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Ceramic membranes are more advantageous alternatives especially for harsh working conditions when compared with the polymeric membranes. The porous multilayer structure of the ceramic membranes (composed of support, intermediate, and top layers) can be prepared via different oxides. Titania and zirconia, having superior properties, are mainly preferred for the top layer formation. The separation properties of the membrane are both dependent on pore morphology and surface charge of the oxide(s) forming the top layer. The effect of surface charge in separation may be very significant in case of filtration of charged species with relatively lower mass as in the ultrafiltration (UF) and nanofiltration (NF). In this study, unsupported membrane top layers were prepared with varying titania/zirconia ratios by sol-gel technique. Their surface charges at different pH conditions after calcination at varying temperatures (400°, 500°, and 600 °C) were determined. The surface charge of the pure titania (full Ti) top layer was decreasing with the increasing calcination temperature. The highest magnitudes of zeta potential for both acidic and basic conditions were measured via Zr rich top layer (TiZr2575) at calcination temperatures ≥ 500 °C, which was composed of anatase, rutile (titania), and tetragonal (zirconia) phases after calcination. The tailor-made top layer can be prepared with modifications during membrane preparation.

Modification of the setting process of brushite cements by varying the concentration of ions that alter calcium phosphate crystallization kinetics, is known to enable control on the monetite conversion extent and the accompanying microporosity. This is useful because monetite serves as a suitable matrix in macroporous scaffolds due to its higher phase stability and finer crystal morphology compared to its hydrous counterpart brushite. In this study the synergistic effect of NaCl and citric acid on the microstructural evolution of brushite cement was demonstrated and microporosity of macroporous monetite-rich cement blocks was minimized by a variable NaCl porogen size distribution approach. Initially, maximum packing ratio of various combinations of NaCl size groups in PEG were determined by their rheological analysis in a range between 57% and 69%. Statistical analysis revealed a positive correlation between the amounts of NaCl particles under 38μm and 212μm and the maximum packing ratio. Further broadening the size distributions of NaCl porogens with fine cement precursors was effective in increasing the solids packing ratio of cement blocks more than the maximum packing ratio for the porogens. This improvement in packing was accompanied by a reduction in microporosity despite the increase in micropore volume with ion induced monetite formation. The detrimental effect of the microporosity introduced to the structure during monetite formation was balanced for some size distributions and not so much for others, thereby resulting in a wide range of porosities and mechanical properties. Thus, the exponential dependence of mechanical properties on porosity and the mechanical properties of monetite-rich macroporous blocks at the theoretical zero-porosity were determined according to Rice's model. Zero-porosity extrapolations were much higher than those predicted for brushite cement, contrary to the common assumption that brushite is mechanically stronger than monetite.

Brushite forming calcium phosphate cements (CPCs) have received growing interest for scaffold applications due to their high surface area and high bioresorbability. The dehydrated form of brushite, monetite, has a finer microstructure with higher surface area, higher strength and bioresorbability comparable to brushite, making it a viable alternative phase in CPCs. The increase in monetite content of the β-tricalcium phosphate (β-TCP)–monocalcium phosphate monohydrate (MCPM) cement system due to the reduction in its supersaturation upon addition of NaCl to excess setting liquid was investigated kinetically. The relaxation period was monitored by pH-stat titration of the cement solution by 0.1 M NaOH. Monetite growth was achieved in shorter periods at higher NaCl concentrations where the supersaturation gap between brushite and monetite is thought to be narrowed due to high ionic strength in accord with Pitzer's ion interaction model. The brushite/monetite ratio decreased consistently with increasing NaCl concentration in the 3–6 M range.

