Alumina (Al2O3) and zirconia (ZrO2) have good overall properties and thus are widely used oxide technical ceramics. The biggest drawback of Al2O3 is its low fracture toughness. In contrast, ZrO2 is relatively tough, but is also much more expensive. In order to improve the alumina toughness, composite ceramics are being developed. Slip casting technology has economic advantages over the conventional hot isostatic pressure technology, but problems may arise when preparing stable highly-concentrated suspensions (slip) for filling the mold. The purpose of this study is to prepare aqueous suspensions using 70 wt. % α-Al2O3, with 0, 1, 5 and 10 wt. % of added t-ZrO2. Suspensions were electrosterically stabilized using the ammonium salt of polymethylacrylic acid, an alkali-free anionic polyelectrolyte dispersant. Also, magnesium oxide in form of magnesium aluminate spinel (MgAl2O4) was used to inhibit the abnormal alumina grain growth during the sintering process. Minimum viscosities were used as stability estimators, where an increase in ZrO2 content required adding more dispersant. After sintering, the Vickers indentation test was used to determine the hardness and the indentation fracture toughness from the measurement of the crack length. Also, the brittleness index (Bi, μm−1/2) was calculated from values of Vickers hardness and the Vickers indentation fracture toughness. It was found that with increasing ZrO2 content the fracture toughness increased, while the hardness as well as the brittleness index decreased. Zirconia loading reduces the crystallite sizes of alumina, as confirmed by the X-ray diffraction analysis. SEM/EDS analysis showed that ZrO2 grains are distributed in the Al2O3 matrix, forming some agglomerates of ZrO2 and some pores, with ZrO2 having a smaller grain size than Al2O3.
In the present work, alumina (Al2O3) foam was prepared by the replica method where a polyurethane (PU) foam (30 pores per inch (ppi)) template was impregnated with a 60 wt.% Al2O3 suspension. Sintered Al2O3 foam was used as substrate for the deposition of sol-gel derived titania (TiO2) film using dip coating. For the preparation of TiO2 sol, titanium(IV) isopropoxide (Ti-iPrOH) was used as the precursor. The common problem of qualification and quantification of a crystalline coating on a highly porous 3D substrate with an uneven surface was addressed using a combination of different structural characterization methods. Using Powder X-ray Diffraction (PXRD) and synchrotron Grazing Incidence X-ray Diffraction (GIXRD) on bulk and powdered Al2O3 foam and TiO2-coated Al2O3 foam samples, it was determined Al2O3 foam crystallizes to corundum and coating to anatase, which was also confirmed by Fourier Transformed Infrared Spectroscopy (FTIR). Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM/EDS) revealed the structural and microstructural properties of the substrate and coating. Differential Thermal Analysis (DTA) and Thermogravimetric Analysis (TGA) were used to clarify the evolution of the porous microstructure. The Al2O3-TiO2 composite was evaluated as a photocatalyst candidate for the degradation of the micropollutant medication memantine. The degradation rate was monitored using a light-emitting diode (LED) lamp operating at electromagnetic (EM) wavelength of 365 nm. The photocatalytic activity of sol-gel-derived TiO2 film immobilized on the Al2O3 foam was compared with commercially available TiO2 nanoparticles, P25-Degussa, in the form of a suspension. The levels of memantine were monitored by High-Performance Liquid Chromatography–Tandem Mass Spectrometry (HPLC–MS/MS). The efficiency and rate of the memantine photodegradation by suspended TiO2 nanoparticles is higher than the TiO2-coated Al2O3 foam. But, from the practical point of view, TiO2-coated Al2O3 foam is more appropriate as a valuable photocatalytic composite material.
The present study examines the potential of microwave heating as an emerging and innovative energy-efficient alternative to conventional heating techniques used for different materials, with a focus on the processing of ceramic materials. Modern ceramics are studied extensively, and their use and different applications are wide due to many advantages of these materials. The most important factor in microwave sintering which differentiates it from conventional heating techniques is a unique heat transfer mechanism. Microwave energy is absorbed by the material, hence the transfer of energy takes place at the molecular level. This way, the heat is generated throughout the material, i.e. on the inside as well on the outside. This allows a very low temperature gradient throughout the material cross section. When conventional sintering is used, typically at high heating rates, high temperature gradients pose a problem. The accelerated microwave heating occurs through the whole volume, so the heating is uniform, which limits the grain growth and coarsening, and leads to a uniform and fine microstructure. The densification is accelerated as well during the unique heat transfer mechanism of microwave sintering, which enhances the mechanical properties of the sintered materials.This paper discusses the use of microwave sintering in the manufacturing of different modern technical materials, namely ceramics, composites, metals and alloys, and glasses. The improvement of different properties is described using the available literature.
