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.     

Effect of polymer concentration on porosity and pore size characteristics of alumina membrane substrates prepared by gelcasting

The effect of urea–formaldehyde (UF) polymer concentration on porosity and average pore size of alumina membrane substrates prepared by gelcasting has been studied. The soluble UF oligomers formed in the initial stages of polymerization act as steric stabilizer for alumina particles in the suspension. The porosity and average pore size of the substrate samples decreased with both the decrease of amount of polymer in the gelcast body and the increase of sintering temperature. Membrane substrates obtained by sintering of gelcast bodies containing UF polymer concentrations from 24.3 to 15.6 wt% at temperatures from 1250 to 1450 °C showed porosity and average pore size of 62.5–27 vol% and 0.43–0.20 μm, respectively. The membrane substrates prepared by the gelcasting method had narrow pore size distribution.     

Oxidation-bonded SiC membrane for microfiltration

Porous SiC is a proven viable material for microfiltration membranes, but its application has been limited by high fabrication cost. In this study, the oxidation bonding technique was used for the first time to fabricate SiC microfiltration membrane. The study was divided into two parts: optimization of the slurry used to dip coat the SiC particles over a porous SiC ceramic support and controlling the oxidation behaviour of SiC with respect to temperature. The oxidation behaviour during different thermal treatments was related to pore morphology and ultimately the membrane permeance. By coating the clay-bonded SiC support with oxidation-bonded SiC and sintering the coating at 1100 °C for 1 h, we prepared a defect-free microfiltration membrane with pure-water membrane permeance of >210 L m^?2 h^?1 bar^?1, an average pore size of 93 nm, and a narrow pore-size distribution.     

Low temperature synthesis of anorthite based glass-ceramics via sintering and crystallization of glass-powder compacts

Anorthite based glass-ceramics were synthesized. The investigated glass compositions are located close to the anorthite-rich corner of the fluorapatite–anorthite–diopside ternary system. Glass powder compacts with mean particle size of 2 and 10 μm were prepared. Sintering behaviour, crystallization and the properties of glass-ceramics were investigated between 800 and 950 °C. In the case of specimens made from the finer particles, complete densification was achieved at a remarkably low temperature (825 °C) and the highest mechanical strength was obtained at 850 °C, but density significantly decreased at higher temperatures. The samples prepared from the larger particles exhibited higher values of density, shrinkage and bending strength within a wider temperature range (825–900 °C). Anorthite was predominantly crystallized between 850 and 950 °C, along with traces of fluorapatite. Diopside was detected only in the MgO richer compositions.     

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.     

Microfiltration of cationic dyes using nano-clay membranes

Water resources cover 70% of earth surface with only 3% as fresh and the remaining frozen or unavailable. As a result, water and wastewater treatment have attracted a great deal of attention during last decades. Among various pollutants, dyes in textile wastewaters can have serious impacts on the environment. In the present study, low-cost ceramic nano-clay microfiltration membranes with low sintering temperature were fabricated via dry pressing, with natural zeolite as pore former. Flat disks were fabricated by sintering a mixture with various proportions of clay, zeolite and polyethylene glycol at 900 °C and characterized using FE-SEM, open porosity test, zeta potential, water permeability and acid-base treatment. Also, Membrane porosity was enhanced by increasing the zeolite content reaching 30.2% at 30 wt% and then decreased. The 30% zeolite membrane was selected for microfiltration of methylene blue, crystal violet and methyl orange from aqueous solutions. Initial and time filtered solution concentrations for each dye were measured using a UV–visible spectrophotometer. Methylene blue and crystal violet are cationic dyes due to the presence of NC(CH)₃ ⁺ while SO₃^- makes methyl orange anionic. The membrane had negative charge at pH = 6, suggesting adsorption of cationic dyes as the removal mechanism. 95.55% removal of crystal violet was obtained for the 54 mg L⁻¹ solution at 1 bar and 90.23% removal of methylene blue was obtained at optimal conditions with a 35.76 mg L⁻¹ concentration and 1.5 bar transmembrane pressure. However, less than 10% methyl orange removal was obtained, due to its negative charge. Membranes can be recovered completely by eliminating the adsorbed dyes via heat treatment at 300 °C for 1 h. The results approve the as-fabricated clay membranes cost-effective with high rejection of cationic dyes.     