The effects of nanostructure on the artificial photosynthesis activities of undoped and Nd doped titania (TiO2) powders prepared by three different chemical co-precipitation methods were investigated. Substitutional/interstitial N and S doping was observed in powders due to the presence of high concentrations of HNO3 (NP) and H2SO4 (SP) in the powder preparation media, respectively. Nd, N and S doping caused anatase/rutile phase transformation inhibition and crystallite size reduction in the nanostructure. Light absorption was significantly enhanced by Nd doping and the residual SO42−/NOx species in the nanostructure. Photocatalytic hydrogen production activity of Nd doped NP powder was 4 times greater than undoped NP powder at 700 °C and had a high purity (CO:H2 ratio∼0.00). CO was determined to be the main product in photocatalytic CO2 reduction. NP powders had the highest CO yields and Nd doping enhanced CO production. The powders with high crystallite sizes and rutile weight fractions had the highest artificial photosynthesis activities.

The development of a better understanding of the low temperature nanophase evolution of high surface area titania (TiO2) based powders is essential for their use in photocatalytic applications. A series of rare earth (RE) element doped TiO2 powders were prepared by sol-gel processing. The effects of RE doping level, ionic size and heat treatment temperature on the nanophase structure evolution and the dopant ion location in TiO2 main matrix were investigated. Anatase was determined to be the main phase up to 900 °C at all doping levels for all REs. Anatase to rutile phase transformation was inhibited by RE doping. The inhibitory effect of REs increased with increasing ionic radius. Oxide phases of La, Nd, Pr, Sm were not present up to 5% and Nd4Ti9O24 phase was formed at 10% doping level at 800 °C. The formation of RE2Ti2O7 phases were determined for the REs with relatively lower ionic radii at 800 °C., Scientific and Technological Research Council of Turkey (TUBITAK 10M739)

Strength distributions of particle agglomerates in six different yttria powders were measured using a calibrated ultrasonic sound field. The density of sintered pellets was directly related to the agglomerate strength of each powder. No systematic relation to the sintered density was observed for bulk densities or pressure-density compaction data for the loose powders, or for pore size distributions or green densities for the pressed compacts.

Monodisperse silica spheres in the 50–520 nm size range were prepared by using the Stober process. Diffusive growth has been determined from Nielsen chronomal analysis for the 520 and 310 nm monodisperse silica spheres. The densification behaviour and evolution of the microstructure of the sphere compacts indicated an inverse dependence of shrinkage rate on the sphere size due to viscous sintering. The increase in sphere size from 50 to 500 nm shifted the densification temperature from ~1120 °C to 1240 °C. The amorphous nature of the spheres was conserved up to 1200 °C where cristobalite crystal nucleation started and complete transformation to cristobalite phase has been observed upon heat treatment at 1300 °C. The activation energies for viscous sintering according to the Frenkel and Mackenzie/Shuttleworth models were calculated as 125 and 335 kJ/mol, respectively. These substantially low activation energies can be attributed to the presence of a significant level of silanol groups.

23rd Symposium and Annual Meeting of International Society for Ceramics in Medicine, ISCM 2011; Istanbul; Turkey; 6 November 2011 through 9 November 2011, The goal of the present work was to investigate the effects of several cement preparation parameters on setting and hardening reaction mechanisms and hydroxyapatite (HA) cement properties. A central composite experimental design (CCD) was conducted by choosing particle size, solid to liquid ratio, pH, seed concentration and buffer concentration as design parameters along with compressive strength and setting time being the responses. Tetracalcium phosphate (TTCP) powders were prepared by heat treatment of calcium and phosphate source mixtures in the 1200-1400°C temperature range followed by quenching to room temperature in a dessicator. The second phase used in the formulations (brushite) was prepared by aqueous chemical methods. A series of HA pastes/cements were prepared by changing the above mentioned design parameters. Cements were characterized by a standardized setting time test, mechanical testing machine, SEM and XRD. HA cements with the desired properties can be formulated by using CCD in which the responses were expressed by a second order polynomial equation of the parameters. Compressive strengths for the majority of HA cements were determined to be in the 100-160 MPa range which is significantly higher than those reported in the literature. © (2012) Trans Tech Publications., TÜBİTAK-TEYDEB to MGM R&D Laboratories under the Tekno Girişim Project No.8070082

