Characterization of porous alumina bodies fabricated by high-temperature evaporation of boric acid with sodium impurity

For steel-making refractories, porous alumina bodies fabricated by the evaporation of chemical impurities at high temperatures was studied. Boron hydroxide and sodium carbonate were added in different proportions as impurities into the starting aluminum hydroxide powder compacts, which were heated at various temperatures for 1 h to form porous alumina bodies. During heating, the borate compounds that reacted with sodium seems to be formed in the liquid phase, so that all alumina particles were able to grow into platelets. Although the sodium inside the compacts was completely evaporated by 1400 °C, the boron melt was maintained above 1400 °C. Hence, alumina platelets grew with a card-house structure, which preserved the high porosity of the alumina body. After heating at 1600 °C for 1 h, the remaining boron oxide was completely evaporated and sintering between the alumina particles began to decrease the porosity. The compressive strength and porosity of the alumina bodies obtained by heating at 1700 °C for 1 h were 0.8 MPa and 64%, respectively. It is expected that the resulting porous alumina bodies can be used as castable porous clinkers.     

Flexural strength evaluations and fractography analyses of slip cast mesoporous submicron alumina

Mesoporous submicron α?Al₂O₃ green compacts were fabricated using slip casting of ultrafine alumina powders. The pre-sintered samples were sintered in air atmosphere at 1300 °C, 1350 °C, 1400 °C, and 1500 °C to obtain a variety of grain morphologies namely submicron equiaxed and micro rod structures. The resulting grain diameters lie between ～ 270 nm and ～ 1590 nm and total porosity fraction between 0.05% and 13%. The room temperature flexural strength (σ) evaluations and fractography analyses of sintered alumina samples were performed. It was observed that the total porosity fraction dictates the flexural strength as compared to grain diameter. Further, it was found that the flexural strength exhibited a decreasing trend for an increase in the total porosity fraction, and proved to be a better effective parameter than open porosity fraction. The fractography analyses suggest that samples sintered at 1300 °C and 1350 °C predominantly underwent intergranular fracture, while those sintered at 1400 °C and 1500 °C underwent a mixture of intergranular and transgranular fracture.     

Processing and properties of sol gel derived alumina–carbon nano tube composites

High purity alumina–carbon nano tube (CNT) composites were prepared by an aqueous sol–gel processing route. CNTs were dispersed in alumina sol containing appropriate amount of MgO precursor. Aqueous slurry of alumina was seeded into the sol followed by gelation, drying and calcination at 1000 °C for 1 h. The calcined powder consisting of alumina-coated CNTs and alumina was milled, sieved, dried, pressed and pressureless sintered at 1400–1600 °C for 1 h in nitrogen atmosphere. Sintered samples were further isostatically hot pressed at 1300 °C and the properties were compared with the pressureless sintered samples. Phase formation was followed by XRD study, CNT retention was confirmed by Raman studies and the samples were further characterized for mechanical and microstructural properties.     

Fabrication of porous fibrous alumina ceramics by direct coagulation casting combined with 3D printing

A novel forming method for preparing porous alumina ceramics using alumina fibers as raw materials by direct coagulation casting (DCC) combined with 3D printing was proposed. Porous fibrous alumina ceramics were fabricated through temperature induced coagulation of aqueous-based DCC process using sodium tripolyphosphate (STPP) as dispersant and adding K₂SO₄ as removable sintering additives. The sacrificial coated sand molds was fabricated by 3D printing technology, followed by the infiltration of silica sol solution for the subsequent suspension casting. Stable alumina suspension of 40 vol% solid loading was obtained by adding 2.0 wt% STPP and 40 wt% K₂SO₄. The controlled coagulation of the suspension could be realized after heating at 90 °C for about 35 min. The ceramic sample sintered at 1450 °C for 2 h showed the highest compressive strength of 24.33 MPa with porosity of 57.38%. All samples sintered at 1300–1450 °C had uniform pore size distributions with average pore size of 7.2 µm, which indicated the good structure stability when sintered at high temperature.     

Preparation and characterization of porous alumina ceramics through starch consolidation casting technique

This work aims at studying the influence of thermal treatment on the microstructure, resistivity and technological properties of porous alumina ceramics prepared via starch consolidation casting (SCC) technique. Colloidal suspensions were prepared with three different contents of alumina solid loading (55, 60 and 65 mass%) and corn starch (3, 8 and 13 mass%). The sintered samples at 1400, 1500, 1600 and 1700 °C, show open porosity between 46 and 64%, depending on the starch content in the precursor suspensions and sintering temperature. The pore structures were analyzed by SEM. The effect of corn starch content on the apparent porosity, pore size distribution, linear shrinkage and electrical resistivity as well as cold crushing strength of the sintered porous alumina ceramics was also measured. These porous alumina ceramics are promising porous ceramic materials for using in a wide range of thermal, electrical and bioceramics applications as well as filters/membranes and gas burners, due to their excellent combination properties.     

