Preparation and characterisation of self-flowing refractory material containing 971U type microsilica

Abstract

A newer composition of self-flowing low cement brown fused alumina castable containing 971U type microsilica was developed. Optimum flow characteristics were achieved using water addition of 4·6?wt-%. This batch was sintered at different firing temperatures up to 1500°C. To understand the effect of both firing temperatures and corresponding phases, the present castable was characterised in terms of X-ray diffraction, scanning electron microscopy, bulk density (BD), apparent porosity (AP), water absorption (WA), cold crushing strength (CCS) and self-leveling flowability. The results revealed that gradual increase in firing temperature from 1100 through 1500°C caused low AP and WA, and high CCS properties due to the densification of the castable.     

Nanocrystalline growth activation energy of alumina polymorphs synthesised by mechanochemical technique

Abstract

Al₂O₃ nanopowders were synthesised via mechanochemical method using AlCl₃ and CaO as raw materials. The effect of thermal treatment on the structural evolutions and morphological characteristics of the nanopowders was investigated using X-ray diffractometry, transmission electron microscopy, scanning electron microscopy, differential thermal analysis and Rietveld refinement. The results showed that the average crystallite size of Al₂O₃ was <100 nm up to ～1200°C. The activation energy for Al₂O₃ nanocrystallite growth during calcinations was calculated to be ～22?598 and 30?195 J mol^?1 for η- and κ-alumina respectively, while for α-Al₂O₃, it was 8373 and 34?131 J mol^?1 at temperatures up to 1200°C and >1200°C respectively. The mechanism of nanocrystalline growth of Al₂O₃ polymorphs during annealing is also discussed.     

牙科用氧化锆/氧化铝/玻璃复合材料的研制

采用熔融渗入法制备了牙科用氧化铝基玻璃复合材料，为了提高材料的强度和韧性，在氧化铝预制体中加入一定量的氧化锆。借助sEM和XRD对材料的微观结构和晶相组成进行了研究。研究结果表明：4Y—TZP的引入量为15wt％，掣合材料的抗折强度可达到182MPa，氧化铝基体经玻璃渗透以后，抗折强度等性能明显改善，而且材料化学性能稳定，色泽逼真，是一种较理想的牙科用材料。     

Long-term evaluation of NiMo/alumina–carbon black composite catalysts in hydroconversion of Mexican 538 °C+ vacuum residue

Alumina with (8–18 wt.%) carbon black composite (AMAC) supports was prepared as bimodal extrudates, containing 11–20% of total pore volume as macropores (i.e. >1000 Å). These supports, in spite of containing carbon black and macropores, showed good side crushing strength (0.67–1.19 kg/mm) after pyrolysis in 6% O₂/N₂. AMAC-catalysts were obtained after impregnating these alumina–carbon black supports with Ni and Mo, to obtain 3.5 wt.% NiO and 15 wt.% MoO₃. These catalysts were evaluated for about 700 h in the hydroconversion of a Mexican vacuum residue (538 °C+) at 415 °C, 200 kg/cm², H₂/HC = 6000 ft³/barrel in a pilot plant equipped with a Robinson–Mahoney reactor. In comparison with a commercial bimodal alumina-based catalyst (ComCat), AMAC catalysts showed much fewer sediments and less Conradson carbon formation. Initial HDS in AMAC containing macropores can be as high as 92%, while that in a ComCat is 86%. On average, yields of naphtha and kerosene were 2.6 and 1.34 times higher with AMAC catalysts than those with ComCat, while diesel yields were similar.     

Fabrication of Fe-, Ni- and FeNi-coated Al2O3 core-shell microspheres by heterogeneous precipitation

The precursors with NiCO₃·2Ni(OH)₂·2H₂O-, Fe₂O₃·nH₂O-, or both of NiCO₃·2Ni(OH)₂·2H₂O- and Fe₂O₃·nH₂O-coated alumina microspheres were prepared, respectively, by the aqueous heterogeneous precipitation using metal salts, ammonium hydro-carbonate and -Al₂O₃ micropowders as the starting materials. Subsequently, magnetic metallic Ni-, -Fe- and γ-FeNi-coated alumina core-shell structural microspheres were successfully obtained by thermal reduction of the as-prepared precursors at 700 °C for 2 h, respectively. Optimized precipitation processing parameters of the concentration of alumina micropowders (15 g/L), the rate of adding reactants (5 mL/min) and pH value were determined by a trial and error method. Powders of the precursors and the resultant metal (Ni, -Fe, γ-FeNi alloy)-coated alumina micropowders were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The experimental results show that it is possible to adjust metal coating thicknesses and fabricate multilayer structured metal/ceramics core-shell microspherical powder materials and these materials may be applied for high performance of functional materials and devices.     

