Effect of microwave sintering on the properties of copper oxide doped Y-TZP ceramics

The effect of various amounts of copper oxide (CuO) up to 1?wt% on the densification behaviour and mechanical properties of 3?mol% yttria-tetragonal zirconia polycrystal (Y-TZP) were studied by using microwave (MW) sintering method. The MW sintering was performed at temperatures between 1100?°C and 1400?°C, with a heating rate of 30?°C/min. and holding time of 5?min. The beneficial effect of MW in enhancing densification was also compared for the undoped and 0.2?wt% CuO-doped Y-TZP when subjected to conventional sintering (CS) method. The results showed that significant enhancement in the relative density and Vickers hardness were observed for the undoped Y-TZP when MW-sintered between 1100?°C and 1250?°C. It was revealed that the 0.2?wt% CuO-doped Y-TZP and MW sintered at 1250–1300?°C could attain ≥?99.8% of theoretical density, Vickers hardness of about 14.4?GPa, fracture toughness of 7.8 MPam^1/2 and exhibited fine equiaxed tetragonal grain size of below 0.25?µm. In contrast, the addition of 1?wt% CuO was detrimental and the samples exhibited about 50% monoclinic phase upon sintering coupled with poor bulk density and mechanical properties. The study also revealed that the addition of 0.2?wt% CuO and subjected to conventional sintering produced similar densification as that obtained for microwave sintering, thus indicating that the dopant played a more significant role than the sintering method.     

Comparison of a laboratorial scale synthesized and a commercial yttria-tetragonal zirconia polycrystals ceramics submitted to microwave sintering

Conventional sintering techniques of yttria-tetragonal zirconia polycrystals (Y-TZP) ceramics have presented limitations regarding the sintering time and temperature, increasing the cost of the final dental and biomedical products. Herein, microwave sintering comes to be an interesting alternative by providing fast heating, high densification, and grain-size control. The aim of this study was to compare the effect of microwave sintering of Y-TZP dental ceramics prepared from a pre-sintered commercial block and produced from powders synthesized in a laboratorial scale by the precipitation route. The synthetized and commercial discs were submitted to microwave sintering at 1450°C and 1350°C for 15, 30, and 60 minutes. Densification, fracture toughness, grain size, and crystalline phase quantification of the sintered groups were evaluated. Both synthetized and commercial groups sintered at 1450°C for 15 and 30 minutes showed the higher densification results (98% TD). XRD quantitative phase analysis indicates that samples present 89% tetragonal and 11% cubic phases, except for the group prepared from coprecipitated powders sintered at 1450°C for 30 minutes, that presented 79% and 21% of tetragonal and cubic phases. The microwave sintering at 1450°C allows hardness and fracture toughness values comparable to conventional sintering.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

The degradation behavior of high-voltage SnO2 based varistors sintered at different temperatures

In this research, for the first time, the stability of SnO₂ based varistor ceramics sintered in the range of 1250–1350 °C against DC-accelerated aging and impulse surge current tests, was systematically studied. Microstructural study of the sintered samples by XRD and FESEM indicated that the sintering temperature only affects densification and grain size, while phase composition remains intact. With the increase of sintering temperature from 1250 °C to 1350 °C, the mean grain size increased from 1.6 to 8 μm. The maximum nonlinear coefficient of 50 and the minimum leakage current density of 1.5 μA/cm² were obtained in the sample sintered at 1300 °C. The breakdown electric field decreased from 800 V/mm to 270 V/mm, when sintering temperature increased from 1250 °C to 1350 °C. The samples sintered at 1250 °C did not show stability against neither of DC-accelerated aging and impulse current tests. The varistors sintered at 1300 °C exhibited the excellent resistance to DC-accelerated aging degradation, while ceramics sintered at 1350 °C showed the best resistance to impulse current degradation.     