Microporous alumina substrate with porosity >70% by gelcasting

Microporous alumina membrane substrate in tubular and planar configurations have been prepared by gelcasting of alumina powder slurry using high amount of urea–formaldehyde as gelling agent followed by humidity controlled drying, binder removal and sintering of the gelled bodies. Porosity of the substrate samples sintered at 1350 °C was more than 70% as measured by mercury porosimeter. More than 51% porosity could be retained even after sintering of the samples at 1450 °C. Average pores size of the membrane substrate samples sintered at temperature in the range from 1250 to 1550 °C varied between 0.42 and 0.56 with a maximum at 1350 °C. More uniform pores were observed in sample sintered at 1450 °C. Urea-formaldehyde polymer present in the gelcast body acts as template for micropores.     

Electrically conductive porous alumina/graphite composite synthesized by starch consolidation with reductive sintering

This paper reports a facile and environment-friendly process to synthesize electrically conductive porous alumina/graphite composites by starch consolidation technique followed by reductive sintering. Green ceramic composites were consolidated with different starches and sintered at different temperatures in an argon atmosphere. Electrical measurements, carbon contents and Raman analyses of carbon structures determined an optimal sintering temperature of 1700 °C, which lead to a uniform formation of conductive graphitic networks at an optimal concentration of about 3.8 vol% in the porous composites. These carbon networks resulted into porous composites having high electrical conductivities measured in the range from 3 to 7 S/cm, which depended on the starch types and their porous properties. Correspondingly, the bulk porosities of the sintered composites were measured from 42 to 46%, with rounded micropores having diameters ranging from 14 to 39 μm. These porous properties of the sintered composites offer promising applications for conductive membrane and porous electrode.     

Sintering of zirconia ceramics by intense high-energy electron beam

A comparative analysis of the efficiency of zirconia ceramics sintering by thermal method and high-energy electron beam sintering was performed for compacts prepared from commercial TZ-3Y-E grade powder. The electron energy was 1.4 MeV. The samples were sintered in the temperature range of 1200–1400 °C. Sintering of zirconia ceramics by high-energy accelerated electron beam is shown to reduce the firing temperature by about 200 °C compared to that in conventional heating technique. Ceramics sintered by accelerated electron beam at 1200 °C is of high density, microhardness and smaller grain size compared to that produced by thermal firing at 1400 °C. Electron beam sintering at higher temperature causes deterioration of ceramics properties due to radiation-induced acceleration of high-temperature recrystallization at higher temperatures.     

Calcium phosphate growth on sintered α-alumina treated with piranha solution using a wet-chemical procedure

Two alumina samples, a high surface powder γ-alumina and a sintered α-alumina have been studied as substrates for apatite growth. In the first case, the initial stage was the calcium adsorption in an alkaline solution, followed by phosphate uptake. On the other hand, the α-alumina was firstly subjected to an acid piranha treatment at 80 °C for four hours, before alternate immersions on calcium and phosphate solutions. Next, the alumina samples were immersed repeatedly in a glycine buffer, pH 10.2, and then in tris buffer solutions, pH 7.4 at 32 °C. The resultant solids were studied by means of XRD, TEM or SEM. Calcium phosphate growth was observed in both cases. An almost uniform and continuous layer was formed on the sintered α-alumina. The results suggest that pretreatment with piranha solution seems to be a fast and efficient alternative to bioactivate the α-alumina surface.     

Hot pressing of bimodal alumina powders with magnesium aluminosilicate (MAS) addition

High quality alumina ceramics were fabricated by hot-pressed sintering using bimodal alumina with superfine component as raw material and magnesium aluminosilicate (MAS) glass as sintering aid. Densification behavior, microstructure evolution and mechanical properties of alumina were investigated from 1300 °C to 1450 °C. The bimodal alumina powders were sintered to 99.8% of the theoretical value at 1400 °C and a comparative dense microstructure with a few plate-like abnormal grains was observed. With increase of sintering temperature up to 1450 °C, many fine matrix grains were consumed and quite a few abnormal grains impinged upon each other. For the alumina ceramics hot-pressed from bimodal alumina with 30 wt.% superfine component, optimal mechanical properties were obtained at 1400 °C. The bending strength and fracture toughness were 522 MPa and 5.0 MPa m^1/2, respectively.     

