Aqueous gelcasting of yttrium iron garnet

N,N-Dimethylacrylamide (DMAA)/N,N′-methylenebis (acrylamide) (MBAM) system was used in the aqueous YIG (yttrium iron garnet) slurry. YIG powders were prepared by using Y₂O₃ and Fe₂O₃ as raw materials through the traditional oxide method. In order to reduce the viscosity and improve the stability of slurries, SD-03 (ammonium polyacrylate) was selected as the dispersant. Zeta potential, pH, dispersant dosage, solid loading and milling time have been optimized. The best conditions were pH 9.86, dispersant dosage 0.2 wt.% and milling time 9 h, which helped to prepare the concentrated slurry with low viscosity and good liquidity. The maximum bending strength of the green body could be up to 13 MPa. The shrinkage and deformation of shaped sintered bodies prepared through gelcasting were small after sintering. The sintering shrinkage, apparent porosity and bulk density were 17%, 0.17% and 5.07 g/cm³, respectively. The dielectric constant and dielectric loss were 14.0 and 2.06 × 10^?4, respectively.     

Mullite coatings on ceramic substrates: Stabilisation of Al2O3–SiO2 suspensions for spray drying of composite granules suitable for reactive plasma spraying

The present work deals with the preparation of stable alumina + silica suspensions with high solid loading for the production of spray-dried composite powders. These composite powders are to be used for reactive plasma spraying whereby the formation of mullite and the coating on a ceramic substrate are achieved in a single step process. Electrostatic stabilisation of alumina and silica suspensions has been studied as a function of pH. Silica suspensions are most stable at basic pH whereas alumina suspensions are stable at acidic pH. The addition of ammonium polymethacrylate (APMA) makes it possible to stabilise alumina and prepare a stable 50 wt% alumina + silica suspension at pH 10. The optimum amounts of dispersant and binder have been determined by zeta potential, viscosity and sedimentation measurements. Spray drying of the suspension yields composite powders whose morphology, size distribution and flowability have been characterized before realizing reactive plasma spraying tests.     

Dispersion of nano-sized yttria powder using triammonium citrate dispersant for the fabrication of transparent ceramics

In the present work, transparent Y₂O₃ ceramics were prepared via colloidal processing method from nano-sized Y₂O₃ powders. The effects of triammonium citrate (TAC) on the colloid stability of aqueous suspensions of nano-sized Y₂O₃ powders were studied. The surface properties of yttria powders were notably affected by the addition of TAC dispersant. The adsorption of TAC on the particle surface shifts the IEP to lower pH values and increases the absolute zeta potential in alkaline region. Rheological characterization of the investigated system revealed an optimal dispersant concentration of 1 wt%, which correlated well with the saturation adsorption of TAC on Y₂O₃ powder surfaces. The suspensions with solid loadings up to 35 vol% were achieved with further addition of Tetramethylammonium hydroxide (TMAH) into the dispersing system. The consolidated green bodies were treated by cold isostatic pressing to further increase the green density. Transparent Y₂O₃ ceramics were prepared after vacuum-sintering at 1700 °C for 5 h. The transmittances of the sample were 74.5% at 800 nm and 79.8% at 2000 nm, respectively.     

Dispersion behaviour of laser-synthesized silicon carbide nanopowders in ethanol for electrophoretic infiltration

SiC nanopowders of 30 nm in diameter were successfully synthesized by laser-pyrolysis with high production rate (1.7 kg/h) and high quantity (>2 kg). The as-synthesized nanopowders were heat-treated in order to slightly oxidize the surface. It was shown that the heat-treatment does not modify structural properties or morphology but modifies the surface chemistry. Ethanolic suspensions with polyethylenimine (PEI) as dispersant were prepared from the heat-treated powders. The suspensions properties were characterized in terms of rheology, zeta potential and size distribution before and after operational pH adjustment with hydrochloric acid (HCl 1 M) or acetic acid (CH₃COOH). High concentrated suspensions (28 wt%) with low viscosity were obtained after pH adjustment with CH₃COOH. Electrophoretic infiltrations of carbon preforms carried out with these suspensions lead to a high quality infiltration of the inter-tows area as well as of the intra-tows area, some tows being completely filled with the nanopowders.     