Chromium-promoted preparation of forsterite refractory materials from ferronickel slag by microwave sintering

The chromium-promoted preparation of forsterite refractory materials from ferronickel slag was investigated by microwave sintering of the slag with the additions of sintered magnesia and 0–10 wt% chromium oxide (Cr₂O₃). The thermodynamic calculations revealed that the addition of Cr₂O₃ can promote the formations of spinel and liquid phase and maintain high content of forsterite below 1500 °C. The experimental results showed that there existed a stronger promoting effect of Cr₂O₃ additive on the properties of refractory materials in the microwave field than that in conventional sintering. It was attributed to the preferential formation and growth of spinel with stronger microwave absorption than other phases (e.g., enstatite), the existence of more forsterite, and the enhanced densification in association with the presence of more liquid phase at the same temperature. By microwave sintering of the mixture of ferronickel slag, 25 wt% sintered magnesia, and 4 wt% Cr₂O₃ at 1350 °C for 20 min, a superior refractory material with refractoriness of 1801 °C, thermal shock resistance of 6 times, bulk density of 2.97 g/cm³, apparent porosity of 1.4%, and compressive strength of 197 MPa was obtained. Compared with that prepared by conventional sintering at 1350 °C for 2 h, the refractoriness and thermal shock resistance were increased by 175 °C and 100%, respectively. The present study provided a novel method for preparing high-quality refractory materials from ferronickel slag and relevant industrial wastes.     

Low-temperature sintering of coarse alumina powder compact with sufficient mechanical strength

Coarse alumina powder compacts doped with various amounts of titania and copper oxide were pressurelessly sintered from 900 °C to 1600 °C. Their phase assemblages and microstructural evolution, as well as their properties, were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), differential scanning calorimetry/thermogravimetric (DSC/TG) analysis, and three-point bending and wetting test. The role of TiO₂ and CuO during the sintering is discussed in detail. The experimental results show that the liquid phase from the copper oxide appeared at approximately 1200 °C, so the solid-state reaction between alumina and titania took place at a lower temperature. Such solid state-reaction sintering had a strong impact on the grain growth and greatly promoted the densification of the alumina compact. In addition, the liquid phase inhibited the abnormal grain growth and microcracking. As a result, the coarse alumina powder compacts doped with 5 wt% TiO₂–CuO were fully densified and exhibited sufficient flexural strength (342±21 MPa) when sintered at a temperature of 1450 °C for 2 h.     

Effect of oxide nanofillers on fabrication,structure, and properties of zirconia-based composites

We have studied the effect of NiO on the sintering of yttria-stabilized zirconia at temperatures ranging from 1300 °C to 1500 °C in air and argon environments. It was found that the addition of NiO stabilized the cubic phase of ZrO₂ independently from the sintering atmosphere. The monoclinic phase of ZrO₂ formed only during sintering within the air environment at temperatures higher than 1450 °C. The transformation of NiO to Ni by reversible decomposition depends on the sintering atmosphere, and this can lead to variations in the nature of inclusions and in changes of the structure and properties of nanocomposite materials in the system ZrO₂–NiO(Ni). NiO and Ni inclusions can increase the indentation fracture toughness of zirconia–nickel oxide composite material more than 50%, which can be compared with zirconia ceramics during sintering in a neutral atmosphere alone.     

Microstructure and electrical conductivity of fast fired Sr- and Mg-doped lanthanum gallate

La_0.9Sr_0.1Ga_0.8Mg_0.2O_3−δ solid electrolytes were consolidated by fast firing aiming to investigate the effects of the sintering method on densification, microstructure and ionic conductivity. Powder mixtures were prepared by solid state reaction at 1250 and 1350 °C for 12 h, and fast fired at 1450 and 1500 °C temperatures for 5 and 10 min. The content of impurity phases was found to be quite low with this sintering method. Relatively high density (>90% of the theoretical value) and low porosity (<1.5%) were readily obtained for powder mixtures calcined at 1250 °C. The activation energy for conduction was approximately 1 eV. Specimens fast fired at 1450 °C for 10 min with a mean grain size of 2.26 µm reached the highest value of total ionic conductivity, 22 mS cm⁻¹, at 600 °C.     

