Heat treatment-improved bond strength of resin cement to lithium disilicate dental glass-ceramic

This study investigated the influence of different hydrofluoric acid (HF) concentrations and heat treatments applied to a lithium disilicate dental glass-ceramic (EMX) on surface morphology and micro-shear bond strength (μSBS) to resin cement. Five HF concentrations (1%, 2.5%, 5%, 7.5% and 10%) and four different heat treatments applied before etching were assessed: 1. etching at room temperature with no previous heat treatment (control group); 2. HF stored at 70 °C for 1 min applied to the ceramic surface at room temperature; 3. HF at room temperature applied after a hot air stream is applied perpendicularly to the ceramic surface for 1 min; 4. the combination of previously heated HF and heated EMX surface. The etching time was fixed for 20 s for all groups. Etched EMX specimens were analyzed on field-emission scanning electron microscope (FE-SEM) and the μSBS was carried out on a universal testing machine at a crosshead speed of 1 mm/min until fracture. For the control groups, FE-SEM images showed greater glassy matrix dissolution and higher μSBS for 7.5% and 10% HF concentrations. The previous heat treatments enhanced the glassy matrix dissolution more evidently for 1%, 2.5% and 5% and yielded increased μSBS values, which were not statistically different for 7.5% and 10% HF concentrations (control group). HF concentrations and previous heat treatments did show to have an influence on the etching/bonding characteristics to lithium disilicate dental glass-ceramic.     

Effect of TiO2 doping on the characteristics of macroporous Al2O3/TiO2 membrane supports

A cost-effective tubular macroporous ceramic support consisting of alumina and titania was prepared by extrusion and subsequent heat treatment. An Al₂O₃/TiO₂ composite support with high porosity (41.4%), an average pore size of 6.8 μm and sufficient mechanical strength (32.7 MPa) was obtained after sintering at 1400 °C. The formation mechanism of this support as investigated with X-ray micromapping, SEM and XRD indicated that the appearance of Al₂TiO₅ plays a key role in the fabrication of high performance composite membrane supports at relatively low temperature. The amount of Al₂TiO₅ present in the composite has a strong impact on the properties of supports, especially with regard to the mechanical strength. A composite of 85 wt.% Al₂O₃/15 wt.% TiO₂ sintered at 1400 °C for 2 h exhibited both high permeability (pure water flux of 45 m³ m^?2 h^?1 bar^?1), together with an excellent corrosive resistance towards hot NaOH and HNO₃ solutions.     

Optical and mechanical properties of cocona chips as affected by the drying process

The effect of the application of a pre-osmotic treatment to obtain hot air dried cocona (Solanum sessiliofurum Dunal) chips was studied. The drying kinetics and the optical and mechanical properties of cocona chips obtained by the combined method of osmotic dehydration and hot air drying (OD + HAD) and by only hot air drying (HAD) were compared. Samples were dried by hot air at 60 °C. For the combined method, they were pre-dried to a moisture content of 75 g_water/100 g, immersed in a 55 °Brix sucrose solution at 25 °C for 48 min. The pre-osmodehydration applied did not influence the subsequent hot air drying kinetics, resulting in a final product with 0.055 ± 0.005 g_water/g_cocona. The optical properties of OD + HAD chips were more favorable, exhibiting a smaller color change with respect to the fresh fruit (±15 units) than the HAD samples (±23 units). On the other hand, the OD + HAD chips presented more fracture peaks than HAD ones, this related with a structure with a higher degree of crispness, a very desirable property for a chip product.     

Significance of hot pressing parameters and reinforcement size on sinterability and mechanical properties of ZrB2–25 vol% SiC UHTCs

The influences of hot pressing parameters and SiC particle size on the bulk density, the average ZrB₂ grain size and Vickers hardness of ZrB₂–25 vol% SiC ultrahigh temperature ceramic composites were investigated. In this paper, the Taguchi methodology (An L9 orthogonal array) was used to specify the contributions of four parameters: the hot pressing temperature, holding time, applied pressure and SiC particle size. The experimental procedure included nine tests for four parameters with three levels which were employed to optimize the process parameters. The statistical analyses recognized the hot pressing pressure and temperature as the most consequential parameters affecting the density and hardness of ZrB₂–SiC composites. The SiC particle size and holding time were specified as the most effective parameters on the average ZrB₂ grain size. The bulk density, average ZrB₂ grain size, Vickers hardness and fracture toughness of the sample, hot pressed at optimal conditions (1850 °C, 90 min, 16 MPa and 200 nm), reached about 5.36 g/cm³, 10.03 µm, ~17.1 GPa and 5.9 MPa m^1/2, respectively. The confirmation test, carried out under optimum conditions, showed that the experimental results were relatively equal to the predicted values from the Taguchi prediction model. Finally, the mechanisms of enhanced fracture toughness of the hot pressed ZrB₂–SiC ceramic composites were discussed.     