In this work, alumina (Al2O3) ceramics were prepared using an environmentally friendly slip casting method. To this end, highly concentrated (70 wt.%) aqueous suspensions of alumina (Al2O3) were prepared with different amounts of the ammonium salt of a polycarboxylic acid, Dolapix CE 64, as an electrosteric dispersant. The stability of highly concentrated Al2O3 aqueous suspensions was monitored by viscosity measurements. Green bodies (ceramics before sintering) were obtained by pouring the stable Al2O3 aqueous suspensions into dry porous plaster molds. The obtained Al2O3 ceramic green bodies were sintered in the electric furnace. Analysis of the effect of three sintering parameters (sintering temperature, heating rate and holding time) on the density of alumina ceramics was performed using the response surface methodology (RSM), based on experimental data obtained according to Box–Behnken experimental design, using the software Design-Expert. From the statistical analysis, linear and nonlinear models with added first-order interaction were developed for prediction and optimization of density-dependent variables: sintering temperature, heating rate and holding time.
The green machining of alumina (Al2O3) green bodies generates a certain amount of waste alumina powder. Waste alumina ceramic powder should be disposed of as non-hazardous waste in a legally compliant manner. The influence of additives on the stability of 70 wt.% (≈40 vol.%) alumina—waste alumina water-based suspension was investigated in the presented research. A Box-Behnken three-factor response surface design was used for the preparation of stable highly-concentrated suspensions with the addition of three additives. The optimal amount of each additive was selected according to the obtained results of minimal apparent viscosity: 0.05 wt.% Tiron as dispersant, 0.1 wt.% poly (vinyl alcohol) as binder and 0.2 wt.% magnesium aluminate spinel as abnormal grain growth inhibitor. The analysis of variance was used to identify the contribution of each additive. The zeta potential and sedimentations tests were performed to confirm the suspension stability measurements at different pH values. Alumina particles were optimally dispersed at pH values between 8 and 11. According to the results, the investigated composition of 20 wt.% waste alumina powder (weight content, dry alumina powder), with the addition of optimal amounts of additives, shows a possible application in the production of ceramics by slip casting.
Slip casting is a widely used colloidal technique for consolidation of ceramic powders from a suspension. The colloidal approach ensures homogeneous microstructure of a green body, thereby reducing post-sintering machining and production costs. The process consists of several steps. The first step is to mix the ceramic powder with a liquid, usually water, where the stabilization of the new obtained suspension with different dispersants follows. When an optimum dispersion of particles is achieved, resulting in low slip viscosity, ceramic slurry can finally be poured into a porous mould, usually a gypsum one. The influence of different dispersants on rheological properties of highly concentrated alumina (Al 2 O 3) suspensions was investigated. The used dispersants were: ammonium polymethacrylate water solution (Darvan C-N), 4,5-dihydroxy-1,3-benzenedisulfonic acid disodium salt (Tiron) and citric acid. The amount of dispersants was varied from 0.1-1.25 wt. % in order to determine the optimum. Rheological properties of the prepared suspensions were determined by measuring the apparent viscosity at different shear rates. The obtained optimal amount was 0.75 wt. % for Darvan, 0.1 wt. % for Tiron and 0.3 wt. % for citric acid. The obtained results show that the most effective dispersant is 4,5-dihydroxy-1,3benzenedisulfonic acid disodium salt, given that only 0.1 wt. % was required to stabilize the 70 wt. % Al 2 O 3 suspension.
In the present study a biowaste, in the form of chicken eggshells, is used for producing a biomaterial – hydroxyapatite by a conventional chemical precipitation method. Hydroxyapatite is a major component of human hard tissues, such as bones and teeth, which makes it a paradigmatic bioactive material. The first step in the synthesis of hydroxyapatite from eggshells is the transformation of their main component calcium carbonate into calcium oxide at 1000 °C. Afterwards, calcium oxide is hydrated in order to produce calcium hydroxide. Hydroxyapatite is then synthesized by the addition of the phosphoric acid. The phase composition of the eggshells is examined by the powder X‐ray diffraction. The surface morphology of the sintered product is determined by the scanning electron microscope equipped with the energy dispersive spectrometer. Powder X‐ray diffraction and scanning electron microscope analyses confirmed hydroxyapatite as the main phase of the final product. The reuse of chicken eggshells reduces the amount of biowaste, as well as the need for the biowaste management. This investigation shows that the eggshells can be a useful raw material for the synthesis of valuable biomaterials.
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