Highly porous nano-SiC with very low thermal conductivity and excellent high temperature behavior

Highly porous nano-SiC is fabricated by partial sintering and decarburizing process using SiC nano-powders as starting materials and graphite flakes as pore forming agents. The prepared porous nano-SiC ceramics possess multiple pore structures, including well-distributed meso-pores in the skeleton and interconnected flakelike micro-pores. The samples prepared at 1800 °C have relatively low thermal conductivities of 5.61 ～ 0.25 W m^?1 K^?1 with porosities of 55.5–76.1%. While the samples sintered at 1500 °C with porosities between 54.0% to 76.3% show very low thermal conductivities of 0.74 ～ 0.14 W m^?1 K^?1, which is attributed to the integrated nano-scale phonon-scattering mechanisms and duplex pore structures. Porous nano-SiC ceramics also show good retention of elastic stiffness up to 1350 °C and low thermal conductivity at 1400 °C. Our results shed light on porous nano-SiC as a promising thermal insulator used in extreme thermal and chemical environments.     

Highly porous α-Al2O3 ceramics obtained by sintering atomic layer deposited inverse opals

A process for generating highly porous α-Al₂O₃ ceramics has been developed. In this paper, a combination of self-assembly and atomic layer deposition is demonstrated as a means to fabricate inverse alumina opals, which have their structures transformed via sintering. The resulting highly porous structure is stable even after a 4 h dwell time at 1400 °C, in contrast to structures generated by conventional powder metallurgy, sol-gel or colloidal powder suspension infiltration methods. TEM analysis reveals that the structure consists of single grain domains of up to 3 µm, each containing a randomly interconnected network of alumina ligaments that share a common crystalline orientation, suggesting a different mechanism of grain boundary migration during sintering. These highly porous α-alumina ceramics are considered to be ideal for filtration or catalysis applications.     

The effect of slip casting and spark plasma sintering (SPS) temperature on the transparency of MgAl2O4 spinel

MgAl₂O₄ bulk samples were fabricated by two different approaches to investigate the effect of slip casting and sintering temperature on their transparency. Three MgAl₂O₄ samples containing 1 wt% LiF, as the sintering aid, were prepared by the spark plasma sintering process (SPS) at 1400 °C and 1500 °C, under 100 MPa, for 15 min. Also, another MgAl₂O₄ sample was prepared by slip casting followed by SPS under similar conditions. It was observed that utilizing slip casting led to more transparency (10% in the visible region and 20% in the IR region) due to the more homogeneous structure. It was also observed that by reducing the SPS temperature from 1500 °C to 1400 °C, the transparency increased (20% in the IR region) because of the lower grain growth rate at the lower temperature.     

Densification behavior and properties of alumina–chrome ceramics: Effect of TiO2

Highly dense alumina–chrome bodies with low porosity are usually used as corrosion and thermal resistant refractories. Alumina–chrome refractory with molar ratio 1:1 was developed using chemical grade hydrated alumina and chromium (III) oxide by conventional sintering route. Batch materials were attrition milled, isostatically pressed and sintered in the temperature range from 1000 °C to 1700 °C with 2 h soaking at peak temperature. Phase development of the sintered materials with temperature was studied by X-ray diffraction. Sintering temperature, sintering condition and addition of sintering aid (TiO₂) have immense effect on the densification of the alumina–chrome refractory. Highly dense alumina–chrome refractory with almost nil apparent porosity was developed at 1500 °C in reducing atmosphere. Flexural strength of the sintered materials at room temperature and at 1200 °C was also measured. 1 wt% TiO₂ gives the optimum result with respect to densification and flexural strength.     

Microstructure and mechanical properties of Ti(C,N)-based cermets fabricated by in situ carbothermal reduction of TiO2 and subsequent liquid phase sintering

Ti(C,N)-based cermets were prepared by in situ carbothermal reduction of TiO₂ and subsequent liquid phase sintering in one single process in vacuum. The densification behavior, phase transformation, and microstructure evolution of the cermets were investigated by DSC, XRD, SEM, and EDX. The results showed that the carbothermal reduction of TiO₂ was completed below 1250 °C, and Ti(C,N)-based cermets with refined grains were obtained after sintered at 1400 °C for 1 h by this method. The hard phase of the cermets mainly exhibited white core/gray rim structure, in great contrast to the typical black core/gray rim structure of hard phase in traditional cermets. Ti(C,N)-based cermets prepared by this novel method showed excellent mechanical properties with a transverse rupture strength of 2516±55 MPa, a Rockwell hardness of 88.6±0.1 HRA, and a fracture toughness of 18.4±0.7 MPa m^1/2, respectively.     