Monodisperse silica sols with well-defined spherical particles ranging in size from 5 to 310 nm were prepared through Stober process. Both particulate and polymeric sol-gel routes were employed for the preparation of stable silica sols. The use of polymeric species in combination with particulate silica spheres may allow the design of predefined membrane pore structures with high thermal stability by cubic/random/close packing of monodisperse spherical particles incorporated into the polymeric network. The size and volume content of spheres were varied in order to modify the consolidation behaviour of 2-structural silica membranes which would enhance the thermal stability. The low shrinkage level for sphere loaded 2-structural systems compared to the pure polymeric counterparts might be explained by the decrease in the structural free energy of the polymeric/particulate 2-structural system. The thermal stability of the microporous membranes may thus be improved by incorporating particulates into the polymeric network through the formation of a lower extent of thermally induced microcrack formation. The N2 permeation through 90 nm silica sphere added silica membranes remained constant when they were heat treated in the 250-400 °C range indicating the stability of the pore network. © 2009 Elsevier B.V. All rights reserved.

The compressive mechanical response of an FP™ continuous fiber (35 vol.%) Mg composite has been determined in the transverse and longitudinal directions at quasi-static and high strain rates. It was found that the composite in the transverse direction exhibited strain rate sensitivity of the flow stress and maximum stress within the studied strain-rate range of 1.3 × 10 −4 to 1550 s −1 . The failure strain in this direction, however, decreased with increasing strain rate. Microscopic observations on the failed samples have shown that the composite failed by shear banding along the diagonal axis, 45° to the loading axis. Twinning was observed in the deformed cross-sections of the samples particularly in and near the shear band region. The strain rate sensitivity of the fracture stress of the composite in transverse direction is attributed to the matrix strain rate sensitivity. In the longitudinal direction, the composite failed by kink formation at quasi-static strain rates, while kinking and splitting were observed at the high strain rates. The maximum stress in the longitudinal direction was, however, found to be strain rate insensitive within the strain rate regime of 1.3 × 10 −4 to 500 s −1 . In this direction, similar to transverse direction, twinning was observed in the highly deformed kink region. Several different reasons are proposed for the strain rate insensitive compressive strength in this direction.

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003, Ceramic supports were prepared from fine alumina and zirconia powders by dry-pressing and slip-casting. These supports were heat treated in the 1100° - 1200°C temperature range and dip-coated with ceramic sols prepared from alkoxides by using sol-gel methods. The average sol particle sizes were measured as 3-7 nm for zirconia and 30-40 nm for alumina by laser scattering technique. The optimum heat treatment temperature range was determined as 500°-600°C for dip-coated membranes by using TGA (thermo gravimetric analysis) results. The microstructure of the ceramic composite membranes was investigated by SEM (Scanning electron microscope). The clean water permeability (CWP) of the membranes was tested by using deionized water in a filtration set-up. Separation experiments were performed with bovine serum albumin (BSA, Stokes diameter: 7 nm) solution and whey to determine the protein separation capacity of the composite membranes. The CWP of the dry pressed alumina supports heat treated at 1100°C was found to be higher than the permeability of the slip-casted zirconia supports heat treated at 1200°C. The protein retention of the slip-casted zirconia support was determined as 60% by using UV-Vis spectrophotometer (Abs. at 280nm). A protein retention value of 96% was achieved for whey after the modification of the support with dip-coating. The permeate flux was 40 L/m2hour for dry-pressed alumina support dip-coated with zirconia sol calcined at 500°C.

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003, The preparation of nanocrystalline titania and alumina was investigated by sol-gel methods using titanium isopropoxide, boehmite and aluminum isopropoxide. Various drying control chemical additives like oxalic acid, acetic acid and polyacrylic acid were used for modifying the drying behaviour and shrinkage of the gels. The sintered densities of the ceramics prepared by sol-gel processing and the dried gels were in the 79-99% of theoretical density for rutile. The green and sintered densities of the pellets prepared by uniaxial pressing of powders derived from sols, gels and precipitation techniques for titania were in the 40-52% and 55-83% respectively. The titania ceramics were observed to experience anatase-rutile phase transformation upon heat treatment at 650oC. The grain size of the sintered ceramics at 650oC was determined to be about 26 nm. Grain size of titania increased to 213 nm. at 850oC. The mechanical properties of these nanocrystalline ceramics were investigated by using microhardness testing.

