¹ being almost unchanged with the heat-treatment. The microhardness values of glass-ceramic samples were in the 763–779 kg/mm² range.     

Study of AC electrical properties of V2O5–P2O5–B2O3–Dy2O3 glasses

The AC conductivity of glass samples of composition 60V₂O₅–5P₂O₅–(35−x)B₂O₃–xDy₂O₃, 0.4≤x≤1.2 has been analyzed. The samples were prepared by the usual melt-quench technique. The prepared compounds were analyzed by X-ray diffraction (XRD) and thermo gravimetric–differential thermal analysis (TG/DTA). The activation energies were evaluated using glass transition temperature (T_g) and peak temperature of crystallization (T_c) from TG/DTA. The dependence of activation energy on composition was discussed. The electrical conductance and capacitance were measured over a frequency range of 20 Hz to 1 MHz and a temperature range of 303–473 K; these reveal semiconducting features based predominantly on an ionic mechanism. The dielectric and complex-impedance response of the sample is discussed. The relaxation time was found to increase with increasing temperature. Jonscher's universal power law is applied to discuss the conductivity. The electrode polarization was found to be negligible and confirmed from electrical modulus.     

Low-temperature preparation and microwave dielectric properties of ZBS glass–Al2O3 composites

The preparation and microwave dielectric properties of ZnAl₂O₄-based glass–ceramic composites were investigated. Using zinc borosilicate (ZBS) glass and Al₂O₃, glass–ZnAl₂O₄ composites with high quality factor was successfully prepared at temperatures below 950 °C. The linear shrinkage for 50 vol% ZBS glass–ZnAl₂O₄ composite showed a steep increase up to 650 °C and a plateau between 700 °C and 950 °C, implying that one-stage densification process occurred. The crystallization of ZnAl₂O₄ was observed above 700 °C and an insufficient densification occurred due to the consumption of the glass. As the sintering temperature increased, the quality factor (Q × f₀) showed an increase with an S-type curve whereas the dielectric constant was almost constant. The formation of ZnAl₂O₄ might correspond to the increase of Q × f₀; a high value of 17,757 GHz (1415 at 12.6 GHz) was obtained for the specimen sintered at 900 °C.     

Microstructure and mechanical properties of fine grained carbon-bonded Al2O3–C materials

Fine grained carbon-bonded Al₂O₃–C materials as used in ceramic filters have been manufactured by uniaxial and isostatic pressing, respectively. The variation in the microstructure over the cross section of the samples which in particular depends on the shaping technique plays an important role in the wetting of the material by liquid steel. Moreover, the amount and grain size of the binder has a decisive influence on the porosity and bulk density and therefore on the mechanical properties. For this, two different grain size distributions of Carbores^® P binder were used, and in addition the fraction of binder was varied from 5–30 wt%. Tests of the cold crushing strength and of the cold modulus of rupture were performed at room temperature. The adjusted bulk density, open porosity and shrinkage of the samples were determined and the microstructure was analyzed by means of scanning electron microscopy. For control of a homogeneous distribution of carbon in the samples, the residual carbon content was measured also within individual samples at different positions.     

Investigation of the effect of ZrO2 and ZrO2/Al2O3 additions on the hot-pressing and properties of equimolecular mixtures of α- and β-Si3N4

In this work, hot-pressing of equimolecular mixtures of α- and β-Si₃N₄ was performed with addition of different amounts of sintering additives selected in the ZrO₂–Al₂O₃ system. Phase composition and microstructure of the hot-pressed samples was investigated. Densification behavior, mechanical and thermal properties were studied and explained based on the microstructure and phase composition. The optimum mixture from the ZrO₂–Al₂O₃ system for hot-pressing of silicon nitride to give high density materials was determined. Near fully dense silicon nitride materials were obtained only with the additions of zirconia and alumina. The liquid phase formed in the zirconia and alumina mixtures is important for effective hot-pressing. Based on these results, we conclude that pure zirconia is not an effective sintering additive. Selected mechanical and thermal properties of these materials are also presented. Hot-pressed Si₃N₄ ceramics, using mixtures from of ZrO₂/Al₂O₃ as additives, gave fracture toughness, K_IC, in the range of 3.7–6.2 MPa m^1/2 and Vicker hardness values in the range of 6–12 GPa. These properties compare well with currently available high performance silicon nitride ceramics. We also report on interesting thermal expansion behavior of these materials including negative thermal expansion coefficients for a few compositions.     

Catalytic removal of NO in waste incineration processes over Rh/Al2O3 and Rh–Na/Al2O3: Effects of particulates,heavy metals,SO2 and HCl

Two novel catalysts Rh/Al₂O₃ and Rh–Na/Al₂O₃ were prepared for NO removal and tested their practical performances in a laboratory-scale waste incineration system. The effects of particulates, heavy metals, and acid gases on the catalysts were evaluated and investigated through several characterization techniques, such as SEM, EA, XRPD, ESCA, and FTIR. The results indicated that the NO conversions were increased with the accumulation of particulates on the surface of catalysts, which was attributed to the increase in carbon content. However, the increase in heavy metals Cd and Pb contents on the surface of catalysts decreased the activity of catalyst for NO removal but did not change the chemical state of Rh and Na. The Rh/Al₂O₃ catalysts were poisoned when the acid gases SO₂ and HCl were present in the flue gas, because Rh and Al reacted with S and Cl to form inactive products. Adding Na to Rh/Al₂O₃ catalysts produced a promoting effect for SO₂ removal due to the formation of Na₂SO₄. The influence levels of different pollutants on the performances of Rh/Al₂O₃ and Rh–Na/Al₂O₃ catalysts for NO removal followed the sequence of HCl > heavy metals > SO₂ > particles.     