Continuous synthesis of fine MgFe2O4 nanoparticles by supercritical hydrothermal reaction

We produced magnesium ferrite (MgFe₂O₄) nanoparticles by hydrothermal synthesis in supercritical water. Suspensions containing varying ratios of Mg(OH)₂ and Fe(OH)₃ at room temperature were pressurized to 30 MPa, fed into a tubular reactor by high-pressure pump, and rapidly heated to reaction temperature by mixing with supercritical water. The MgFe₂O₄ phase forms at 460 °C. The Mg/Fe molar ratio was varied from 0.5 to 1.5 with the goal of obtaining single-phase MgFe₂O₄. At the stoichiometric ratio for MgFe₂O₄, Mg/Fe = 0.5, the product contains both MgFe₂O₄ and α-Fe₂O₃. At Mg/Fe = 1.0 and 1.5, the product is the desired single-phase MgFe₂O₄. The synthesized MgFe₂O₄ nanoparticles, with particle size of about 20 nm, exhibit superparamagnetic behavior.     

Evaluation of water treatment sludge as a catalyst for aqueous ozone decomposition

A new, novel, efficient, and stable green catalyst has been successfully used as a catalyst in aqueous ozone decomposition in acidic medium. The catalyst was characterized by using X-ray fluorescence (XRF), transmission electron microscope (TEM), scanning electron microscope (SEM), and X-ray diffraction (XRD) techniques. The sludge mainly consists of various metal and non-metal oxides. The effect of various experimental parameters such as catalyst loading, initial ozone concentrations, and various metal oxide catalysts on the decomposition of ozone was investigated. The decomposition of dissolved ozone was substantially enhanced by increasing the catalyst loading from 125 to 750 mg and by increasing the initial ozone concentration. The ozone decomposition efficiencies of Al₂O₃, SiO₂, TiO₂, Fe₂O₃, ZnO, and sludge have been studied and the efficiencies of these catalysts were found to be in the following order: ZnO ≈ sludge > TiO₂ > SiO₂ > Al₂O₃ ≈ Fe₂O₃. The catalytic stability was also investigated for up to four successive cycles and it was found that the catalyst was stable and ozone did not affect the catalyst morphology and its composition. However, the surface area of the catalyst increased after 1st cycle then it became stable. It was concluded that the sludge powder used in this study was a promising catalyst for aqueous ozone decomposition.     

Temperature dependent hardness and strength properties of TiB2 with TiSi2 sinter-aid

From the perspective of high temperature structural applications, it is important to evaluate temperature dependent mechanical properties of titanium diboride (TiB₂) ceramics. The present study reports the effect of TiSi₂ content (up to 10 wt.%) and temperature on hardness and strength of TiB₂. The hardness properties were measured from room temperature (RT)—900 °C in vacuum; the four-point flexural strength properties were evaluated at selected temperatures in air up to 1000 °C. An attempt has been made to discuss the difference in hardness and strength properties with sinter-aid amount and microstructure. Our experimental results clearly indicated that the addition of 2.5 wt.% TiSi₂ to TiB₂ resulted almost full densification at a lower hot pressing temperature of 1650 °C without compromising on the high temperature strength and hardness properties. The hot pressed TiB₂–2.5 wt.% TiSi₂ ceramic could retain moderate strength of more than 400 MPa and hardness of 9 GPa at 1000 °C and 900 °C, respectively.     

Ammonium oxidization at room temperature and plasmonic photocatalytic enhancement

In an alkaline condition, ammonium can be efficiently reduced with hydroxide ion using a spinning disk reactor at room temperature. To some extent, illumination can boost the processing efficiency by warming water. A homogeneous 8 nm crystallized platinum thin film deposited on a B270-glass substrate by plasma-enhanced atomic layer deposition absorbs light from 350 nm to 2500 nm. The absorbed light transforms plasmonic resonance energy on the platinum thin film and forms a high temperature hot layer. The plasmonic heating effect, or plasmonic photocatalytic reaction, enhances the activity of the Pt thin film for the oxidation of NH₄⁺.     