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003, Magnesia-chromite (MgO + MgO·Cr2O3) and magnesia-spinel (MgO + MgO·Al2O3) refractory bricks that are used in the high temperature zones of rotary cement kilns are investigated for their microstructural characteristics. Their microstructures are important because the size, shape and distribution of periclase grains, chromites and the quality of their bonding phases significantly affect their service performances. The purpose of this study was to characterize the microstructures of industrial brick samples to develop a protocol to compare different products e.g. for evaluation as replacement bricks. In some of the chromite containing bricks iron-rich rims were observed, while a domestic brick with similar chemistry had no such feature. These iron-rich rims were examined using SEM-EDS. It was found that the counter-diffusion of Fe+3 and Cr+3 were responsible for their formation. Exsolved chrome-spinel was widely observed in the microstructures of chromite bricks. Magnesia-spinel bricks were found to contain low melting calcium aluminates as bond phases in the microstructure, posing a threat to service performance. Portmortem microanalysis of industrially used bricks revealed alkali attack in addition to creep as main destruction mechanisms for brick. Traces of elements like Mo, S and alkalies were observed and thought to originate from the use of waste derived fuels.

In the present study, the preparation and characterization of polylactide-Hydroxyapatite(HA) composite films for biomedical applications have been studied. The effects of number of parameters such as polymer type, HA loading, surface modification and its concentration on the mechanical and microstructural properties of the composites were investigated. Poly-L-Lactide and 96/4 Poly(L-Lactide co D-Lactide) copolymer-HA composites containing 10-40 wt% HA particles have been prepared by solvent casting technique. The HA powder was synthesized by precipitation technique. Interfacial interactions between HA and polylactide polymer were modified to improve filler compatibility and mechanical properties of the composites by surface treatment of the HA with two different silane coupling agents; 3-aminopropyltriemoxysilane (AMPTES) and 3-mercaptopropyltrimethoxysilane (MPTMS) at three different concentrations(0.5-2 wt%). Silane treatment indicated improvements in the mechanical properties of the composites compared to the untreated HA loaded polylactide composites. Tensile test results showed that the maximum improvement in the mechanical properties of the composites was obtained for PLA composites containing 1 wt% aminofunctional silane treated HA and 0.5-wt% mercaptopropyltrimethoxy silane treated HA for PDLA composites. Scanning electron microscopy studies also revealed better dispersion of silane treated HA particles in the polymer matrix.

Nanocrystalline mesoporous titania powders were synthesized by hydrolyzing titanium isopropoxide in ethanol–water mixtures which were ultrasonically treated without using any templates or chemicals. Titanium isopropoxide–ethanol mixture was added dropwise to a water–ethanol mixture placed in an ultrasonic bath. The properties of the sonochemically synthesized powder were compared with those of the powders prepared without ultrasonic treatment along with Degussa P-25 titania powder. The phase structure, crystallite size, surface area, particle size, powder density were determined and sintering behavior was analyzed in this work. The nanotitania powder prepared during ultrasonic induced hydrolysis (TiO 2 -U) was determined to be formed from a mixture of anatase and brookite phases at 25 °C. The brookite phase in nanotitania powder prepared without ultrasonic treatment (TiO 2 -NoU) was detected at 70 °C. The anatase–rutile phase transformation was completed in the 500–700 °C range for both powders. The average crystallite sizes of the powders at 25 °C were determined as 10 and 5 nm for TiO 2 -NoU and TiO 2 -U, respectively. The surface area decreased from 238 to106 m 2 /g for TiO 2 -NoU and from 287 to 82 m 2 /g for TiO 2 -U when the calcination temperature was increased from 200 to 500 °C. The evolution of the N 2 adsorption–desorption behavior with calcination temperature and the corresponding pore size distributions/volumes was attributed to the formation of closely packed submicron aggregates during powder synthesis and calcination. The sintering behavior was concluded to be controlled by 7–10 nm crystallites and the submicron aggregates. The determination of the densification behavior of titania powders prepared by different methods with various levels of dopants may prove to be very useful for a better understanding of the phase/pore structure evolution which is crucial for a significant number of applications.

