Analyses of Young's modulus and thermal expansion coefficient of sintered porous alumina compacts

This paper reports the derivation of Young's modulus (E) and thermal expansion coefficient (TEC, β) for a sintered porous structure with open pores. The theoretical E is affected by the number of grains and the grain boundary area in sintered ceramics. The measured E–porosity relationship for porous alumina compacts were compared with the theoretical E values that were derived for the present open-pore structure and also for the dispersed (closed)-pore structure treated previously. With decreasing porosity (50% → 10%), the scattered E values showed a gradually increasing tendency, which were located between two theoretical curves for the open-pore structure. The sudden increase of E values in the porosity range from 10% to 0% was well explained by the theoretical dependence of E on porosity for the open- or closed-pore structure. The β values for the porous alumina structures were independent of porosity and close to the β values reported for fully dense alumina compacts. This result was in accordance with the theoretical β–porosity relationships for the open-pore and closed-pore structures.     

Calcium carbonate decomposition in white-body tiles during firing in the presence of carbon dioxide

This study examines the thermal decomposition process of the calcium carbonate (calcite powder) contained in test pieces of porous ceramics, of the same composition as that used in manufacturing ceramic wall tile bodies, in the presence of carbon dioxide, in the temperature range 1123–1223 K. The experiments were carried out in a tubular reactor, under isothermal conditions, in a gas stream comprising different concentrations of air and carbon dioxide.     

Utilization of granodiorite in the production of porcelain stoneware tiles

In the present study, the use of granodiorite, as fluxing agent in a body mix for stoneware ceramic tiles production, was assessed. Four batches were formulated using clay from Khaboba, and natural granodiorite from Saint Katherine, Sinai, Egypt. The batches were tailored to completely replace both feldspatic and inert components of stoneware ceramic tiles. Densification was studied according to ISO rules, while sinterability was estimated by optical dilatometry. The dependence of microstructure and mechanical properties of stoneware ceramic tiles on granodiorite content was discussed. Strength measurements showed that increasing granodiorite content the bending strength of the bodies increased. In particular the studied batches can be used for the production of industrial fast firing tiles. The obtained ceramic tiles possess properties similar to commercial ceramic floor and/or wall tiles.     

Synthetic carbons activated with phosphoric acid III. Carbons prepared in air

Synthetic activated carbons were prepared by phosphoric acid activation of a styrene-divinylbenzene copolymer in an air atmosphere at various temperatures in the 400-900 °C interval. The carbons were characterized by elemental analysis, cation-exchange capacity measurement, infrared spectroscopy, potentiometric titration, copper adsorption from solution and physical adsorption of N₂ at −196 °C and CO₂ at 0 °C. It was shown that, similarly to synthetic phosphoric acid activated carbons obtained in argon, the synthetic carbons activated with phosphoric acid in air possess an acidic character and show considerable cation-exchange properties. The contribution of oxygen-containing surface groups along with phosphorus-containing groups to CEC is higher for carbons obtained in air. Three types of surface groups were identified on carbons prepared at temperatures up to 600 °C, and four types on carbons prepared at higher temperatures. These groups were assigned to ‘super-acidic’ (pK<0), phosphorus-containing (pK=1.1-1.2), carboxylic (pK=4.7-6.0) and phenolic (pK=8.1-9.4) groups. The cation-exchange capacity was at a maximum for the carbon prepared at 800 °C. Copper adsorption by synthetic phosphoric acid activated carbons obtained in air at temperatures lower than 800 °C is higher than for similar carbons obtained in argon. The increase is due to additional formation of oxygen-containing surface groups. Calculated copper binding constants revealed the importance of phosphorus-containing and carboxylic groups for adsorption of copper from aqueous solution. All carbons show a multimodal pore size distribution including simultaneously micropores and mesopores, but the porous texture is not a prime factor in determining the cation-exchange capacities of these carbons. Synthetic phosphoric acid activated carbons show a greater development of porosity when obtained in air as compared to carbons carbonized in argon.     

New multifunctional porous Yb2SiO5 ceramics prepared by freeze casting

New porous Yb₂SiO₅ ceramics were prepared by a water-based freeze casting technique using synthesized Yb₂SiO₅ powders. The prepared porous Yb₂SiO₅ ceramics exhibit multiple pore structures, including lamellar channel pores and small pores, in its skeleton. The effects of the solid content and sintering temperature on the pore structure, porosity, dielectric and mechanical properties of the porous Yb₂SiO₅ ceramics were investigated. The sample with 20 vol% solids content prepared at 1550 °C exhibited an ultra-low linear shrinkage (i.e. 4.5%), a high porosity (i.e. 79.1%), a high compressive strength (i.e. 4.9 MPa), a low dielectric constant (i.e. 2.38) and low thermal conductivity (i.e. 0.168 W/(m K)). These results indicate that porous Yb₂SiO₅ ceramics are good candidates for ultra-high temperature broadband radome structures and thermal insulator materials.     