Effect of nano CuO addition on the tribo-mechanical behavior of alumina ceramics in non-conformal contact

Sintering of alumina from 1500°C to 1650°C and tribo-mechanical properties at room temperature had been investigated using nano CuO as a sintering aid. Bulk density gradually increases with sintering temperature from 1500°C to 1600°C and is optimized at 1600°C, beyond this, bulk density does not significantly increase at 1650°C. The addition of 2 wt% CuO showed the best result on densification. Densification of about 97.74% was attained at 1600°C with the incorporation of 2 wt% CuO. Nano CuO at grain boundaries forms CuAl₂O₄ liquid which modifies the morphology of the grain and improves mechanical properties. The formation of self-lubricating tribo-film on the wear track results in a low coefficient of friction <0.2 and reduces specific wear rate. 4 wt% CuO addition increases contact tensile stress (σ_max) by 51.2% and high Hertzian contact pressure (P_max≈1.51 GPa) causes plastic deformation of wear track. The re-solidified strengthening bond phase on the wear track simultaneously increases in friction coefficient and wear resistance with CuO addition. The optimizing effect of CuO addition shows that 2 wt% significantly decreases wear rate, and increases hardness and fracture toughness.     

Densification and biocompatibility of sintering 3.0 mol% yttria-tetragonal ZrO2 polycrystal ceramics with x wt% Fe2O3 and 5.0 wt% mica powders additive

The densification and biocompatibility of sintered 3.0 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) ceramics, with X wt% Fe₂O₃ and 5.0 wt% mica powders (denoted by 3Y-TZP: X-5.0 wt% mica) have been studied. When the pellets of 3Y-TZP: X-5.0 wt% mica were sintered at 1300 °C for 1 h, the relative shrinkage increases from 19.20–19.43% with the X increased from 0.3 to 1.0. The relative shrinkage of pellets containing 1.0 wt% Fe₂O₃ (X=1.0) increased from 19.43–19.59% when sintering temperatures were raised from 1300 °C to 1450 °C. X-ray diffraction results show that the pellets of 3Y-TZP: X-5.0 wt% mica sintered at 1400 °C for 1 h only contained single phase of tetragonal ZrO₂ (t-ZrO₂). When the sintering temperature was higher than 1400 °C, the Vickers microhardness was greatest in the pellets with X=0.5. Within pellets with the same Fe₂O₃ content, the dominant wavelength (λ_d) was only slightly different for pellets sintered at 1300 °C and those sintered at 1450 °C. The results of the materials were evaluated in vitro cytotoxicity tests reveals that the powders and sintered pellets are safe materials. The oral mucosa irritation tests did not find erythema or histopathological change including normal epithelium, and was free from leucocyte infiltration, vascular congestion and oedema.     

Dry-sliding wear behavior of 3Y-TZP/Al2O3-NbC nanocomposites produced by conventional sintering and spark plasma sintering

This work presents the initial results of the dry-sliding wear behavior of 3 mol% yttria-stabilized zirconia reinforced with 5 vol% alumina-niobium carbide (3Y-TZP/5 vol% Al₂O₃-NbC) nanocomposites sintered by conventional sintering and spark plasma sintering methods in the temperature range of 1350-1450°C. The reinforcement of 3Y-TZP matrix with hard nanoparticles aimed to improve wear strength of the composites. Wear tests were performed by the ball-on-disc method using alumina (Al₂O₃) and tungsten carbide with 6 wt% cobalt cermet (WC-6%Co) balls as counter-materials, a load of 15 N, a sliding distance of 2000 m, and a sliding speed of 0.1 m/s. Wear behavior was evaluated in terms of wear rate and FE-SEM micrograph analysis of the wear tracks. The nanocomposite sintered at 1450°C by conventional sintering exhibited the least wear when tested with the WC-6%Co ball. Generally, the wear mechanism showed evidence of severe wear regime with both counter-materials.     