In this study, the effects of partial Sb 3+ ion substitutions for the Y sites and the Cu sites on the superconducting properties of YBa 2Cu 3O y (Y123) ceramic superconductors were investigated. The samples were prepared by the conventional solid-state reaction method and the properties of the samples were investigated by means of X-ray diffraction, AC magnetic susceptibility measurements, scanning electron microscope, and energy dispersive X-ray analysis. The critical temperatures were determined to be in the range of 80-92 K for both Systems I and II. It was found that Sb-addition leads to the formation of the non-superconducting YBa 2SbO 6 phase, which has a negative effect on the critical temperature, since the highest critical temperature was measured for pure Y123. However, the increasing substitution level has a negligible effect on the X-ray diffraction analysis peak intensities of the superconducting phases. In addition, SEM images showed that Sb substitution decreases the grain size and modifies the microstructure development, which makes the samples denser.

Diphasic gels prepared by mixing freshly prepared polymeric silica and polymeric boehmite sols through a modified Al-alkoxide route in mullite compositions led to the crystallization of mullite upon heat treatment at 775 °C. Mullite formation was observed at a 100 °C higher temperature when diphasic gels were formed by mixing aged polymeric sols containing about 2 nm in diameter boehmite species. These relatively low mullite formation temperatures were attributed to the nanoscale sizes of the polymeric species of the two amorphous phases present in the diphasic gels.

Stable polymeric and colloidal boehmite sols were prepared by sol-gel process through controlled hydrolysis/condensation reactions. The particle sizes of the colloidal sols were in the 12-25 nm range depending on the process parameters and about 2 nm for polymeric sols. The presence of a significant increase in the microporosity content of the heat treated polymeric membranes relative to the mesoporous colloidal membranes might make the design of thermally stable microporous alumina membranes with controlled pore structures possible. The phase structure evolution in the 600-800 °C range had shown that the crystallization of the gamma alumina in the amorphous matrix starts at about 800 °C. This indicated that the pore structure stability may be enhanced through processing up to this relatively high temperature in polymeric alumina derived unsupported membranes. The permeance values of the two and three layered colloidal alumina membranes were observed to be independent of pressure which implies that the dominant gas transport mechanism is Knudsen diffusion in these structures. This was also supported by the 2.8 nm BJH pore sizes of the colloidal membranes. The Knudsen diffusion equation derived permeances of the polymeric alumina membranes with thicknesses of about 300 nm were determined to be very close to the experimentally determined permeance values. © 2010 Springer Science+Business Media, LLC.

In this work, effects of compaction pressure on the structural and superconducting properties of BSCCO ceramic superconductors were investigated. The study was carried out on two systems which were, System I: Bi 1.7Pb 0.3Sr 2Ca 2Cu 3O y and System II: Bi 1.6Pb 0.3Ag 0.1Sr 2Ca 2Cu 3O y, respectively. Ceramic powders were prepared by conventional solid-state reaction method and sintered at 850°C after compaction at five different pressures in the 150-750 MPa range. Critical temperatures of samples were determined by resistivity-temperature determinations made by four-point probe method in liquid nitrogen conditions. XRD analysis was conducted by powder X-ray diffraction method. Morphology of the grains present in the samples were determined by using scanning electron microscope (SEM) photographs at 2 K× and 2.5 K× magnifications for System I and System II, respectively. Sintered densities of the superconducting ceramics were measured by Archimedes water displacement method and unit cell parameters were additionally obtained from XRD data. T c values for System I was determined to be in the 109-115 K with sample D having the highest T c of 115 K while T c varied in the 104-109 K range and sample B had the highest T c value of 109 K for System II. The transition width, which is a sign of the purity of the samples, was determined to be narrow for both systems. The data obtained from X-ray diffraction measurements have shown that 2223 high-T c phase was dominant in both systems. The determination of the optimum pellet compaction pressure for BSCCO ceramic superconductors was the main purpose of this work. The results of this work indicated that compaction at around 450 MPa improves the superconducting and structural properties of the BSCCO ceramic superconductors. © 2009 Springer Science+Business Media, LLC.