Effect of starch addition on microstructure and properties of highly porous alumina ceramics

Porous alumina ceramics with ultra-high porosity were prepared through combining the gel-casting process with the pore-forming agent technique. Porosity and pore size distribution of the sintered bulks were evaluated with and without adding starch, respectively. In particular, the influences of starch addition on the properties, including thermal conductivity and compressive strength were studied. It was found that the incorporation of starch increased the nominal solid loading in the suspension and subsequently promoted the particle packing efficiency. The porosity is raised with increasing starch content from 0 to 30 vol%, which brings the decrease in thermal conductivity, whereas the compressive strength isn't seriously degraded. The further higher starch addition (40 vol%), however, would deteriorate the performance of the alumina porous ceramics. It is believed that the appropriate starch amount (lower than 30 vol%), working as a pore-forming agent, suppresses the driving force of densification without affecting the connections of neighboring grains while excessive starch amount would lead to the collapse of the porous structure.     

Nanomechanical behavior of yttria stabilized zirconia (YSZ) based thermal barrier coating

In the present study, the detailed evaluation of nanomechanical properties in terms of hardness and Young׳s modulus of duplex and compositionally graded YSZ based thermal barrier coating (TBC) have been evaluated by nanoindentation technique. Duplex and compositionally graded TBCs have been fabricated by thermal spray deposition technique. As TBCs are commonly applied for high temperature protection, effect of isothermal treatment in air (at 900 °C and 1000 °C) on nanomechanical properties has also been evaluated. Finally, the mechanical properties have been correlated with characteristics of the coating. The hardness and Young׳s modulus of the TBCs are found to increase with increased duration of thermal exposure. Modulus of resilience and resistance to plastic deformation of the duplex and compositionally graded TBC have also been evaluated at room temperature and with thermal exposure and discussed in detail.     

Microstructure and properties of lightweight fibrous porous mullite ceramics prepared by vacuum squeeze moulding technique

A novel fibrous porous mullite network with a quasi-layered microstructure was produced by a simple vacuum squeeze moulding technique. The effects of organic binder content, inorganic binder and adsorbent on the microstructure and the room-temperature thermal and mechanical properties of fibrous porous mullite ceramics were systematically investigated. An anisotropy microstructure without agglomeration and layering was achieved. The fibrous porous mullite ceramics reported in this study exhibited low density (0.40 g/cm³), low thermal conductivity (~0.095 W/(m K)), and high compressive strength (~2.1 MPa in the x/y direction). This study reports an optimal processing method for the production of fibrous porous ceramics, which have the potential for use as high-temperature thermal insulation material.     

Thermal expansion and heat capacities of holmium and erbium orthotantalates ceramics

Monoclinic M-orthotantalates of holmium and erbium ceramics were obtained by co-precipitation and annealing at 1773 K and characterized by X-ray powder diffraction, scanning electron microscopy, and chemical analysis. Using the high-temperature X-ray diffraction method, the temperature dependence of the monoclinic lattice parameters of both ceramics were determined at range 298-1273 K. The molar heat capacity of M-HoTaO₄ and M-ErTaO₄ were measured by adiabatic (7-350 K) and differential scanning (320-1350 K) calorimetry. Standard thermodynamic function (entropy, enthalpy change, and reduced Gibbs energy) were calculated on the smoothed values of molar capacity, without taking into account contribution of low-temperature interval: 0-7 K for M-HoTaO₄ and 0-8 K for M-ErTaO₄. The general shape of the anomalous Schottky contribution to the molar heat capacity was determined.     

Dense yttria-stabilized zirconia coatings fabricated by plasma spray-physical vapor deposition

Plasma spray-physical vapor deposition (PS-PVD) is a novel technique which can offer new opportunities to obtain advanced microstructures. In this study, dense yttria-stabilized zirconia (YSZ) coatings were deposited using PS-PVD with proper parameters. The dependencies of the microstructure of the as-sprayed coatings on axial spray distance and radial position were discussed. Four typical coatings were selected for the current work. The corresponding microstructures, phase compositions and mechanical properties were studied in detail. These as-sprayed coatings had dense lamellar or lamellar/columnar hybrid microstructures, the lowest porosity was 0.44%. Both monoclinic and tetragonal zirconia were detected in the as-sprayed coatings. The distribution of yttrium was not homogeneous, especially in the coatings deposited at shorter spray distance. Furthermore, oxygen got lost partly during the spraying process with decreasing spray distance. The hardness (H) and Young's modulus (E) of the coatings changed simultaneously with the different microstructures. The maximum values of H and E were 16.6±0.6 and 234.3±10.1 GPa respectively, which were found in the densest coatings. The dense PS-PVD ceramic coatings might be applicable in anti-corrosion fields (such as alkali corrosion, marine corrosion and hot corrosion).     