Analysis of reactions during sintering of CuO-doped 3Y-TZP nano-powder composites

3Y-TZP (yttria-doped tetragonal zirconia) and CuO nano powders were prepared by co-precipitation and copper oxalate complexation–precipitation techniques, respectively. During sintering of powder compacts (8 mol% CuO-doped 3Y-TZP) of this two-phase system several solid-state reactions clearly influence densification behaviour. These reactions were analysed by several techniques like XPS, DSC/TGA and high-temperature XRD. A strong dissolution of CuO in the 3Y-TZP matrix occurs below 600 °C, resulting in significant enrichment of CuO in a 3Y-TZP grain-boundary layer with a thickness of several nanometres. This “transient” liquid phase strongly enhances densification. Around 860 °C a solid-state reaction between CuO and yttria as segregated to the 3Y-TZP grain boundaries occurs, forming Y₂Cu₂O₅. This solid-state reaction induces the formation of the thermodynamic stable monoclinic zirconia phase. The formation of this solid phase also retards densification. Using this knowledge of microstructural development during sintering it was possible to obtain a dense nano–nano composite with a grain size of only 120 nm after sintering at 960 °C.     

Microporous alumina substrate with porosity >70% by gelcasting

Microporous alumina membrane substrate in tubular and planar configurations have been prepared by gelcasting of alumina powder slurry using high amount of urea–formaldehyde as gelling agent followed by humidity controlled drying, binder removal and sintering of the gelled bodies. Porosity of the substrate samples sintered at 1350 °C was more than 70% as measured by mercury porosimeter. More than 51% porosity could be retained even after sintering of the samples at 1450 °C. Average pores size of the membrane substrate samples sintered at temperature in the range from 1250 to 1550 °C varied between 0.42 and 0.56 with a maximum at 1350 °C. More uniform pores were observed in sample sintered at 1450 °C. Urea-formaldehyde polymer present in the gelcast body acts as template for micropores.     

Properties of magnesium-aluminate spinel derived from bauxite and magnesia

The synthesis of magnesium-aluminate spinel divided from bauxites and magnesias, the starting materials with different molar mass ratios (Al₂O₃: MgO) of 3, 1, and 0.6 were developed using solid-state reaction sintering at 1350-1500°C. The effects of different mass ratios and sintering temperatures on the phase composition, densification behavior, shrinkage, flexural strength, and microstructure of the synthetic materials were studied. It was found that as the relative content of bauxite decreased, the flexural strength first decreased before increasing. When n(Al₂O₃)/n(MgO) was 1, the spinel was the primary phase and the sample was dense. When the temperature became 1450°C, the flexural strength became maximized at 106.48 MPa.     

Effect of annealing on grain growth and Y segregation behavior in tetragonal ZrO2 thin film

In order to fabricate tetragonal yttria stabilized zirconia samples with large grain size, 3 mol% Y₂O₃ doped zirconia thin films were grown on (0001) α-Al₂O₃ substrate by pulsed laser deposition (PLD) followed by subsequent high temperature annealing. The thin film samples were annealed at 1200°C, 1250°C, 1300°C, and 1350°C in order to obtain larger grain size without Y segregation. The microstructure and chemical composition of these annealed films were analyzed using atomic force microscopy, scanning transmission electron microscopy, and energy-dispersive X-ray spectroscopy. The as-grown thin film was found to be composed of [111]-oriented grains of ∼100 nm connected with small-angle tilt boundaries. Based on analysis of annealed thin films, it was revealed that grain growth of tetragonal zirconia occurred anisotropically. Cross section scanning transmission electron microscopy observations revealed that such grain growth behavior is affected by the step-terrace structures of the sapphire substrate. Energy-dispersive X-ray spectroscopy showed that Y was found to distribute almost uniformly below 1300°C but to segregate at the grain boundaries at 1350°C. As a conclusion, the 1300°C-annealed sample shows the largest grain size with homogeneous Y distributions.     