Yttria nettings by colloidal processing

Porous ceramic burners have been shown as a promising technology to produce heat and lighting by burning low calorific fuels like modern biomass. Among ceramics, yttria (Y₂O₃) presents considerable luminescent proprieties for gas burner technology. By colloidal processing of yttria, this work aims to produce luminescence ceramic nettings with potential to be used as gas burners. Processing parameters such as mean particle size, zeta potential and flow behavior were evaluated in order to prepare suitable suspensions for replica method. Yttria nanoparticles presented light emission with λ = 550 nm when being thermal stimulated at 150 °C. Besides, the nano sized powders d₅₀ = 113.8 nm and specific surface area of 13.6 m² g⁻¹ could be highly stabilized at pH 10.5. Suspensions with 30 vol% of solids, pH 10.5, 1 wt% of dispersant and 0.3 wt% of binder presented shear thinning behavior and thixotropy suitable for replica method. As a result, samples sintered at 1600 °C/1 h showed homogeneous morphology of struts and porous microstructure desirable for gas recirculation and burning process.     

Preparation of silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction and liquid phase sintering

Dense silicon carbide ceramics using chemical treated powder by DCC via dispersant reaction method and liquid phase sintering was reported. Ammonium peroxydisulfate ((NH₄)₂S₂O₈) and ammonium carbonate ((NH₄)₂CO₃) were used as acid and base solutions to treat the silicon carbide powder, respectively. Influence of silicon carbide powder with chemical treatment on the preparation of silicon carbide suspension was studied. It was indicated that 50 vol% and 52 vol% silicon carbide suspensions with viscosities of 0.71 Pa s and 0.80 Pa s could be prepared using acid and base treated powders. Influence of silicon carbide powder with chemical treatment on the coagulation process and properties of green bodies and sintered ceramics were studied. It was indicated that silicon carbide green bodies with compressive strength of 1.13 MPa could be prepared using base treated powder. Dense silicon carbide ceramics with relative density above 99.3% and flexural strength of 697 ± 30 MPa had been prepared by DCC via dispersant reaction and liquid phase sintering using Al₂O₃ and Y₂O₃ as additives at 1950 °C for 2 h.     

Electrophoretic deposition of CoFe2O4 films from aqueous suspensions

CoFe₂O₄ nano-particles with average size of ～40 nm were synthesized via the chemical coprecipitation method. PAMANH₄ was used as dispersant to improve the stability of aqueous suspensions. Zeta potential and sediment volumes were tested to study the effects of pH and dispersant amounts on the stability of suspensions. The most stable suspension was obtained when using 0.6 wt.% PAMANH₄ as dispersant at pH = 10. Conductivity results showed that thoroughly dispersed suspensions were formed after being ultrasonic agitated for 30 min. CoFe₂O₄ films on Al₂O₃/Pt substrates fabricated via EPD sintered at 1250 °C exhibited preferentially oriented structure. The XRD analyses showed (2 2 0) and (5 1 1) were the preferential orientations. Anisotropy was also observed in magnetic hysteresis loops. Stronger ferromagnetic effect was observed in the in-plane orientation, with saturation magnetization of ～290 emu/cm³.     

Dispersion of Cu2O particles in aqueous suspensions containing 4,5-dihydroxy-1,3-benzenedisulfonic acid disodium salt

Effect of 4,5-dihydroxy-1,3-benzenedisulfonic acid disodium salt's addition upon Cu₂O dispersion properties is studied to clarify dispersant's role in colloidal properties change and its underlying stabilization mechanism, and to quantify processing conditions for the oxide. Dispersing effectiveness was studied through adsorption, rheological and electrophoretic measurements, using as-received and surface charge modified Cu₂O particles. Maximum solid loading attained without dispersant was 73 wt.% (31 vol.%), with corresponding viscosity of 152.5 ± 7.3 Pa s. Addition of dispersant resulted in viscosity between 21.0 Pa s and 5.4 Pa s. No isoelectric point was found for as-received particles’ suspensions nor for dispersed suspensions, with particles presenting negative surface charge in all studied pH range, from pH 4 to 10. Adsorption of the organic molecule caused an absolute downshift of 8–25 mV of the electrophoresis curve. Dispersant/Cu₂O interaction was assessed through FTIR analysis. Attained results suggest that, at the natural suspensions pH, dispersant-modified Cu₂O suspensions are stabilized through inner-sphere complexation mechanism, resulting in high dispersion ability.     