Damage tolerance in additively manufactured ceramic architected materials

Technical ceramics exhibit exceptional high-temperature properties, but unfortunately their extreme crack sensitivity and high melting point make it challenging to manufacture geometrically complex structures with sufficient strength and toughness. Emerging additive manufacturing technologies enable the fabrication of large-scale complex-shape artifacts with architected internal topology; when such topology can be arranged at the microscale, the defect population can be controlled, thus improving the strength of the material. Here, ceramic micro-architected materials are fabricated using direct ink writing (DIW) of an alumina nanoparticle-loaded ink, followed by sintering. After characterizing the rheology of the ink and extracting optimal processing parameters, the microstructure of the sintered structures is investigated to assess composition, density, grain size and defect population. Mechanical experiments reveal that woodpile architected materials with relative densities of 0.38–0.73 exhibit higher strength and damage tolerance than fully dense ceramics printed under identical conditions, an intriguing feature that can be attributed to topological toughening.     

Novel silica-modified boehmite aerogels and fiber-reinforced insulation composites with ultra-high thermal stability and low thermal conductivity

Alumina–silica composite aerogels have drawn vast attention due to their enhanced thermal stability compared to pristine alumina aerogels. However, they are generally weakly-crystallized and tend to experience inevitable sintering and significant surface area loss especially above 1200 °C. In this study, we developed a hydrothermal treatment and supercritical drying strategy for synthesizing novel, well-crystallized, silica-modified boehmite aerogels and fiber-reinforced composites. For the prepared aerogel, network coarsening was significantly hindered and the α-Al₂O₃ transition was completely prevented even at 1400 °C. As a result, the aerogel exhibits extremely high surface area maintenance (87 % and 53 % after 1300 °C and 1400 °C calcination, respectively) and low linear shrinkage (14 % after 1300 °C calcination) at elevated temperatures. The composite with good toughness shows excellent heat resistance and thermal insulating performance up to 1500 °C. These findings provide a general, direct new idea to improve the thermal tolerance of alumina-based aerogels and extend their applications to higher temperatures.     

Explosive compaction of Al2O3 nanopowders

Dense bulk alumina (Al₂O₃) has been prepared by explosive compaction and its microstructure has been investigated by optical microscopy, Raman spectroscopy, scanning electron microscopy and transmission electron microscopy. The average microhardness of the alumina compact is about 171 HV0.025. Ultra-thin alumina films with glassy (translucent) appearance formed during the explosive compaction process. Nanograin Al₂O₃ particles are covered by amorphous Al₂O₃ which help to achieve a dense microstructure by promoting interparticles bonding. Phase transformation from γ-Al₂O₃ to α-Al₂O₃ during the explosive compaction process has been confirmed. Formation of the alumina compact is due to the large cooling rate and the high pressure during the explosive compaction.     

The influence of nano alumina additions on the coefficient of thermal expansion of a LZS glass–ceramic composition

In this work a 19.58Li₂O·11.10ZrO₂·69.32SiO₂ (mol%) glass–ceramic matrix was prepared and milled in order to determine its coefficient of thermal expansion (CTE) and to study how it is influenced by the addition of nanosized Al₂O₃ particles (1–5 vol%) and submicrometric Al₂O₃ particles (5 vol%). Comminution studies from the LZS parent glass frit showed that a powder with an adequate particle size (3.5 µm) is achieved after 120 min of dry milling followed by a second step of 60 h wet milling. The obtained LZS glass–ceramic samples (fired at 900 °C/30 min) showed an average relative density of ∼98% with zirconium silicate and lithium disilicate as main crystalline phases. Prepared composites with 1, 2.5 and 5 vol% of nanosized Al₂O₃ and 5 vol% submicrometric Al₂O₃ showed average relative densities varying from 97% to 94% as the alumina content increased. The formation of β-spodumene in the obtained composites leads to reduce the CTEs, whose values ranged from 9.5 to 4.4×10⁻⁶ °C⁻¹. Composites with 5% nanosized alumina showed a CTE lower than that of the equivalent formulation with submicrometric alumina.     

Effects of particle size distribution and sintering temperature on properties of alumina mold material prepared by stereolithography

Alumina mold materials prepared by stereolithography usually have considerable sintering shrinkage, and their properties related to casting have been rarely studied. In this study, alumina molds materials were prepared by stereolithography, and the effects of particle size distribution and sintering temperature on the properties of the materials were investigated. Results show that the viscosity of the slurries decreases as the fraction of fine powder increases, and the particle size distribution affects the curing behaviors slightly. Sintering shrinkage increases as the fraction of fine powder or the sintering temperature increases. Although lower sintering shrinkage can be achieved by sintering at 1350 °C or 1450 °C, the mold materials sintered at lower temperatures would continue to shrink under the service temperature of 1550 °C, and thus 1550 °C is determined as the optimal sintering temperature. As the fraction of fine powder increases, the creep resistance first increases and then decreases, and specimens prepared with 0.1 fraction of fine powder exhibit the best creep resistance with the droop distance of 4.44 ± 0.45 mm. Specimens prepared with 0.1 fraction of fine powder and sintered at 1550 °C exhibit linear shrinkage of 6.36% along the X/Y direction and 11.39% along the Z direction, and have a flexural strength of 78.15 ± 3.50 MPa and porosity of 30.12 ± 0.08%. The resulting material possesses relatively low sintering shrinkage, proper mechanical strength, porosity and high-temperature properties that meet the requirements for casting purposes.