Monodisperse silica spheres were synthesized by TEOS hydrolysis, then consolidated by three different processes. Spheres of 270 nm were dispersed in water and centrifuged to form highly ordered compacts with packing efficiencies of 67–68% of the powder density. Dilute sphere suspensions were filtered to form relatively thin dense cakes. Pellets were also prepared from randomly agglomerated powders by uniaxial pressing. Green bodies were sintered at temperatures between 800–1 100 °C for 2–24 h. Pore size distributions of the ordered compacts were determined by mercury porosimetry. No major changes in the pore size distributions were observed for samples sintered between 800 and 950 °C. The sintered ordered samples were not translucent and reached approximately 96–97% of theoretical density at 1 000 °C. In contrast to the centrifugally ordered samples, the filtered cakes became translucent at 1 000 °C. Temperatures of almost 1 100 °C were required to reach high density for compacts made from agglomerated powders. SEM micrographs of the sintered and ordered compacts show the presence of narrow void regions with sizes on the order of the sphere size. These areas are most likely the remnants of the domain boundaries which existed in the ordered green compact. The results of this study show the interference of the domain boundaries in the green compacts to be detrimental to densification, limiting the achievable final densities and degrading the properties of the sintered ceramics. This is despite the fact that the centrifugally-ordered samples had the highest densities in the green state.

The effect of partial substitution of Ca by Zn in Bi1.7Pb0.3Sr2Ca2−x Zn x Cu3O y at x=0.00, 0.05, 0.10, 0.15 and 0.20 levels on the electrical and structural properties was investigated in this work. The characterization of the ceramics prepared by the conventional solid-state reaction method were done by resistance–temperature measurements, XRD, SEM and density analysis. Low levels of Zn substitution of Ca caused significant changes in the properties of the ceramics. The low-T c superconducting properties were enhanced and the fraction of the low-T c (2212) phase were found to increase at x=0.15 level of Zn substitution at 830 °C sintering temperature. Zero resistance was observed only in sample D with x=0.15 and the T c was determined as 92 K. The SEM micrographs and the density analysis have shown that this was the densest packed ceramic.

A characterization technique has been developed to quantitatively determine agglomerate strength distributions in bulk powders. This technique may be used throughout a powder processing procedure to determine the source of agglomeration, as well as an aid in the elimination of these agglomerates by helping the user to understand the nature of the interparticle bonds. Quantitative strength distributions are determined via exposure of a powder dispersion to a calibrated ultrasonic field and following the ensuing changes in the dispersion via particle size analysis. The ultrasonic field calibration method, developed by Ciftcioglu et al. , was examined to ascertain its quantitative ability. Difficulties encountered with the calibration method are discussed at length and suggestions made for its applicability and use.

The extent of ultrasonic cavitation forces on suspended particles was characterized by comparison to hollow glass bubble strength distributions obtained via mercury porosimetry. The effective breaking strength of the different energy input levels of the ultrasonic disruptor were found to vary between 1.1 and 80.5 MPa. Model ordered monosize silica sphere agglomerates were ultrasonically treated and the changes in the particle size distribution followed in order to determine the strength of these agglomerates. Similar analyses done on synthesized titania powders have shown the importance of drying and ethanol washing of precursor precipitates to the strength of the final oxide agglomerates.

