Preparation and characterization of porous mullite ceramics via foam-gelcasting

Porous mullite ceramics were prepared via foam-gelcasting using industrial grade mullite powder as the main raw materials, Isobam-104 as the dispersing and gelling agent, sodium carboxymethyl cellulose as the foam stabilizing agent, and triethanolamine lauryl sulfate as the foaming agent. The effects of processing parameters such as type and amount of additive, solid loading level and gelling temperature on rheological properties and gelling behaviors of the slurries were investigated. The green samples after drying at 100 °C for 24 h were fired at 1600 °C for 2 h, and the microstructures and properties of the resultant porous ceramic samples were characterized. Based on the results, the effects of foaming agent on the porosity level, pore structure and size and mechanical properties of the as-prepared porous mullite ceramics were examined. Porosity levels and pore sizes of the as-prepared samples increased with increasing the foaming agent content up to 1.0%, above which both porosity levels and pore sizes did not change. The compressive strength and flexural strength of the as-prepared sample with porosity of 76% and average pore size of 313 μm remained as high as 15.3±0.3 MPa and 3.7±0.2 MPa, respectively, and permeability increased exponentially with increasing the porosity.     

Macro-porous ceramic supports for membranes prepared from quartz sand and calcite mixtures

A new type of porous ceramic supports for membranes has been designed. The new supports have been fabricated from polycrystalline quartz sand and calcite raw materials. In this work, two configurations of support (tubular and flat) have been produced using extrusion method. The open porosity, the pore size distribution, the average pore size (APS), the strength and the permeability of sintered supports have been found to depend mainly on the weight ratio of calcite (CaCO₃) additive. The results showed that with the addition of 15–35 wt.% of calcite and sintering temperature of about 1375 °C for 1 h the best characteristics of sintered supports could be obtained. The developed tubular ceramic supports with the APS 6.3–12 μm, open porosity 42–55%, the water permeability (16–68 m³/h m² bar) and flexural strength 8–18 MPa hopefully offer many perspectives for a wide use in membranes technology.     

Preparation of porous Al2TiO5-Mullite ceramic by starch consolidation casting and its corrosion resistance characterization

Stabilized Al₂TiO₅ (AT)-mullite (M) porous ceramics were fabricated by starch consolidation casting using corn starch as curing agent and their microstructure, mechanical properties, pore size distribution and corrosion resistance were examined. Results showed that AT-M porous ceramic with the flexural strength of 11.5 MPa, apparent porosity of about 54.7% and pore size distribution in the range of 1–15 µm could be obtained with 10 wt% corn starch addition. Corrosion resistance results showed mass losses in hot H₂SO₄ solution and NaOH solution for 10 h to decreased from 1.03% to 0.36% and 4.39–2% when the calcination temperature increased from 1400 °C to 1450 °C, which proved these AT-M porous ceramics to possess an excellent corrosion resistance in acidic condition when calcined at 1450 °C.     

Preparation processes and characterizations of alumina-coated alumina support layers and alumina-coated natural material-based support layers for microfiltration

Recently, porous ceramic membranes have become a subject of significant interest due to their outstanding thermal and chemical stability. To reduce the high manufacturing costs of these porous ceramic membranes, recent research has focused on the utilization of inexpensive natural materials. However, there have not been any well-established direct comparisons of the membrane properties between typical alumina-based membranes and novel natural material-based membranes. Therefore, we compared alumina-coated alumina support layers (with average pore sizes ranging from 0.10 µm ~0.18 µm), alumina-coated diatomite-kaolin composite support layers (with an average pore size of 0.12 µm), and alumina-coated pyrophyllite-diatomite composite support layers (with an average pore size of 0.11 µm) via the dip-coating method and subsequent heat treatment ranging from 1200 °C–1400 °C for 1 h. The pure water permeability of the alumina-coated diatomite-kaolin composite support layer and the alumina-coated pyrophyllite-diatomite composite support layer was found to be approximately 2.0×10² L m⁻² h⁻¹ bar⁻¹, which is similar to that of an alumina-coated alumina support layer. Therefore, we suggest that the average pore size of an alumina-coated natural material-based support layer can be effectively controlled while exhibiting acceptable water permeability.     