Direct coagulation casting of silicon nitride suspension via a dispersant reaction method

A direct coagulation casting method for silicon nitride suspension via dispersant reaction was reported. Tetramethylammonium hydroxide (TMAOH) was used as dispersant to prepare silicon nitride suspension with high solid loading and low viscosity. Influences of TMAOH and pH value on the dispersion of silicon nitride powder were investigated. Glycerol diacetate (GDA) was used to coagulate the silicon nitride suspension. Influences of the concentration of glycerol diacetate on the viscosity and pH value of the suspension were investigated. It was indicated that high viscosity sufficient to coagulate the suspension was achieved by adding 1.0–2.0 vol% glycerol diacetate at 40–70 °C. The coagulation mechanism was proposed that the silicon nitride suspension was destabilized by dispersant reacting with acetic acid which was hydrolyzed from glycerol diacetate at elevated temperature. Coagulated samples could be demolded without deformation by treating 50 vol% silicon nitride suspensions with 0.2 wt% tetramethylammonium hydroxide and 1.0–2.0 vol% glycerol diacetate at different temperatures. Dense silicon nitride ceramics with relative density above 98.8% had been prepared by this method using glycerol diacetate as coagulating agent sintered by different methods.     

Aqueous tape casting and crystallization kinetics of Ce0.8La0.2O1.9 powder

An aqueous tape casting of Ce_0.8La_0.2O_1.9 (LDC) ceramics was developed using PAA as dispersant, PVA as binder, PEG as plasticizer, and deionized water as solvent. Surface properties of LDC powder with and without PAA dispersant were characterized by electrokinetic measurements. The rheology of the LDC slurries was evaluated with a rotary viscometer. The zeta potential measurement showed that the isoelectric point for LDC powders in the absence of dispersant corresponds to a pH value of 4.02. The experimental results showed the pH value greatly affects the rheology of the slurry. The optimum content to get a stable dispersed slurry is 1.5 wt% PAA at pH value of 9–10. In presence of 1.5 wt% PAA dispersant, 5 wt% PVA binder, 5 wt% PEG plasticizer, and 55 wt% LDC powders exhibited shear thinning behavior, indicating that LDC slurry was homogenous and well stabilized. With an appropriate formulation homogeneous, smooth, and defect-free green tapes were successfully obtained. Moreover, the crystallization kinetics of LDC powders prepared by coprecipitation process also has been investigated in this study. The activation energy of crystallization was calculated on the basis of differential scanning calorimetry (DSC) at different heating rates. From non-isothermal DSC data presented values in the range of 343.3–379.1 kJ/mol and 2.282–2.030 for the activation energy of crystallization and the Avrami exponent, respectively, at specific temperatures ranging from 280 to 285 °C.     

Nanocrystalline scandia-doped zirconia (ScSZ) powders prepared by a glycine–nitrate solution combustion route

Nanocrystalline scandia doped zirconia (ScSZ) powders were synthesized by a solution combustion route using glycine, zirconyl nitrate and scandia as the starting materials. The properties of the as-synthesized powders are strongly influenced by the molar ratio of glycine-to-nitrate (g/n), where with the g/n ratio increasing from 0.14 to 1.12, the crystallite sizes of the powders decrease from 15.9 to 7.9 nm. 11ScSZ powders of specific surface areas up to 29 m²/g can be obtained through adjusting the initial g/n to 0.56 or greater. Incorporation of an appropriate amount of PEG dispersant into the starting solution can reduce the tendency of hard agglomeration formation. Investigations showed that powders from start solutions with the PEG incorporation have better sinterability than that of powders without the initial PEG incorporation, e.g., with the incorporation of 1.5 wt.% PEG dispersant in the starting solution, the resultant powders can be sintered to over 96% of theoretical density at 1200 °C, which is nearly 100 °C lower than that of powders without the initial PEG incorporation.     

Roles of polymeric dispersant charge density on lead zirconate titanate aqueous processing

Poly(acrylic acid) (PAA) and poly(acrylic acid-co-maleic acid) (PACM) were used as dispersants in preparation of lead zirconate titanate (PZT) aqueous suspensions. The effects of dispersant structure on particle stabilization were investigated through properties of the suspensions. Viscosity and sedimentation height measurements showed that addition of the dispersants improved particle stabilization. The dispersant concentrations to obtain the lowest viscosity were 0.4 wt% for PAA and 0.2 wt% for PACM based on powder dried weight basis. Furthermore, effects of pH were studied on the suspensions prepared with 0.2 wt% dispersants. Viscosity and sedimentation behaviors indicated the improvements of particle dispersion and suspension stability with an increasing pH. Particle dispersion revealed by laser light scattering and scanning electron microscopy supported an improvement of particle dispersion at alkaline pHs. Detailed analysis of these data indicated that the PACM exhibited higher dispersant efficiency for PZT aqueous suspension in all conditions. The results were discussed based on the concentrations of anionic –COO^? groups at various pHs and charge density along polymeric backbone of the dispersants.     