Influence of cassava starch content and sintering temperature on the alumina consolidation technique

The influence of starch content and sintering temperature on the preparation of alumina bodies were studied. The process was water-based and cassava starch was used as consolidator, binder and pore former. Colloidal suspensions were prepared with three different starch concentrations and the ideal dispersant content and gel point were determined by rheological analysis. The wet samples were demolded after consolidation in silicone mold at 60 °C for 2 h. After the drying step the samples were sintered at 1200, 1400 and 1600 °C, showing open porosities between 13 and 55%, depending on the starch content on the precursor suspensions and sintering temperature. The pore structures were analyzed by SEM (scanning electron microscopy) and Hg porosimetry. Basically, the pore structures are dominated by large spherically shaped pores left by the starch particles, which are connected through small pore channels.     

Reaction sintering of AlN–AlON composites

Sintering behavior of three different compositions in the AlN–Al₂O₃ system using Y₂O₃ as a sintering aid was investigated. Samples with various ratios of AlN/Al₂O₃ were sintered in nitrogen atmosphere using a gas pressure furnace in the temperature range 1750–1950 °C. The densification of the samples was studied by shrinkage and relative density measurements. Results showed that samples containing 1 and 70 wt.% alumina were sintered to near theoretical density at 1800 °C; whereas the sample with 20 wt.% alumina never reached densities higher than 93% in the temperature range considered. It was found that the AlN/Al₂O₃ ratio and the sintering temperature had a great influence on the microstructure and crystalline phases present in the samples, namely, AlN, γ-AlON, 27R, and YAG. In the sample with 20 wt.% alumina, porosity formation prevented further densification. These porosities were probably due to the release of oxygen during sintering.     

Effect of sintering temperature on phase constitution and mechanical properties of WC-1.0 wt% carbon nanotube composites

Ultrafine grain WC-1.0 wt% carbon nanotube (CNT) composites were prepared using spark plasma sintering and the influence of sintering temperature on the properties of the composites was investigated. The specimen tested in this study achieved an optimum hardness of 22.81±0.81 GPa and fracture toughness of 8.95±0.38 MPa m^1/2 after sintering at 1700 °C. On applying a sintering temperature of 1900 °C, the mechanical properties of the specimens deteriorated. Raman spectroscopic analysis results indicated that the structure of the CNTs changed and the graphite phase occurred at 1900 °C, which was responsible for the deteriorating hardness, elastic modulus, and fracture toughness. This study provides details of the transformation of the CNTs in the tungsten carbide matrix, indicating that the WC-CNT composites should be sintered at moderate temperatures.     

Dense zircon (ZrSiO4) ceramics by high energy ball milling and spark plasma sintering

The addition of sintering additives has always been detrimental to the mechanical properties of sintered ceramics; therefore, methods to reduce or, as in this case, eliminate sintering additives are usually relevant. In this paper, dense zircon ceramics were obtained starting from mechanically activated powder compacted by spark plasma sintering without employing sintering additives.The high energy ball milling (HEBM) of starting powder was effective to enhance the sintering kinetics. The structural changes of the zircon powder introduced by the HEBM were evaluated. The phase composition and the microstructure of bulk zircon material were analyzed by SEM (EDAX) and XRD. The Vickers hardness and the fracture toughness were evaluated as well.Fully dense materials were obtained at 1400 °C with a heating rate of 100 °C/min, 10 min soaking time and 100 MPa uniaxial pressure. The zircon samples sintered at temperatures above 1400 °C were dissociated in monoclinic zirconia and amorphous silica. The dissociation was detrimental for the mechanical properties. Unlike conventional sintering methods (hot pressing, pressureless sintering) SPS permitted to overcome the dissociation of the zircon material and to obtain additive free, fully dense zircon ceramic with outstanding mechanical properties.     

Red mud as a substitute coloring agent for the hematite pigment

Red mud (RM), a highly alkaline iron oxide rich sludge obtained during the production of alumina, was treated to work as a coloring agent for ceramic glazes. The approach aims the valorization of this residue, adding environmental and economic value. RM was sintered at different temperatures (1100 °C, 1150 °C, 1200 °C, 1250 °C, 1300 °C and 1350 °C) to assess changes in its mineralogical composition. The obtained powders were characterized by XRD, UV–Vis and CIELab. The samples were added to glazes (transparent, opaque and matte) and their color stability analyzed by CIELab. RM sintered at 1300 °C was compared with commercial hematite producing lower coloring power but yielding better color stability on glazes for temperatures of 1100 °C ± 15 °C, thus presenting RM_1300C as a suitable substitute for the hematite pigment.