Preparation and characterization of low-cost ceramic microfiltration membranes for the removal of chromate from aqueous solutions

Low-cost ceramic microfiltration membranes were prepared using clay of IIT Guwahati. Two membranes were prepared by paste casting followed by sintering at different temperatures, the first one from clay only (membrane A) and the second one from clay with small amounts of sodium carbonate, sodium metasilicate and boric acid (membrane B). Both the membranes were characterized by TGA, SEM, XRD, water permeability test and acid–base treatment. With the increase of sintering temperature, pore size as well as permeability and flexural strength were increasing while porosity and pore density were decreasing. The overall performance of membrane B was better than membrane A. The average pore size, porosity, pore density and flexural strength of membrane B sintered at 1000 °C were 4.58 μm, 0.42, 2.06 × 10¹⁰ m^− 2 and 11.55 MPa respectively. This membrane was used for the removal of chromate from aqueous solutions by micellar enhanced microfiltration (MEMF) using cetylpyridinium chloride (CPC). 100% rejection of chromate ions were obtained at a feed ratio (CPC/chromate) of 10. Based on raw material prices, the membrane cost was estimated to be $19/m². The prepared low-cost membrane showed good promise for the treatment of wastewater containing such heavy metals.     

Thermal conductivity of ceramic/metal composites from preforms produced by freeze casting

Porous alumina and zirconia preforms, processed by ice templating, have been used to manufacture ceramic/metal composites by aluminium alloy infiltration. The aim of the present work is to study the influence of the ceramic material nature and of the initial porous structure on the thermal conductivity anisotropy of the composite in order to assess potential applications in the field of thermal management. The materials are characterised in terms of pore volume fraction and pore size before and after metal infiltration. The freeze casted preforms exhibit anisotropic lamellar structures with ellipsoidal pores ranging from 35 µm to 40 µm and porosity fractions from 64 to 67%. After metal infiltration, composite parts present the same anisotropic morphology, which correspond to alternating ceramic and metal layers. Thermal conductivities have been determined, with an average of 80 W m⁻¹ K⁻¹ and 13 W m⁻¹ K⁻¹ parallel and perpendicular to the freezing direction respectively, for zirconia/metal composites. Theoretical values of thermal conductivity can be calculated using the Maxwell-Eucken relation, to handle the residual porosity, in combination with series and parallel resistance models to describe the overall anisotropic character. These give good agreement to experiment.     

Effect of phase composition of natural quartz raw material on characterization of microfiltration ceramic membranes

The results of development of multi-layer ceramic membranes on the basis of natural quartz raw material from Mongolia are presented. The influence of the phase composition and temperature of calcination on the porosity, morphology and mechanical strength of large-porous ceramic support obtained by the method of isostatic pressing was studied. It was established that multi-layer ceramic membranes obtained by the application of water suspension of high-disperse quartz sand of Mongolia and alumosilicate binder with the addition of 15–35 wt% of quartz are characterized by optimal properties. The developed tubular ceramic membranes with the average pore size 5.3 µm, coefficient of air permeability (4.17–4.41)×10⁻¹³ m², productivity by water 46.3–48.0 m³/(h×m²×bar) and mechanical strength 2.27–2.53 MPa are perspective for wide use in microfiltration processes.     

Preparation and characterization of porous MgAl2O4 spinel ceramic supports from bauxite and magnesite

Porous magnesium aluminate spinel (MgAl₂O₄) ceramic supports were fabricated by reactive sintering from low-cost bauxite and magnesite at different temperatures ranging from 1100 to 1400 °C and their sintering behavior and phase evolution were evaluated. The effects of sintering temperature on the pore structure, size and distribution as well as on the main properties of spinel ceramic supports such as flexural strength, nitrogen permeation flux and chemical resistance were investigated. The supports prepared at 1300 °C showed a homogeneous pore structure with the average pore size of 4.42 μm, and exhibited high flexural strength (35.6 MPa), high gas permeability (with nitrogen gas flux of 3057 m³ m⁻² h⁻¹ under a trans-membrane pressure of 0.1 MPa) and excellent chemical resistance.     