Aqueous gelcasting of ZrB2–SiC ultra high temperature ceramics

ZrB₂–SiC ultra high temperature ceramics containing B₄C and C as sintering additives were successfully prepared by aqueous gelcasting and pressureless sintering. Polyacrylic acid (PAA) was used as the dispersant throughout this research. The various effects of zeta potential, pH value, dispersant concentration, solid loading and ball-milling time on the rheology and fluidity behavior of ZrB₂–SiC suspension were investigated in detail. A well-dispersed suspension with 50 vol.% solid loading was prepared at pH 10 with 0.4 wt.% PAA after ball milling at 240 rpm for 24 h. Then crack-free green ZrB₂–SiC ceramics were obtained by gelcasting process and then pressureless sintered at 2100 °C to about 98% relative density. The microstructure and mechanical properties were examined, and the flexural strength and fracture toughness were 405 ± 27 MPa and 4.3 ± 0.3 MPa m^1/2, respectively.     

Dispersion of mixtures of submicrometer and nanometre sized titanias to obtain porous bodies

The stability and rheological behaviour of bimodal titania suspensions was studied. Bimodal mixtures were prepared by mixing nanosized TiO₂ powders with an average primary size of ～20–40 nm and surface area of ～50 m² g^?1 and/or a colloidal titania suspension of the same nanopowders dispersed in water with a submicrometer sized titania. The dispersing conditions were studied as a function of pH, type and content of dispersant, and sonication time for a constant solids content of 30 vol% (62 wt%). The mixtures were slip cast and presintered at low temperatures (800–1000 °C) in order to obtain porous materials with anatase as the major phase. The pore size distribution, microstructure and phase composition were characterised using MIP, SEM and XRD techniques, respectively.     

Nanoscaled BaTiO3 powders with a large surface area synthesized by precipitation from aqueous solutions: Preparation,characterization and sintering

Nanosized BaTiO₃ powders with a specific surface area of 60–75 m²/g have been prepared by precipitation of a titanium ester with Ba(OH)₂ solution at temperatures less than 100 °C. The effects of the Ba(OH)₂ concentration, isopropanol mixing with water as a solvent, the Ba:Ti ratio and surface modifiers on the surface area, the particle size, the crystalline phase, the agglomeration and aggregation degree of the synthesized powders as well as dielectric properties of sintered pellets have been investigated. The properties of the obtained powders have been characterized with XRD, BET, TG-DTA, ICP-AES, HRTEM and dilatometer. A high concentration of Ba(OH)₂ can increase the agglomeration and aggregation degree of the particles while the addition of isopropanol in water is beneficial for lowering it. To obtain stoichiometrical barium titanate, the ratio of Ba:Ti should be 1.1. The leaching of barium ions during processing can be limited by washing the powder with ammonia solution at pH10.2. A BaTiO₃ ceramic (95.8% of the theoretic density) has been fabricated by sintering the powders at 1250 °C for 2 h.     

Heterocoagulation moulding of alumina powder suspensions prepared using citrate dispersant

Coagulation characteristics of aqueous alumina suspensions prepared using di-ammonium hydrogen citrate (DHC) dispersant has been studied using MgO coagulating agent for direct coagulation casting (DCC). Mg–citrate complexes formed by the reaction between the DHC and MgO act as dispersant for alumina at pH near its iso-electric point. Setting of the alumina suspensions takes place, at MgO concentrations higher than the equivalent amount required to react with the DHC, by heterocoagulation of the alumina and MgO particles due to their opposite surface charges. The yield strength and Young's modulus of the wet-coagulated alumina bodies increased with aging time due to the hydration of the excess MgO. The minimum time required for mould removal decreases and yield strength and Young's modulus of the wet-coagulated bodies increases with MgO concentration. Alumina green bodies prepared at MgO concentrations in the range of 0.2–0.5 wt% sintered to ～97% theoretical density at 1550 °C and the sintered ceramics showed more or less similar microstructures irrespective of MgO concentrations.     