Structural and magnetic properties of the copper ferrite obtained by reactive milling and heat treatment

Copper ferrite (CuFe₂O₄) was synthesised from an equimolar mixture of copper and iron oxides by mechanosynthesis and subsequent heat treatment. After mechanosynthesis, depending on the milling time, the powder consists in a mixture of phases. The heat treatment at 600 °C did not lead to a complete reaction of the mechano-activated precursors. After the heat treatments at 800 and 1000 °C, the complete formation of copper ferrite for almost all the milling times was noticed. The crystal structure of the copper ferrite was found to be cubic for all the samples heat treated at 1000 °C and a mixture of tetragonal and cubic for the samples heat treated at 800 °C. The amount of copper ferrite with cubic structure predominates in the samples with prolonged milling duration and a decrease of the tetragonal distortion by increasing the milling time occurs. The crystallisation of CuFe₂O₄ in cubic structure for the samples milled for prolonged time is influenced by the powder contamination with iron. The magnetisations of the samples obtained after heat treatment at 1000 °C were found to be larger compared to the ones of the samples heat treated at 800 °C. The iron contamination, milling duration and heat treatment temperature influence the cations distribution, thus leading to the saturation magnetisation of the copper ferrite samples ranging from 11.9 μ_B/f.u. to 16.4 μ_B/f.u.     

Tailoring of morphology and orientation of LaNiO3 films from polymeric precursors

The aim of this work was to prepare lanthanum nickel oxide (LaNiO₃, LNO) thin films of different morphology and orientation. The precursor solutions were prepared by a chemical method from citric salts of lanthanum and nickel. Films were deposited using spin-on technique on Si (1 0 0) substrates. Tailoring of the films orientation and morphology has been attained through two thermal treatment processes with different heating devices: tubular furnace (process 1) and hot plate (process 2). Films were annealed at 600 and 700 °C, with heating rates: 20 °C/min (process 1) and 1 °C/min (process 2). Annealing times were from 30 min to 20 h. LNO films were characterized by AFM and X-ray diffraction analysis. Depending on the heating process applied, the obtained films showed very different structures, from completely amorphous to well crystallized and highly oriented. Films treated by process 1 were polycrystalline, had smaller oval grains and lower roughness parameters than films heated on a hot plate. Due to the low heating rate and heating from the substrate side, films obtained through process 2 were highly (1 1 0) oriented with elongated grains aligned along one direction.     

Heat conduction mechanisms in hot pressed ZrB2 and ZrB2–SiC composites

Thermal diffusivity and conductivity of hot pressed ZrB₂ with different amounts of B₄C (0–5 wt%) and ZrB₂–SiC composites (10–30 vol% SiC) were investigated experimentally over a wide range of temperature (25–1500 °C). Both thermal diffusivity and thermal conductivity were found to decrease with increase in temperature for all the hot pressed ZrB₂ and ZrB₂–SiC composites. At around 200 °C, thermal conductivity of ZrB₂–SiC composites was found to be composition independent. Thermal conductivity of ZrB₂–SiC composites was also correlated with theoretical predictions of the Maxwell–Eucken relation. The dominated mechanisms of heat transport for all hot pressed ZrB₂ and ZrB₂–SiC composites at room temperature were confirmed by Wiedemann–Franz analysis by using measured electrical conductivity of these materials at room temperature. It was found that electronic thermal conductivity dominated for all monolithic ZrB₂ whereas the phonon contribution to thermal conductivity increased with SiC contents for ZrB₂–SiC composites.     