Preparation and characterization of novel ceramic membranes for micro-filtration applications

Porous microfiltration range ceramic membranes were prepared using kaolin and other suitable materials like feldspar, quartz, boric acid, activated carbon, sodium metasilicate and titanium dioxide following standard paste casting route. The membranes were casted as circular disks of 40 mm ID and 5 mm thickness. They were characterized using thermo gravimetric analysis (TGA), particle size distribution (PSD), X-ray diffraction (XRD) and scanning electron microscope (SEM) to evaluate the effect of maximum sintering temperature on the structure, porosity and mechanical integrity. The prepared membranes were initially dried at 120 °C and 250 °C for 24 h each and finally sintered at 850 °C, 900 °C and 950 °C for 6 h. Morphological parameters viz. pore size distribution, porosity, average pore size of the prepared membranes were determined and the membrane performance were evaluated by carrying out the permeation experiment with pure water. Results show that the average pore size of the membranes increases from 1.59 µm to 2.56 µm and porosity of the membrane supports decreases from 18.88% to 5.59% with increase in sintering temperature from 850 °C to 950 °C. The membrane corrosion resistance was also tested using acid and base and it is observed that there is no significant weight loss in the process. Based on market price of the inorganic precursors, the membrane cost was estimated to be $92/m² which can be considered low cost in the microfiltration range for industrial applications.     

Porosity features and gas permeability analysis of bi-modal porous alumina and mullite for filtration applications

Bimodal porous structures were prepared by combining conventional sacrificial template and partial sintering methods. These porous structures were analysed by comparing pore characteristics and gas permeation properties of alumina/mullite specimens sintered at different temperatures. The pore characteristics were investigated by SEM, mercury porosimetry, and capillary flow porosimetry. A bimodal pore structure was observed. One type of pore was induced by starch, which acted as a sacrificial template. The other pore type was due to partial sintering. The pores produced by starch were between 2 and 10 µm whereas those produced by partial sintering exhibited pore size of 0.1–0.5 µm. The effects of sintering temperature on porosity, gas permeability, and mullite phase formation were studied. The formation of the mullite phase was confirmed by XRD. Compressive strengths of 37.9 MPa and 12.4 MPa with porosities of 65.3% and 70% were achieved in alumina and mullite specimens sintered at 1600 °C.     

Permeability and elastic modulus of cement paste as a function of curing temperature

The permeability and elastic modulus of mature cement paste cured at temperatures between 8 °C and 60 °C were measured using a previously described beam bending method. The permeability increases by two orders of magnitude over this range, with most of the increase occurring when the curing temperature increases from 40 °C to 60 °C. The elastic modulus varies much less, decreasing by about 20% as the curing temperature increases from 20 °C to 60 °C. All specimens had very low permeability, k < 0.1 nm², despite having relatively high porosity, ? ~ 40%. Concomitant investigations of the microstructure using small angle neutron scattering and thermoporometry indicate that the porosity is characterized by nanometric pores, and that the characteristic size of pores controlling transport increases with curing temperature. The variation of the microstructure with curing temperature is attributed to changes in the pore structure of the calcium–silicate–hydrate reaction product. Both the empirical Carmen–Kozeny, and modified Carmen–Kozeny permeability models suggest that the tortuosity is very high regardless of curing temperature, ξ ~ 1000.     

The impact of heat treatment on the microstructure of a clay ceramic and its thermal and mechanical properties

This paper presents the results of an experimental study on the microstructure, the thermal and the mechanical properties of a clay-based ceramic used in building applications. The X-ray tomography analysis showed a layered microstructure of clay with 200 µm sheets of porosity after the extrusion process. The gas release from the dehydration, dehydroxylation and decarbonation induced a 7 vol% formation of porosity during the heat treatment of the clay-based ceramic up to 850 °C. The porosity increase and the development of metakaolin led to a 38% decrease in the thermal conductivity. On the other hand, the Young's modulus of the clay-based ceramic was conserved due to the formation of smaller pores than the 200 µm sheets of porosity. The densification and the crystallization of amorphous phases also led to a 110% increase of the Young's modulus from 850 °C to 1050 °C. The Young's modulus of the clay-based ceramic was only decreased by the β→α quartz inversion of the cooling due to sand addition. Hence, this study provided a useful insight into how the microstructure of fired clay bricks can be specifically transformed by the porosity during the heat treatment to control the thermal and mechanical properties.     