Natural zeolites undergo structural changes after heating which open their possible use in different fields, related to their chemical and physical properties, such as building stone, lightweight aggregate, ceramic foam, concrete bricks, tiles, porcelain stoneware and additive in puzzolonic cements. In this study, thermal behavior of zeolitic tuff quarried from Gördes-Manisa, region of Turkey was investigated. Zeolitic rocks were first reduced to 2 μm and pellets were prepared by dry-pressing. The pellets were heated for 30 min in the temperature range of 200-1200 °C. Heating the tuff up to 600 °C did not cause any structural change detectable by X-Ray powder diffraction (X-Ray), Fourier Transform Infrared Spectroscopy (FTIR) and thermal characterization methods with regard to the original sample, while further increase in the temperature caused structural breakdown of zeolitic tuff. The appearance of the broad low intensity peaks in X-Ray diffraction diagrams indicated most probably a partial transformation of crystal structure into an amorphous structure. The Scanning Electron Microscopy (SEM) micrographs showed that the crystals seen in the original rock sample were broken during grinding and pressing processes. The crystal structure disappeared above 1000 °C and the spherical pores was observed at 1200 °C. Chemical composition of the zeolitic tuff did not change significantly with respect to temperature. The highest density (2.28 g/cm3) and hardness (387 Hv) were obtained by sintering the pellets at 1000 °C for 30 min., İYTE 96K121240

Presented at the 10th Aachen Membrane Colloquium, 16–17 March 2005, Aachen, Germany, Ceramic supports were prepared from alumina powder and dip-coated with zirconia sol. The ceramic composite membranes prepared were characterized with respect to their microstructure/pore structures. The supports were 40% porous of which 87% were open pores. The average particle size of the sol particles was 35 nm. The prepared membrane has good protein lactose separation properties with a relatively high protein content (PR ∼80%) and with relatively low lactose retention (LR ∼7%). The permeate flux value was around 40 l/m2h. These results indicate the possibility of the preparation of ceramic composite membranes for separation of whey components with higher yields.

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003, Low temperature synthesis of spinel powder via intense mechanical grinding was performed. A dramatic decrease in the synthesis temperatures of ground powders was achieved. We were able to produce partially crystallized spinel at room temperature via a 110 minute grinding. Characterization of the synthesized powders was performed using SEM, XRD and DTA. Each stage of synthesis was analyzed using these techniques. Mixtures of Mg(OH)2 and Al(OH) 3 were used for synthesis. Temperatures as low as 800°C were able to produce bumps in the XRD patterns of ground powders at the 2θ angles for spinel crystals.

The aim of this study was to investigate the stability and dispersion behaviour of aqueous alumina suspensions in the presence of polyethylene oxide-polypropylene oxide-polyethylene oxide (PEO/PPO/PEO) type block copolymers. The influence of water soluble triblock copolymers with molecular weight ranging from 2900 to 12600 g/mole were tested at Φ = 0.125, 1, 10, 20 vol % solid loading alumina suspensions by rheological, turbidity, sedimentation and surface tension measurements. The results indicate that an alternative dispersant for alumina suspensions is the PEO/PPO triblock copolymers. Their stabilisation mechanism was attributed to the depletion stabilisation. Rheological measurements indicated that these block copolymers (at high EO percentages) coupled with ultrasonic treatment have a positive effect on the dispersion of the agglomerated alumina suspensions. It was not possible to create stable dispersions in the absence of ultrasonic bath treatment. Turbidity measurements at Φ = 0.025, 0.125 vol % showed that, alumina suspensions with PEO/PPO added were stable and have higher turbidity values than block copolymer free suspensions.

The effect of partial substitution of Cu in Bi 1.7 Pb 0.3 Sr 2 Ca 2 Cu 3-x Sb x O y at x = 0.0, 0.05, 0.1, 0.15, and 0.2 levels on the electrical and structural properties was investigated in this work. X-ray diffraction analysis shows that these materials have a multiphase structure. Two different types of particles with different morphologies were observed in scanning electron micrographs, The T c values decreased from 103.5 to 87 K for x = 0.1 Sb substitution level with a subsequent increase to 101 K at x = 0.2.