Aqueous processing of Ce0.8Sm0.2O1.9 green tapes

An aqueous tape casting of Ce_0.8Sm_0.2O_1.9 (SDC) ceramics was developed using poly(acrylic acid) (PAA) as dispersant, poly(vinyl alcohol) (PVA) as binder, poly(ethylene glycol) (PEG) as plasticizer, and deionized water as solvent. Surface properties of SDC powder with and without PAA dispersant were characterized by electrokinetic measurements. The rheology of the SDC slurries was evaluated with a rotary viscometer. The zeta potential measurement showed that the isoelectric point (IEP) for SDC powders in the absence of dispersant corresponds to a pH value of 3.66. The experimental results showed that the pH value greatly affects the rheology of the slurry. The optimum content to get a stable dispersed slurry is 2 wt% PAA in pH value range of 9–10. In presence of 2 wt% PAA dispersant, 55 wt% SDC powders exhibited shear thinning behavior, indicating that SDC slurry was homogenous and well stabilized. Homogeneous, smooth, and defect-free green tapes were successfully obtained by an appropriate slurry formula.     

Gelcasting of alumina suspensions containing nanoparticles with glycerol monoacrylate

An acrylic monomer of low toxicity containing two hydroxyl groups has been synthesized and used for gelcasting in water. The results have been compared to those achieved with the use of a commercially available monomer (2-hydroxyethyl acrylate). Due to the chemical structure of the synthesized monomer, no addition of the crosslinking agent was necessary for gelation and similar results in terms of rheology of suspensions, density and microstructure of the bodies were obtained with respect to those obtained with the commercial monomer. However, higher time for gelation was observed.Two alumina powders with very different particle sizes were used in this study: a commercial submicron-sized powder (d₅₀ = 0.35 μm) and a nanometer-sized alumina obtained by freeze-drying from aluminum sulphate solutions. The rheological behavior of concentrated suspensions was studied in order to establish their stability and to analyse the effect of the different monomers used in the process. Once the suspensions were optimized, the influence of the size of the powder on the gelation process was studied. The sintered density of submicrometer-sized alumina was higher (99%) than that measured when the bimodal suspension was used due to the difficulty to obtain highly concentrated suspensions from nanometric powder.     

Synthesis and sintering of pre-mullite powders obtained via carbonate precipitation

Ultrafine pre-mullite powders, which yield mullite at high temperatures, have been prepared from colloidal silica and aluminium nitrate via carbonate coprecipitation and followed by calcination. The chemical and structural evolutions of the as-prepared precipitation powder during thermal treatment were studied and the sinterability of pre-mullite powders were investigated. The as-prepared powders are comprised of ammonium aluminum carbonate hydroxide and amorphous silica, which convert to mullite via the Al–Si spinel phase at 1250 °C. Calcination of the as-prepared powders at 1000 °C gives a very active powder which can be reactively sintered to 98.2% theoretical density at 1550 °C. The sintered body possesses a relatively uniform chemical composition with Al₂O₃/SiO₂ mole ratio of 1.48 and exhibits a very fine interlocking equiaxed and polygonal grain morphology with grain size of 100–200 nm.     

Effect of milling type on the microstructural and mechanical properties of W-Ni-ZrC-Y2O3 composites

This study reports the effect of milling type on the microstructural, physical and mechanical properties of the W-Ni-ZrC-Y₂O₃ composites. Powder blends having the composition of W-1 wt% Ni-2 wt% ZrC-1 wt% Y₂O₃ were milled at room temperature for 12 h using a Spex™ 8000D Mixer/Mill or cryomilled in the presence of externally circulated liquid nitrogen for 10 min using a Spex™ 6870 Freezer/Mill or sequentially milled at room temperature and cryogenic condition. Then, powders were compacted in a hydraulic press under a uniaxial pressure of 400 MPa and green bodies were sintered at 1400 °C for 1 h under Ar/H₂ atmosphere. Phase and microstructural characterization of the milled powders and sintered samples were performed using X-ray diffractometer (XRD), TOPAS software, scanning electron microscope/energy dispersive spectrometer (SEM/EDS), X-ray fluorescence (XRF) spectrometer and particle size analyzer (PSA). Archimedes density and Vickers microhardness measurements, and sliding wear tests were also conducted on the sintered samples. The results showed that sequential milling enables the lowest average particle size (214.90 nm) and it is effective in inhibiting W grain coarsening during sintering. The cryomilled and sintered composite yielded a lower hardness value (5.80±0.23 GPa) and higher wear volume loss value (149.42 µm³) than that of the sintered sample after room temperature milling (6.66±0.39 GPa; 102.50 µm³). However, the sequentially milled and sintered sample had the highest relative density and microhardness values of 95.09% and 7.16±0.59 GPa and the lowest wear volume loss value of 66.0 µm³.