Effect of sintering temperature on microstructure and mechanical properties of zirconia-toughened alumina machinable dental ceramics

This study investigated the effect of sintering temperature on the microstructure and mechanical properties of dental zirconia-toughened alumina (ZTA) machinable ceramics. Six groups of gelcast ZTA ceramic samples sintered at temperatures between 1100 °C and 1450 °C were prepared. The microstructure was investigated by mercury intrusion porosimetry (MIP), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques. The mechanical properties were characterized by flexural strength, fracture toughness, Vickers hardness, and machinability. Overall, with increasing temperature, the relative density, flexural strength, fracture toughness, and Vickers hardness values increased and more tetragonal ZrO₂ transformed into monoclinic ZrO₂; on the other hand, the porosity and pore size decreased. Significantly lower brittleness indexes were observed in groups sintered below 1300 °C, and the lowest values were observed at 1200 °C. The highest flexural strength and fracture toughness of ceramics reached 348.27 MPa and 5.23 MPa m^1/2 when sintered at 1450 °C, respectively. By considering the various properties of gelcast ZTA that varied with the sintering temperature, the optimal temperature for excellent machinability was determined to be approximately 1200–1250 °C, and in this range, a low brittleness index and moderate strength of 0.74–1.19 µm^−1/2 and 46.89–120.15 MPa, respectively, were realized.     

Design and preparation of high permeability porous mullite support for membranes by in-situ reaction

The natural mineral kaolin combined with alumina additives Al(OH)₃,α-Al₂O₃ and AlF₃ was used to prepare porous mullite ceramic membrane supports using an in-situ reaction. The effects of composition and sintering temperature on the sintering behavior, pore structure, permeability and microstructure of the resulting porous mullite supports were extensively investigated. The experimental results showed that excess SiO₂ in kaolin can be consumed by adding alumina precursors, which resulted in a stiff skeleton of interlinked needle-like mullite crystals in-situ during the sintering. The needle-like mullite crystals touched each other and formed a short network, which acted as a porous skeletal network structure. This network resulted in a highly permeable porous structure. The resulting support is suitable for the preparation of asymmetric ceramic membranes. The densification and pore structure of the support can be effectively adjusted by control of the quantity of alumina precursors in the composition and the sintering temperature. Sintering the subject mullite compositions at 1500 °C for two hours resulted in support structures with an average porosity of 45.9%, an average pore size of 1.3 µm and a penetrating porosity of 35.9%.     

Biomass assisted microfiltration of chromium(VI) using Baker's yeast by ceramic membrane prepared from low cost raw materials

This work deals with the preparation of ceramic microfiltration membrane from inexpensive raw materials such as kaolin, quartz, calcium carbonate by uniaxial dry compaction method. The prepared green membrane was initially dried at 100 °C for 24 h, 200 °C for 24 h and finally sintered at 900 °C for 6 h. The properties of the membrane such as porosity, flexural strength, chemical stability and hydraulic permeability were investigated. The fabricated membrane possessed an average pore diameter of 1.32 μm, porosity of 30% and flexural strength of 34 MPa. Furthermore, the chemical stability of the membrane was found to be excellent. Eventually, the separation performance of the membrane in terms of flux and removal of chromium(VI) ion using baker's yeast biomass as a function of applied pressure, pH, metal ion concentration and biomass dosage was also studied. The removal of Cr(VI) was found to be strongly dependent on the initial pH of the solution. At lower pH, the metal solution shows higher removal due to higher binding of the metal ion with biomass. It was also observed that the removal of Cr(VI) ion increases with increasing the biomass concentration and decreases with increasing the metal ion concentration. The removal of Cr(VI) was found to be independent of the applied pressure. The maximum removal of Cr(VI) was found to be 94% with the permeate flux of 2.07 × 10^-5 (m³/m² s) for a metal solution concentration of 100 mg/L.     

Fabrication and characterization of anorthite–mullite–corundum porous ceramics from construction waste

In this work, anorthite–mullite–corundum porous ceramics were prepared from construction waste and Al₂O₃ powders by adding AlF₃ and MoO₃ as mineralizer and crystallization catalyst, respectively. The effects of the sintering temperature and time on open porosity, mechanical properties, pore size distribution, microstructure, and phase composition were characterized in detail. The results showed that the formation of the mullite whiskers and the properties of the anorthite–mullite–corundum porous ceramics depended more on the sintering temperature than the holding time. By co-adding 12 wt% AlF₃ and 4 wt% MoO₃, mullite whiskers were successfully obtained at sintering temperatures upon 1350 °C for 1 h. Furthermore, the resultant specimens exhibited excellent properties, including open porosity of 66.1±0.7%, biaxial flexural strength of 23.8±0.9 MPa, and average pore size of 1.32 µm (the corresponding cumulative volume percent was 37.29%).     