Influences of La and Er on structure and properties of Bi2O3–B2O3 glass

Bi₂O₃·2B₂O₃ glasses doped with La₂O₃ and Er₂O₃ were prepared by the melting-quenching method with AR-grade oxides. IR analysis was used to investigate the glass network structure. The characteristic temperatures including the glass transition temperature (T_g), crystallization temperature (T_p), and melting temperature (T_m) were estimated by DSC. The coefficient of thermal expansion (α), mass density (D), and Vickers hardness (H_v) were also measured. The results show that the basic network structure of Bi₂O₃·2B₂O₃ glasses doped with rare-earth oxides consists of chains composed of [BO₃], [BO₄], and [BiO₆] units. La₂O₃ and Er₂O₃ act as network modifiers. As the doping concentrations of the rare-earth oxides were increased, T_g increased and α decreased, indicating that a more rigid glass was obtained. Er₂O₃ reduces the melting temperature and prevents glass crystallization. La₂O₃ contributes to the improvement of the microhardness of Bi₂O₃·2B₂O₃ glass.     

Al2O3-3Al2O3·2SiO2-ZrO2耐火材料的相组成

Al2O3-SiO2-ZrO2系耐火材料应用范围广,特别被用作陶瓷辊,具有力学强度高、抗热震性能优良、耐碱类化合物侵蚀和高温蠕变率低的特性。Al2O3-SiO2-ZrO2系耐火材料性能很大程度上取决于其结晶相和玻璃相的总量和化学成分,采用定量XRPD和XRF研究了原料中Al2O3/SiO2比和氧化铝颗粒尺寸分布对结晶相和玻璃相的总量及其化学成分的影响。耐火材料由莫来石、刚玉、ZrO2的多晶体和总量各异的玻璃相组成。莫来石含量及其晶胞参数和成分随烧成温度改变,但主要受原料中Al2O3/SiO2比的影响。     

Effect of ceramic bonding phases on the thermo-mechanical properties of Al2O3–C refractories

Ceramic bonding phases of non-oxide whiskers can enhance the hot strength and the thermal shock resistance of Al₂O₃–C refractories. In this paper, the effect of different metals on the microstructure and thermo-mechanical properties of Al₂O₃–C refractories has been investigated. Thermodynamic calculation of Al–Si–O–C–N systems shows that Al₄C₃, AlN, SiC and β-Sialon are stable at elevated temperature. AlN with the shape of short column can be generated in Al₂O₃–C refractories with metallic Al, which leads to high hot modulus of rupture (HMOR) and poor resistance to thermal shock. SiC whiskers formed in Al₂O₃–C refractories with metallic Si give rise to low HMOR and good resistance to thermal shock. When metallic Si and Al are added together in the refractories, β-Sialon (z=2) with plane structure can be generated under the action of catalyst (nano-sized Ni). The existence of the catalyst promotes the diffusion of Al and O in Si₃N₄ crystals and contributes to the generation of plane-shaped β-Sialon. The corresponding HMOR and residual cold modulus of rupture respectively increase to about 20 MPa and 10.3 MPa. The plane-shaped β-Sialon can significantly enhance both hot strength and thermal shock resistance of Al₂O₃–C refractories.     

多组元BaO–SrO–CaO–MgO–Al2O3–2SiO2环境障涂层的制备与抗CaO–MgO–Al2O3–SiO2腐蚀性能

采用固相法制备不同摩尔 Ba、Sr、Ca、Mg 配比的 Ba O–Sr O–Ca O–Mg O–Al₂O₃–SiO₂ （BSCMAS）陶瓷材料,研究多组元陶瓷的制备工艺、显微结构及其抗 CMAS 腐蚀性能。结果表明：通过调控 MgO 的含量,在 1 400 ℃条件下制备了Ba_0.3Sr_0.3Ca_0.35Mg_0.05Al₂Si₂O₈ (B_0.3S_0.3C_0.35M_0.05AS)单相多组元陶瓷材料。在 1 250、1 300 ℃和 1 350 ℃对 B_0.3S_0.3C_0.35M_0.05AS 进行 CMAS 腐蚀实验,相比于 Ba_0.5Sr_0.5Al     

Microwave dielectric characteristics of Nb2O5-added 0.9Al2O3–0.1TiO2 ceramics

The sintering characteristics, phase composition, and microwave dielectric properties of Nb₂O₅-added 0.9Al₂O₃–0.1TiO₂ ceramics sintered at 1300–1500 °C have been investigated. Results show that Nb⁵⁺ and Al³⁺ can co-substitute for Ti⁴⁺ and form Ti_0.8Al_0.1Nb_0.1O₂, which can lower effectively the sintering temperature, and improve the quality factor of 0.9Al₂O₃–0.1TiO₂ ceramics.