Preparation of microfiltration membrane supports using coarse alumina grains coated by nano TiO2 as raw materials

To increase the mixing uniformity of coarse alumina grains with a small amount of nano TiO₂ particles, TiO₂ particles were prepared on the surface of coarse Al₂O₃ grains by in-situ hydrolysis of TiCl₄. The coated coarse Al₂O₃ powder was used to prepare microfiltration membranes supports. The effects of TiO₂ content and sintering temperatures on the bending strength, porosity and pore size distribution of the obtained supports were studied. The results show that the melted nano TiO₂ grains locate mainly at the neck of Al₂O₃ grains, which increases the bending strength of the support by increases the neck area. However, the bending strength is weakened if the TiO₂ content is excessive. No aggregated nano TiO₂ grainsare found. The resulting supports sintered at 1650 °C for 2 h yields a bending strength of 55.4 MPa, a porosity of 38% with a mean pore size of 8.0 μm.     

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.     

Fabrication of polyetherimide microporous membrane using supercritical CO2 technology and its application for affinity membrane matrix

Polyetherimide (PEI) microporous membranes with uniform cellular structure, high porosity, and narrow pore size distribution were formed by supercritical CO₂ (ScCO₂) phase inversion method, and the membrane was modified to be a matrix for the preparation of affinity membrane due to its low solvent residue and appropriate porous structure. The effects of ScCO₂ temperature and pressure on the morphology and pure water flux of the membrane were investigated. The membrane prepared at 24 MPa and 45 °C with a large mean cell diameter of 6.0 μm, high porosity of 73%, narrow pore size distribution and a pure water flux of 56 L/(m² h bar) was coated with chitosan to improve its hydrophilicity and coupled with Cibacron Blue F3GA (CB) as a special ligand to form an affinity membrane (PEI-coated chitosan-CB membrane). The PEI-coated chitosan-CB membrane showed a high adsorption capacity of 33.9 mg/g membrane to bovine serum albumin and was higher than most of affinity membranes. Moreover, the tensile strength of PEI-coated chitosan-CB membrane was 11.58 MPa and was much higher than those of affinity membranes. This work demonstrates that ScCO₂ phase inversion method is a potential method to prepare an affinity matrix.     

Processing of alumina-coated clay–diatomite composite membranes for oily wastewater treatment

Crack-free alumina-coated clay–diatomite composite membranes were successfully prepared by a simple pressing and dip-coating route using inexpensive raw materials at a temperature as low as 1000 °C in air. The changes of porosity, flexural strength, pore size, flux, and oil rejection rate of the membranes were investigated while changing the diatomite content. A simple burn-out process subjected to the used membranes in air completely recovered the specific surface area, steady state flux, and oil rejection rate of the virgin membranes. The recycled membranes showed an exceptionally high oil rejection rate (99.9%) with a feed oil concentration of 600 mg/L at an applied pressure of 101 kPa. The typical porosity, pore size, flexural strength, oil rejection rate, and steady state flux of the recycled alumina-coated clay–diatomite composite membrane were 36.5%, 0.12 μm, 32 MPa, 99.9%, and 6.91×10⁻⁶ m³ m⁻² s⁻¹, respectively, at an applied pressure of 101 kPa.     

