In this work, magnetic nanoparticles based on magnetite were successfully prepared via rapid microwave-assisted synthesis. In order to obtain the ternary core–shell Fe3O4/SiO2/TiO2 nanocomposite, first magnetite (Fe3O4) nanoparticles were coated with a protective layer of silica (SiO2) and finally with titania (TiO2). The composite configuration comprising porous and photoactive shells should facilitate the removal of organic micropollutants (OMPs) from water. Furthermore, the magnetic core is critical for processing the management of the photocatalytic powder suspension. The magnetization of the prepared magnetic nanoparticles was confirmed by vibrating-sample magnetometry (VSM), while the structure and morphology of the core–shell nanocomposite were investigated by means of XRD, FTIR, and SEM. Adsorption and photocatalysis were evaluated by investigating the removal efficiency of ciprofloxacin (CIP) as a model OMP using the prepared magnetic core–shell nanocomposite under UV-A light irradiation. It was found that the Fe3O4/SiO2/TiO2 nanocomposite showed good synergistic adsorption and photocatalytic properties. The measurement of iron in eluate confirmed that no leaching occurred during the photocatalytic examination. The recovery of magnetic nanocomposite by an external magnetic field confirmed that the magnetically separated catalyst is highly suitable for recycling and reuse.
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.
In this work, a single-layer TiO2–ZrO2 thin film is deposited on the AISI 316L austenitic stainless steel by the sol–gel process and the dip coating method to improve its corrosion resistance properties. For the sol preparation, titanium isopropoxide and zirconium butoxide are used as the precursors, yttrium acetate hydrate is used for the ZrO2 stabilization, i-propanol as the solvent, nitric acid as the catalyst, acetylacetone as the chelating agent, and the distilled water for the hydrolysis. The deposited films are annealed at 400 °C or 600 °C. Morphology and phase composition of the sol–gel TiO2–ZrO2 films and powders are analyzed by scanning electron microscopy (SEM) equipped with EDX detector and X-ray diffraction (XRD), respectively. The thickness of the sol–gel TiO2–ZrO2 films deposited on the stainless steel is determined by glow discharge optical emission spectrometry (GD-OES). The corrosion behavior of the stainless steel, coated by amorphous films, is evaluated in 3 wt% NaCl and 0.5 mol dm−3 HCl by potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. It is found that the sol–gel TiO2–ZrO2 films with the amorphous structure, deposited by the sol–gel process, and calcined at 400 °C significantly enhance the corrosion properties of AISI 316L in both chloride media.
The goal of this study is to compare the properties of cold isostatically pressed (CIP) alumina (A2O3) samples sintered by conventional (electrical) and nonconventional (hybrid microwave) techniques. X-ray diffraction was used to determine phase composition of A2O3 samples (raw powder and granules). Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were used to investigate the thermal behaviour of the Al2O3 powder and granules during the thermal treatment. Compaction of spray dried A2O3 granules into green compact bodies was performed by CIP, followed by sintering of green bodies at 1600 °C in an electrical and hybrid microwave kiln, respectively. Scanning electron microscopy (SEM) was used to analyse morphology of the Al2O3 granules and fracture surface of Al2O3 compacts derived by both sintering techniques. Higher linear shrinkage and densification were obtained for alumina samples sintered in electrical kiln (conventional method), while sintering by faster and more energy efficient hybrid microwave kiln (non-conventional sintering method) yielded alumina samples with finer grain size. Alumina samples sintered by electrical kiln displayed higher relative densities and lower porosities.
Porous ceramics can be used in various industrial applications, such as thermal insulation, orthopedic implants, high-temperature filtration, lightweight structural components, and catalyst supports, etc., and can be obtained using various methods. In this study, the sacrificial fugitive method was used to prepare a porous alumina ceramic. The appropriate amount of sacrificial fugitive was combined with raw ceramic powder as a pore-forming agent, and was then evaporated or burned out either before or during the sintering process to create the desired pores. Various materials can be used as pore-forming agents; in this work, eco-friendly waste coffee grounds (WCG) were utilized. First, alumina ceramic green bodies were prepared via slip casting of 60 wt. % alumina suspensions with five different amounts of WCG (0 wt. %, 1 wt. %, 5 wt. %, 10 wt. % and 15 wt. %) and the dispersant Dolapix (0.2 wt. %), and using PVA (0.5 wt. %) as a binder for all solutions. The effect of the various amounts of WCG on the alumina ceramic green bodies, and subsequently on the obtained sintered ceramics, was tracked and validated through different analyses. Suspension viscosity was determined through a rotational viscometer. Simultaneous differential thermal and thermogravimetric (DTA/TGA) analyses were used to observe the thermal decomposition of WCG and to determine the sintering regime. After sintering, the density, porosity, and shrinkage of the samples were examined and calculated. In addition, the phase composition and crystallite size of all sintered samples were determined by powder X-ray diffraction (PXRD) analysis, as well as their morphology and composition using Scanning Electron Microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS). The results show that density decreased from 3.743 to 2.172 g/cm3 and porosity increased from 6.12% to 45.52%, both with the increasing amount of WCG (from 0 wt. % to 15 wt. %).