Structural,mechanical, and in vitro characterization of freeze-cast scaffolds prepared using a sol-gel-derived bioactive glass from the SiO2–CaO–Na2O–P2O5–K2O–MgO system

This work deals with the preparation of freeze-cast scaffolds using a bioactive glass from the SiO₂–CaO–Na₂O–P₂O₅–K₂O–MgO system. This material could be sintered at lower temperatures (650 °C) than other variations of bioactive glasses, which is an important advantage in terms of energy and cost savings. This behavior represents a great advantage in terms of energy and cost savings. The freeze-casting step was conducted using water as a solvent and liquid nitrogen as a coolant. The prepared samples were examined according to their pore structure, thermal behavior, mechanical stability, and bioactivity. The glass transition temperature (T_g), crystallization onset temperature (T_x), and maximum crystallization temperature (T_c) evaluated for this bioactive glass were about 660 °C, 690 °C, and 705 °C. Consequently, the freeze-cast scaffolds could be sintered at 650 °C for 2–8 h, which favored viscous flow sintering without crystallization. Bioactivity assays were conducted by soaking the scaffolds in simulated body fluid for up to 21 days, showing that these materials present a bioactive behavior, inducing hydroxyapatite formation. These materials' mechanical properties and biocompatibility make them promising candidates for use in trabecular bone repair.     

Sintering effect on mechanical properties of composites of natural hydroxyapatites and titanium

This study presents the fabrication and characterization of composite materials of hydroxyapatite and Ti. Hydroxyapatite (HA) powder was obtained from bovine bones (BHA) and human enamel (EHA) via calcination technique. Fine powders of HA were admixed with 5 and 10 wt.% fine powder of metallic Ti. Powder-compacts were sintered at different temperatures between 1000 and 1300 °C. Compression strength, Vickers microhardness and elastic modulus as well as density were measured. SEM and X-ray diffraction studies were also conducted. The experimental results showed that addition of Ti to EHA and BHA decreases the elastic modulus, comparing to samples of pure BHA. The best mechanical properties for BHA–Ti composites were obtained after sintering in the range of 1200–1300 °C and for EHA–Ti composites in the range of 1100–1300 °C.     

Fabrication and microstructure of porous SiC ceramics with Al2O3 and CeO2 as sintering additives

In the present study, porous silicon carbide ceramics were prepared via spark plasma sintering at relatively low temperatures using Al₂O₃ and CeO₂ as sintering additives. Sacrificial template was selected as the pore forming mechanism, and gelcasting was used to fix the slurry in a short time. The evolution process of the microstructures during different steps was observed by SEM. The influence of the sintering temperature and sintering additives on the shrinkage and porosity of the samples was studied. The microstructures of different samples were characterized, and the mechanical properties were also evaluated.     

Effect of the calcination temperature on the composition and microstructure of hydroxyapatite derived from human and animal bone

The present work focus the study of cortical bone samples of different origins (human and animal) subjected to different calcination temperatures (600, 900 and 1200 °C) with regard to their chemical and structural properties. For that, not only standard techniques such as thermogravimetric analysis, Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscopy were used but also mercury intrusion porosimetry. The latter technique was applied to evaluate the effects of the temperature on the microstructure of the calcined samples regarding porosity and pore size distribution.     

Synthesis of nano-sized indium oxide (In2O3) powder by a polymer solution route

Indium oxide (In₂O₃) is a n-type semiconductor with various applications in thin film coatings, on the basis of its optical properties, and in gas sensing equipment, due to its high sensitivity to various oxides such as CO_x and NO_x. In this study, a synthesis process for obtaining In₂O₃ nanoparticles is examined. The precursor used is indium nitrate hydrate (InN₃O₉·H₂O) because of its high solubility in water. By dissolving the nitrate salt in a PVA (polyvinyl alcohol) solution, the precursor is dispersed homogeneously, which reduces the agglomeration of the resulting powder. Calcination at a low temperature of 200–250 °C burns out the organic materials of the PVA with NO_x gas emission and allows the oxidation of the indium, resulting in indium oxide nanoparticles. The influence of the PVA solution characteristics and the heat treatment temperature on the powder morphology and size was analyzed by using SEM, TEM, XRD, TGA/DSC, and four point BET for a specific surface area analysis. The measured specific surface area varies from 3 m²/g to 76 m²/g depending on the calcination temperature, and the particle size of the synthesized powders is under 10 nm for the samples heat treated at 300 °C.     