Porous ceramic monoliths based on diatomite

Porous silica ceramics were obtained at low forming pressure and low sintering temperature by using diatomaceous earth as a silica source and boric acid as an inexpensive additive. The starting raw material, diatomite from surface coal mine Kolubara, Serbia, was purified from organic and inorganic impurities by using heat and chemical treatment. Boric acid was used as binding and sintering aid up to 2 wt%. Powder was compacted by using different pressures of 40, 60 and 80 MPa. The pressed samples were sintered at 850, 1000, 1150, and 1300 °C for 4 h in air. A relatively high porosity in the range of 60–70% is obtained for the samples pressed at 40, 60 and 80 MPa and sintered at 1000 °C. Median pore size diameters are in the range of macroporous up to 2 μm in the samples sintered at 1150 and 1300 °C. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scaning electron microscopy (SEM) and mercury porosimetry measurements were employed to characterize the phases, functional groups, microstructure and pore size distribution of the obtained samples. In addition, measurements of densities and open porosities by immersion technique, according to Archimedes principle, were used. The relations between mechanical properties (Young modulus, Poisson ratio, and compressive strength) versus content of boric acid in the investigated samples were studied and disscussed.     

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.     

Low-cost porous mullite ceramic membrane supports fabricated from kyanite by casting and reaction sintering

Porous mullite supports are firstly fabricated by casting and reaction sintering based on kyanite with Al(OH)₃ as porogenic agent. The effects of composition and sintering temperature on phase evolution, microstructure, apparent porosity, pore size distribution, linear shrinkage, gas permeation flux and mechanical property of supports are systematically investigated. Results show that the mullitization of kyanite generates needle-like mullite crystals, which form skeleton structures and improve the apparent porosity and strength of supports. Al(OH)₃ addition not only promotes the formation of needle-like mullite but also enhances the apparent porosity of supports. Temperature promotes the development of mullite, from 1450 to 1500 °C, the amount and size of needle-like mullite crystals increase, ≥1500 °C, they reveal columnar morphology. The support prepared with kyanite+40 wt%Al(OH)₃ sintered at 1500–1550 °C exhibits high apparent porosity, good gas permeation flux, excellent mechanical performance and interlocked network structure composed of well development needle-like mullite.     

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%).     

Porous anorthite ceramics with ultra-low thermal conductivity

Porous anorthite ceramics with an ultra-low thermal conductivity of 0.018 W/m K have been fabricated by hydrous foam-gelcasting process and pressureless sintering method using γ-alumina, calcium carbonate and silica powders as raw materials. Microstructure and phase composition were analyzed by SEM and XRD respectively. Properties such as porosity, pore size distribution and thermal conductivity were measured. High porosity (69–91%) and low thermal conductivity (0.018–0.13 W/m K) were obtained after sintering samples with different catalyst additions at 1300–1450 °C. Porosity, pore size, pore structure and grain size had obvious effect on heat conduction, resulting in the low thermal conductivity. The experimental thermal conductivity data of porous anorthite ceramics were found to be fit well with the computed values derived from a universal model.     

Thermoelectric Ca0.9Yb0.1MnO3−δ grain growth controlled by spark plasma sintering

n-Type Ca_0.9Yb_0.1MnO_3?δ thermoelectric (TE) powders were prepared by solid state synthesis (SSS) and co-precipitation method (Cop). The bulk TE materials were consolidated using conventional sintering (CS) and spark plasma sintering (SPS) respectively. The shrinkage behavior, as well as the sample densification strongly depends on the starting particle size. Consequently, the bulk samples from normal powder (SSS) and nano-powder (Cop) were prepared with similar density by using different sintering temperatures, of 1400 °C and 1200 °C, then 1200 and 950 °C for CS and SPS respectively. Such a decrease (up to 200 °C) of the sintering temperature is a consequent progress in terms of engineering for applications. Another advantage of the co-precipitation process compared to the conventional solid state synthesis is that, due to the small particle sizes and the decreased sintering temperature, grain growth was limited and TE properties were enhanced. The interest of the SPS process was also evidenced and we are presenting here the structural and microstructural investigations. In addition, the thermoelectric properties of samples prepared with two different processes were studied with the figure of merit of 0.18 at 750 °C.     