Synergetic effects of SiC and Csf in ZrB2-based ceramic composites. Part I: Densification behavior

The effects of processing variables on densification behavior of hot pressed ZrB₂-based composites, reinforced with SiC particles and short carbon fibers (C_sf), were studied. A design of experiment approach, Taguchi methodology, was used to investigate the characteristics of ZrB₂–SiC–C_sf composites concentrated upon the hot pressing parameters (sintering temperature, dwell time and applied pressure) as well as the composition (vol% SiC/vol% C_sf). The analysis of variance recognized the sintering temperature and SiC/C_sf ratio as the most effective variables on the relative density of hot pressed composites. The microstructural investigations showed that C_sf can act as a sintering aid and eliminate the oxide impurities (e.g. B₂O₃, ZrO₂ and SiO₂) from the surfaces of raw materials. A fully dense composite was achieved by adding 10 vol% C_sf and 20 vol% SiC to the ZrB₂ matrix via hot pressing at 1850 °C for 30 min under a pressure of 16 MPa. Moreover, the in-situ formation of interfacial ZrC, which also improves the sinterability of ZrB₂-based composites, was studied by energy-dispersive X-ray spectroscopy analysis and verified thermodynamically.     

Synergetic effects of SiC and Csf in ZrB2-based ceramic composites. Part II: Grain growth

The synergetic effects SiC particles and short carbon fibers (C_sf) as well as hot pressing parameters (sintering temperature, dwell time and applied pressure) on the grain growth of ZrB₂-based composites were investigated. Taguchi methodology was employed for the design of experiments to study the microstructure and grain growth of ZrB₂–SiC–C_sf ceramic composites. Three hot pressing parameters and SiC/C_sf ratio were selected as the scrutinized variables. The sintering temperature and SiC/C_sf ratio were identified by ANOVA as the most effective variables on the gain growth of ZrB₂-based samples. Removal of oxide impurities from the surface of starting particles by the reactant C_sf, not only hindered the extraordinary grain growth of ZrB₂ matrix, but also improved the sinterability of the ceramics. A fully dense ceramic with an average grain size of 8.3 µm was obtained by hot pressing at 1850 °C for 30 min under 16 MPa through adding 20 vol% SiC and 10 vol% C_sf to the ZrB₂ matrix. SEM observations and EDS analysis verified the in-situ formation of ZrC which can restrain the growth of ZrB₂ particles, similar to the role of SiC, by the pinning of grain boundaries as another stationary secondary phase.     

Synthesis of nanosized zirconium carbide by a sol–gel route

Nanosized zirconium carbide was synthesized by a new simple sol–gel method using zirconium n-propoxide, acetic acid as chemical modifier, and saccharose as carbon source. When heat-treated at 900 °C under flowing argon, gels transformed into intimately mixed amorphous carbon and nanosized tetragonal ZrO₂. Further heat treatments above 1200 °C led to the formation of zirconium carbide with some dissolved oxygen in the lattice. Oxygen content could be reduced by increasing the heat treatment temperature from 1400 to 1600 °C, which unfortunately also induced a mean crystallites size increase from 90 to 150 nm. Short heat treatments above 1600 °C were carried out to further purify the samples and to limit the particles growth. A compromise between purity and average crystallite's size could then be found. Powders were assessed using X-ray diffraction, thermal analysis and scanning electron microscopy.     

Macro-porous ceramic supports for membranes prepared from quartz sand and calcite mixtures

A new type of porous ceramic supports for membranes has been designed. The new supports have been fabricated from polycrystalline quartz sand and calcite raw materials. In this work, two configurations of support (tubular and flat) have been produced using extrusion method. The open porosity, the pore size distribution, the average pore size (APS), the strength and the permeability of sintered supports have been found to depend mainly on the weight ratio of calcite (CaCO₃) additive. The results showed that with the addition of 15–35 wt.% of calcite and sintering temperature of about 1375 °C for 1 h the best characteristics of sintered supports could be obtained. The developed tubular ceramic supports with the APS 6.3–12 μm, open porosity 42–55%, the water permeability (16–68 m³/h m² bar) and flexural strength 8–18 MPa hopefully offer many perspectives for a wide use in membranes technology.     

Investigations of effect of radial flow impeller type swirl generator fitted in an electronic heat sink and Al2O3/water nanofluid on heat transfer enhancement

In this paper experimental investigations on convective heat transfer and pressure drop characteristics in a novel electronic heat sink fitted with dynamic mixers using water and Al₂O₃/water nanofluid are presented. For this, Al₂O₃ nanoparticles of average size 47 nm are synthesized using microwave assisted chemical precipitation method and characterized using XRD and SEM. Heat transfer and pressure drop characteristics of water and nanofluid are studied in the electronic heat sink of base size 60 mm × 60 mm made of copper with and without the dynamic mixer. The enhancements in the heat transfer and pressure drop results are compared with water and the heat sink without any mixer. The results reveal that there is significant increase in the convective heat transfer when the dynamic mixer is used for enhancing the heat transfer and further increase in heat transfer is found for the nanofluid. The rise in pressure drop compared with the increase of heat transfer is less.     