Effects of mono-dispersed PMMA micro-balls as pore-forming agent on the properties of porous YSZ ceramics

Porous yttria-stabilized zirconia (YSZ) ceramics were successfully fabricated by the dry pressing method with different size (1.8–20 μm) and amount (2–60 vol.%) of mono-dispersed poly methyl methacrylate (PMMA) micro-balls. Different PMMA additions with different size and amount were investigated to achieve optimal thermal and mechanical properties. With increases of the amount of PMMA, the porosity of porous YSZ ceramics ranges from 7.29% to 51.6%, the flexural strength increases firstly and then decreases, and the thermal conductivity decreases continuously. With decreases of the diameter of PMMA micro-balls, the mean pore size and thermal conductivity of porous YSZ ceramics decrease, and the flexural strength of porous YSZ ceramics with same porosity increases firstly and then decreases. The porous YSZ ceramics with a higher porosity (18.44 ± 1.24%), the highest flexural strength (106.88 ± 3.2179 MPa) and low thermal conductivity (1.105 ± 0.15 W/m K) can be obtained when the particle diameter and the amount of PMMA are 5 μm and 20 vol.%, respectively.     

Dry pressed ceramic tiles based on fly ash–clay body: Influence of fly ash granulometry and pentasodium triphosphate addition

Fly ash from brown coal (70 wt.%) and stoneware clay (30 wt.%) were used for the dry pressed ceramic tiles (according to EN 14411) raw materials mixture. The effects of fly ash milling and pentasodium triphosphate addition as a deflocculant and fluxing agent on the properties of green body (flexural strength, bulk density) and fired body (EN ISO 10545—water absorption, bulk density, true density, apparent porosity, flexural strength, frost resistance) were studied and explained as a function of the firing temperature (1000–1150 °C). Fly ash milling (corresponding to 5 wt.% residue of fly ash grains on 0.063 mm sieve) increased the sintering abilities of the fly ash–clay body. A similar effect was achieved by 1.3 wt.% pentasodium triphosphate (PST) addition with an increase in green body flexural strength and a decrease in water content of the granulate. Fly ash–clay bodies can be frost resistant with water absorption above 10% due to positive pore size distribution, which were examined using the high-pressure mercury porosimetry method.     

Effects of heating rate on the structure and properties of SiOC ceramic foams derived from silicone resin

Silicon oxycarbide ceramic foams were fabricated in a single step manufacturing process using in situ foaming of SiOC powders loaded silicone resin. The effects of heating rate on the porosity, compressive strength and microstructure of the ceramic foams were investigated. The porosity (total and open) increased firstly and then decreased with increasing heating rate. It was possible to control the total and open porosity of ceramic foams within a range of 81.9–88.2% and 62.4–72.5% respectively, by adjusting the heating rate from 0.25 °C/min to 3 °C/min while keeping the silicone resin content at 90 vol%. However, the compressive strength decreased with increasing the heating rate progressively, and the average compressive strength of the foams was in the range of 1.0–2.3 MPa. Micrographs indicated that the ceramic foams which cross-linked at a heating rate less than 1 °C/min had a well-defined open-cell and regular pore structure.     

Mechanical and optical properties of spark plasma sintered transparent Y2O3 ceramics

Commercial Y₂O₃ nanopowder was used to fabricate transparent Y₂O₃ ceramics by spark plasma sintering under the pressure of 100 MPa for 20 min with the heating rate of 100 °C/min. The microstructures, mechanical and optical properties of the Y₂O₃ ceramics sintered at different temperatures were investigated in detail. Densification occurred up to a sintering temperature of 1500 °C, and above 1500 °C, rapid grain growth and pore growth occurred. The highest relative density of 99.58% and the minimum average grain size of 0.58±0.11 µm were obtained at 1500 °C. The flexural strength, hardness and fracture toughness of the optimal spark plasma sintered Y₂O₃ ceramic were 122 MPa, 7.60 GPa and 2.06 MPa.m^1/2, respectively. The Y₂O₃ ceramic sintered at 1500 °C had the in-line transmission of about 11–54% and 80% in the wavelength range of 400–800 nm and 3–5 µm, respectively.