Elaboration of new tubular ceramic membrane from local Moroccan Perlite for microfiltration process. Application to treatment of industrial wastewaters

In this study, an original microfiltration tubular membrane (M1) made from local Moroccan Perlite was used to treat three wastewater types: effluents coming from beamhouse section of tannery (effluent A), textile effluent coming from jeans washing process (effluent B), and dicing wafer effluent generated by electronic industries (effluent C). The prepared membrane is composed of two layers of Perlite with two different granulometries: a macroporous support with a pore diameter centered near 6.6 μm and porosity of about 42%, and a microfiltration layer, performed by slip casting method, with a mean pore size of 0.27 μm. The water permeability determined of the membrane is 815 L/h m² bar. Tangential microfiltration using Perlite membrane proved to be effective in removing pollutants from the three effluents with almost the same efficiencies than that obtained with a commercial Alumina membrane (M2) with a pore diameter of 0.2 μm and a water permeability of 1022 L/h m² bar. Tangential microfiltration process operated at lower pressure (1 bar) was seen to remove turbidity from the three feeds completely. Perlite membrane allowed significant reduction of Chemical Oxygen Demand COD (50–54%) and Total Kjeldahl Nitrogen TKN (56%) of beamhouse effluent. It showed a significant decrease of COD (54–57%) and a complete discoloration of textile wastewater.     

New morphological Ba0.5Sr0.5Co0.8Fe0.2O3−α hollow fibre membranes with high oxygen permeation fluxes

Perovskite Ba_0.5Sr_0.5Co_0.8Fe_0.2O_3?α (BSCF) hollow fibre membranes were fabricated by a combined phase inversion and sintering technique. The membranes were characterised by XRD, SEM and tested for air separation. The membrane possesses a novel morphology consisting of one dense layer and one porous layer. Oxygen permeation fluxes through the obtained hollow fibre membranes were measured in the temperature range 650–950 °C using helium sweep gas rates from 50 to 200 mL min^?1. Experimental results indicated the oxygen permeation flux through the BSCF hollow fibre membrane sintered at 1050 °C was approximately 11.46 mL min^?1 cm^?2 at 950 °C when the helium sweep rate was kept at 200 mL min^?1. The BSCF hollow fibre membrane showed a stable oxygen permeation flux of 8.60 mL min^?1 cm^?2 over the investigated period of 120 h at 900 °C.     

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.     

Sinterability,microstructure and compressive strength of porous glass-ceramics from metallurgical silicon slag and waste glass

Porous glass-ceramics have been prepared by the direct sintering of powder mixtures of metallurgical silicon slag and waste glass. The thermal behavior of silicon slag was examined by differential thermal analysis and thermogravimetry to clarify the foaming mechanism of porous glass-ceramics. The mass loss of silicon slag below 700 °C was attributed to the oxidation of amorphous carbon from residual metallurgical coke in the silicon slag, and the mass gain above 800 °C to the passive oxidation of silicon carbide. The porosity of sintered glass-ceramics was characterized in terms of the apparent density and pore size. By simply adjusting the content of waste glass and sintering parameters (i.e. temperature, time and heating rate), the apparent density changed from 0.4 g/cm³ to 0.5 g/cm³, and the pore size from 0.7 mm to 1.4 mm. In addition to the existing crystalline phases in the silicon slag, the gehlenite phase appeared in the sintered glass-ceramics. The compressive strength of porous glass-ceramics firstly increased and then decreased with the sintering temperature, reaching a maximal value of 1.8 MPa at 750 °C. The mechanical strength was primarily influenced by the crystallinity of glass-ceramics and the interfaces between the crystalline phases and the glassy matrix. These sintered porous glass-ceramics exhibit superior properties such as light-weight, heat-insulation and sound-absorption, and could found their potential applications in the construction decoration.