Microstructural evolution,mechanical and thermal properties of LaB6 embedded in Si-B-C-N prepared by spark plasma sintering

Si-B-C-N monoliths with 5 wt% LaB₆ additives were prepared by spark plasma sintering at 1250–2000 °C and 50 MPa using a mechanically alloyed mixture of graphite, c-Si, h-BN and LaB₆ powders as the starting materials. Microstructural evolution, mechanical and thermal properties of the as-prepared La/Si-B-C-N monoliths were investigated. The densification of the ceramics starts at 1160° and ends at 1800 °C with the formation of La-containing compounds coupled with SiC and BN(C) phases. La-containing BN(C) grains develop into a lamellar structure at 1900 °C offering improved fracture toughness and decreased Vickers hardness, flexural strength and elastic modulus. The formation of lamellar BN(C) is also responsible for a high thermal expansion coefficient of 4.2×10⁻⁶ /°C.     

Effect of porosity on the elastic properties of porcelainized stoneware tiles by a multi-layered model

Porcelainized stoneware represents a leading product in the world market of ceramic tiles, thanks to its relevant bending strength (with respect to other classes of tiles) and extremely low water absorption: these properties derive from its really low content of residual porosity. Nevertheless, an accurate investigation of the cross section of a porcelainized stoneware tile reveals a non-uniform distribution of the residual pores through the thickness, which results in a spatial gradient of properties. Porcelainized stoneware, therefore, may be looked at as a functionally graded material. In the present research, commercial porcelainized stonewares were analysed in order to define the effect of the residual porosity and its spatial distribution on the mechanical properties of tiles. Polished cross sections of porcelainized stoneware tiles were investigated by optical and scanning electron microscopy in order to define the content and distribution of residual pores as a function of distance from the working surface. For each porcelainized stoneware, the local elastic properties of the ceramic matrix were measured by a depth-sensing Vickers micro-indentation technique, then the so-obtained microstructural images and elastic properties were used to model the stoneware tile mechanical properties. In particular, the cross section of each tile was described as a multi-layered system, each layer of which was considered as a composite material formed by a ceramic matrix and residual pores. The elastic properties of each layer were predicted by applying analytical equations derived from the theory of composite materials and, as a new approach, by performing microstructure-based finite element simulations. In order to validate the proposed multi-layered model and identify the most reliable predictive technique, the numerical results were compared with experimental data obtained by a resonance-based method.     

Synthesis and characterization of Si/SiC ceramics prepared using cotton fabric

A Si/SiC ceramic was prepared from cotton fabric by the reactive infiltration of liquid silicon into the carbon template. A large density difference between the samples has been observed. This may be due to the variation in the pore size and its distribution within the sample. Scanning electron microscopy with energy dispersive spectroscopy shows the presence of three distinct phases, i.e., SiC, free Si and free carbon. X-ray diffraction pattern also confirms the presence of SiC and Si phases. However, there is no peak corresponding to carbon. So, it is inferred that the carbon exists in amorphous form. Micro-hardness, fracture toughness and bending strength of the ceramics were also studied. The values are lower than commercially available SiC ceramics. This may be due to the highly porous nature of cotton fabric-based SiC, as compared to commercially available SiC.     

Dispersion studies of La substitution on dielectric and ferroelectric properties of multiferroic BiFeO3 ceramic

Lanthanum La-substituted multiferroic Bi_1−xLa_xFeO₃ ceramics with x = 0.0, 0.05, 0.10, 0.15, 0.20 and 0.25 have been prepared by solution combustion method. The effect of La substitution for the dispersion studies on dielectric and ferroelectric properties of Bi_1−xLa_xFeO₃ samples have been studied by performing x-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), density, dc resistivity and dielectric measurements as well as characterizing the polarization-field hysteresis loop. The results of prepared samples are compared with those of bismuth ferrite (BiFeO₃). In the measuring frequency of 10 KHz to 1 MHz, the dielectric constants and dielectric losses for samples x = 0.20, 0.25 are almost stable and exhibited lowest dielectric loss close to 0.1. The resistivity of Bi_1−xLa_xFeO₃ samples reaches a maximum value of 10⁹ ohm-cm, which is about three times higher than that for pure BiFeO₃. The results also show that stabilization of crystal structure and nonuniformity in spin cycloid structure by La substitution enhances the resistivity, dielectric and ferroelectric properties. Furthermore, the substitution of rare earth La for Bi helps to eliminate the impurity phase in BiFeO₃ ceramic.