Effect of manganese oxide on the sintered properties and low temperature degradation of Y-TZP ceramics

The sinterability of yttria-tetragonal zirconia polycrystals (Y-TZP) containing small amounts of MnO₂ as sintering aid was investigated over the temperature range of 1250–1500 °C. Sintered samples were evaluated to determine bulk density, Young's modulus, Vickers hardness and fracture toughness. In addition, the tetragonal phase stability of selected samples was evaluated by subjecting the samples to hydrothermal ageing in superheated steam at 180 °C/10 bar for up to 24 h. The results showed that the addition of MnO₂, particularly ≥0.3 wt% was effective in aiding densification, improving the matrix stiffness and hardness when compared to the undoped Y-TZP sintered at temperatures below 1350 °C. On the other hand, the fracture toughness of Y-TZP was unaffected by MnO₂ addition except for the 1 wt% MnO₂-doped Y-TZP samples sintered above 1400 °C. The hydrothermal ageing resistance of Y-TZP was significantly improved with the additions of MnO₂ in the Y-TZP matrix.     

Pressureless densification and mechanical properties of hafnium diboride doped with B4C: From solid state sintering to liquid phase sintering

A pressureless sintering process, using a small amount of boron carbide (≤2 wt%) as sintering aid, was developed for the densification of hafnium diboride. Hafnium diboride ceramics with high relative density were obtained when the sintering temperature changed from 2100 °C to 2350 °C. However, the sintering mechanism was varied from solid state sintering (SSS, below 2300 °C) to liquid phase sintering (LPS, above 2300 °C). Boron carbide addition improved densification by removing the oxide impurities during solid state sintering and by forming a liquid phase which was well wetting hafnium diboride grains during liquid phase sintering process. The different roles of B₄C on the microstructure development and mechanical properties of the sintered ceramics were investigated.     

Heat treatment effects on microstructure and mechanical properties of CVI SiCf/PyC/SiC composites with Cansas-Ⅲ SiC fibers

The microstructure and mechanical properties of CVI-Cansas-III/PyC/SiC composites were systematically investigated after heat treatment under high temperature argon atmosphere, ranging from 1000 °C to 1500 °C, for different time durations. The results showed that the Cansas-III fibres degraded with increasing heat treatment temperature, resulting in degradation of the fibre properties due to pyrolysis of the SiOC phase inside the fibres. The bending strength of the composites remained nearly constant upon heat treatment at 1000 °C and 1250 °C, while a decline in bending strength was observed upon increasing the heat treatment temperature and time, specifically at 1350 °C and above. Moreover, the composites maintained their pseudo-plastic fracture behaviour below 1450 °C, while displaying brittle fracture of the ceramic after 100 h of heat treatment at 1500 °C, due to the complete crystallisation of the fibres.     

Alumina Toughened Zirconia Nanocomposite Incorporating Al2O3 Whiskers

We investigated the Vickers hardness and fracture toughness of an Al₂O_3(n) + 70 wt% ZrO₂ (TZ‐3Y)_n nanocomposite with addition of 2.5 wt% Al₂O₃ whiskers. Densities greater than 95% were reached after conventional sintering at 1500°C. The fracture toughness was increased 62% over pure Al₂O₃. Microcracking and crack deflection can be the mechanisms responsible to improve the fracture toughness. The use of ATZ composites with a low percent of whiskers can be a promising biomedical material for medical and dental applications given its large increase in fracture toughness over pure alumina and the observed relief from aging issues of zirconia.     

Graphene nanoplatelets for electrically conductive 3YTZP composites densified by pressureless sintering

3 mol% yttria tetragonal zirconia polycrystalline (3YTZP) ceramic composites with 2.5, 5 and 10 vol% graphene nanoplatelets (GNP) were pressureless sintered in argon atmosphere between 1350 and 1450 °C. The effects of the GNP content and the sintering temperature on the densification, microstructure and electrical properties of the composites were investigated. An isotropic distribution of GNP surrounding ceramic regions was exhibited regardless the GNP content and sintering temperature used. Electrical conductivity values comparable to the ones of fully dense composites prepared by more complex techniques were obtained, even though full densification was not achieved. While the composite with 5 vol% GNP exhibited electrical anisotropy with a semiconductor-type behaviour, the composite with 10 vol% GNP showed an electrically isotropic metallic-type behaviour.