The effects of substituting poly(acrylic acid), PAA, and mucic acid for citric acid in the standard Pechini powder synthesis process was studied. Strontium titanate was chosen as the model system for this study. Powders were prepared from precursor solutions in which PAA (average molecular weight = 2,000 and 5000) was substituted for citric acid (up to 70% by weight), and with reduced weight of total organic reagents (50% reduction). The powders prepared with a 30% substitution of PAA for citric acid produced weakly agglomerated submicron particles after calcining. These powders contained a larger fraction of weak agglomerates than the powders prepared by the original Pechini process. As such, the PAA derived powder could be easily fractionated and dispersed with greater than 70% of the calcined powder having particle sizes less than 0.5 μm

Methods of preparing non-agglomerated powders for three systems -- yttria, titania, and yttria-stabilized zirconia -- are reviewed. The non-agglomerated nature of these powders should make it possible to sinter them into dense ceramic bodies with nanocrystalline grain sizes. Experiments with yttria-stabilized zirconia have shown that this is indeed the case, with mean linear intercept grain sizes of 60 nm resulting from original powder particle diameters of 13 nm. This ultrafine-grained zirconia is shown, in turn, to have superplastic forming rates 34 times faster than a 0.3 μm-grained commercial zirconia of the same composition.

TiO2 has been fabricated using a modified alkoxide hydrolysis route; the process yields about 50 g/day of nanocrystalline powder on a laboratory scale, which can be used to make large (1–10 g) samples. Pore size distributions show the powder is non-agglomerated, and TEM and BET analyses confirm the nanocrystalline size of the particles at about 20 nm. The powder is extremely reactive, sintering at about half the temperatures required of commercial powders. The chemically produced powder compacts to only 62% of the density that can be achieved by compacting a gas phase condensation (GPC)-produced TiO2. Nevertheless, the reactivity of this less dense compact is such that it reaches final densities comparable to that of the GPC TiO2. The difficulties in compacting and sintering large nanocrystalline samples are discussed. It is hoped that an understanding of these problems will lead to more intelligent densification of ultrafine powders so that full densification can be accomplished while retaining a nanocrystalline grain size.

Intrusion—extrusion hysteresis in mercury porosimetry is thought to be caused either by mercury contact angle hysteresis or by the domination of extrusion by pore bodies and intrusion by throats to the pore network. Mostly, only the information obtained during the intrusion of mercury has been used in the pore structure characterization of materials via mercury porosimetry. The use of the data obtained during extrusion has been the subject of several recent studies in an attempt to reach a more complete picture of pore structure. In this work, the possible use of both intrusion and extrusion for pore structure characterization have been investigated. Submicron monosize spherical particles of silica and yttrium hydroxycarbonate were synthesized and ordered compacts of these powders have been prepared. Mercury porosimetry tests on these high-density compacts (typically 68 – 70% of sphere density) have shown the presence of two pore peaks for intrusion and extrusion with the exception of one compact. Comparisons of intrusion pore sizes with the theoretical sizes of the constrictions for ordered sphere packings have shown reasonable agreements. Similar comparisons between the sizes of cavities in sphere packings and the extrusion pore sizes did not show the same agreement. Results for one sample did not show a distinct extrusion pore size even at very large pore sizes, most probably due to the domination of mercury extrusion by very few large pores present in the sample. For all other samples, the extrusion pore sizes were close to the actual sphere size and the extrusion was most probably dominated by a few vacant sphere sites in the ] ordered structures. The results of this work have shown that the possibility of using extrusion data for pore body size distribution determination is in serious doubt. The presence of very few larger pores in the porous body may dominate the whole extrusion process and can cause the extraction of inaccurate pore size information from the extrusion data.

Proceedings of the 8th Conference and Exhibition of the European Ceramic Society; Istanbul; Turkey; 29 June 2003 through 3 July 2003, Sintering and mechanical behavior of pure and hydroxyapatite (HA) whisker reinforced HA composites were investigated in this work. Pure and composite samples were prepared by using a commercial powder and whiskers prepared by molten salt synthesis. The dry-pressed samples were sintered in the 800 and 1300°C range. The effect of whisker-addition on the mechanical properties of HA was investigated through compression and hardness testing. Compressive strength and fracture strain were observed to increase by the addition of whiskers.