The volume erosion rate of the slip cast monolithic and composite ceramics was studied using SiO 2 and SiC particles as erodents, under different impact angles (30°, 60°, 90°), at room temperature. Therefore, three groups of samples were prepared: (i) monolithic alumina (Al 2 O 3 ); (ii) composite alumina-zirconia (Al 2 O 3 -ZrO 2 ) containing 99 wt-% Al 2 O 3 and 1 wt-% ZrO 2 and (iii) composite alumina-zirconia (Al 2 O 3 -ZrO 2 ) containing 90 wt-% Al 2 O 3 and 10 wt-% ZrO 2 . Erosion mechanisms of all prepared ceramic samples were evaluated by the volume erosion rate (v, mm 3 •g -1 ). Obtained results were compared with the analytical Wiederhorn and Evans equations. The mechanical properties (hardness and fracture toughness) of prepared ceramic samples were compared with their v under the above-mentioned conditions. It was found that the erosion of monolithic and composite ceramics increased with the increase of the impact angle. Volume erosion rate was highest at an impact angle of 90°and amounts to 115 mm 3 •g -1 with SiC, and 12 mm 3 •g -1 with SiO 2 erodent particles for monolithic alumina ceramics, 77 mm 3 •g -1 with SiC, and 8 mm 3 •g -1 with SiO 2 erodent particles for ceramics with the addition of 1 wt-% of ZrO 2 , and 61 mm 3 •g -1 with SiC, and 7 mm 3 •g -1 with SiO 2 erodent particles for ceramics with the addition of 10 wt-% of ZrO 2 . Therefore, it can be concluded that the erosion resistance of monolithic Al 2 O 3 increases with the increasing amount of ZrO 2 in the composite Al 2 O 3 -ZrO 2 ceramics, thus erosion resistance can be improved with the addition of ZrO 2 .
The goal of this research is the statistical optimisation of the chemical stability of hybrid microwave-sintered alumina ceramics in nitric acid. The chemical stability of ceramic materials in corrosive media depends on many parameters, such as the chemical and phase composition of the ceramics, the properties of the aggressive medium (concentration, temperature, and pressure), and the exposure time. Therefore, the chemical stability of alumina ceramics in different aqueous nitric acid solution concentrations (0.50 mol dm−3, 1.25 mol dm−3, and 2.00 mol dm−3), different exposure times (up to 10 days), as well as different temperatures (25, 40, and 55 °C), was investigated, modelled, and optimised. The chemical stability of high purity alumina ceramics (99.8345 wt.% of Al2O3) was determined by measuring the amount of eluted ions (Al3+, Ca2+, Fe3+, Mg2+, Na+, and Si4+) obtained by inductively coupled plasma atomic emission spectrometry. The changes in the density of alumina ceramics during the chemical stability monitoring were also determined. The Box–Behnken approach was employed to reach the optimum conditions for obtaining the highest possible chemical stability of alumina at a given temperature range, exposure time, and molar concentration of nitric acid. It was found that an increase in exposure time, temperature, and nitric acid concentration led to an increase in the elution of ions from hybrid microwave-sintered alumina. Higher amounts of eluted ions, Al3+ (14.805 µg cm−2), Ca2+ (7.079 µg cm−2), Fe3+ (0.361 µg cm−2), Mg2+ (3.654 µg cm−2), and Na+ ions (13.261 µg cm−2), were obtained at 55 °C in the 2 mol dm− 3 nitric acid. The amount of eluted Si4+ ions is below the detection limit of inductively coupled plasma atomic emission spectrometry. The change in the alumina ceramic density during the corrosion test was negligible.
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