Effect of spinel content on hot strength of alumina-spinel castables in the temperature range 1000–1500°C

Hot modulus of rupture of Al₂O₃-spinel castables containing 5–15 wt% alumina-rich magnesia alumina spinel and 1·7 wt% CaO generally increases with increase in spinel content and temperature from 1000 to 1500°C. The magnitudes of hot modulus of rupture of castables containing 15 wt% spinel and 1·7 wt% CaO are 14·3 MPa at 1400°C and 15·6 MPa at 1500°C, while those of castables containing 20 wt% spinel and 1·7 wt% CaO are 12·5 MPa at 1400°C and 14·7 MPa at 1500°C. The former castables contained 15 wt% spinel of −75 μm size, while the latter contained 10 wt% spinel of +75 μm size and another 10 wt% spinel of −75 μm size. The bond linkage between the CA₆ and spinel grains in the matrix is believed to cause both the spinel content and temperature dependence of hot strength of Al₂O₃-spinel castables, as well as fine grain spinel even in amount less than coarser grain spinel to be more effective for enhancing hot strength. The trend of the magnitude of thermal expansion under load (0·2 MPa) above 1500°C of the castables is not necessarily indicative of the magnitude of hot modulus of rupture at 1400 or 1500°C. ©     

Oxygen permeation properties of BSCF5582 tubular membrane fabricated by the slip casting method

BSCF5582 tubular oxygen separation membranes were prepared using the most cost effective slip casting techniques. The optimum slurry composition was identified and a dense, and crack free 60 mm long BSCF5582 tubular membrane being successfully prepared after the programmed sintering process. The effects of the feed flow rate and the sweeping flow rate on the oxygen permeation flux of the tubular BSCF5582 membrane were investigated. The oxygen permeation flux increased with an increase of the oxygen chemical potential gradient to a maximum of 42.5 cm³/min in an O₂/N₂ condition at 1223 K for the 1.5 mm thick, 60 mm long BSCF tube, a value which corresponds to 1.42 cm³/min cm². The ionic conductivity of the oxygen was successfully calculated in the dominant electron conducting regime. The ionic conductivity was found to increase with an increase of the temperature to 900 °C, indicating that it is a thermally activated process with an activation energy of 0.70 ± 0.1 eV in an air environment.     

Hydrogen production from glycerol by reforming in supercritical water over Ru/Al2O3 catalyst

Supercritical water is a promising medium for the reforming of hydrocarbons and alcohols for the production of hydrogen at high pressures in a short reaction time. Water serves both as a dense solvent as well as a reactant. In this work, hydrogen is produced from glycerol by supercritical water reforming over a Ru/Al₂O₃ catalyst with low methane and carbon monoxide formation. Experiments were conducted in a tubular fixed-bed flow reactor over a temperature range of 700–800 °C, feed concentrations up to 40 wt% glycerol, all at short reaction time of less than 5 s. Glycerol was completely gasified to hydrogen, carbon dioxide, and methane along with small amounts of carbon monoxide. At dilute feed concentrations, near-theoretical yield of 7 mol of hydrogen/mol of glycerol was obtained, which decreases with an increase in the feed concentration. Based on a kinetic model for glycerol reforming, an activation energy of 55.9 kJ/mol was observed.     

Reclamation of used SiC grinding powder and its sintering characteristics

A process of recycling used abrasive SiC powder after grinding Si wafer was proposed to raw powder for sintering. The used SiC powder could be successfully converted to composite powders consisting of SiC particle and Si₃N₄ whisker via a heat treatment in N₂ atmosphere, in which iron oxide acted as a catalyst in the vapor–liquid–solid (VLS) formation of Si₃N₄. With the addition of 3 mass% Al₂O₃ and 1 mass% Y₂O₃, the composite powders sintered at 1900 °C for 2 h exhibited a 3-point bending strength of 626 ± 48 MPa and a fracture toughness of 3.9 ± 0.1 MPa m^1/2, which were significantly enhanced as compared with those of using recovered powder merely composed of SiC particle. The strength and fracture toughness of the sintered material could be improved by optimization of chemical and heat treatment parameters and controlling the amount of sintering additives and hot pressing conditions.