Y<Subscript>2</Subscript>O<Subscript>3</Subscript> and Nd<Subscript>2</Subscript>O<Subscript>3</Subscript> co-stabilized ZrO<Subscript>2</Subscript>-WC composites

Y₂O₃ + Nd₂O₃ co-stabilized ZrO₂-based composites with 40 vol% WC were fully densified by pulsed electric current sintering (PECS) at 1350 °C and 1450 °C. The influence of the PECS temperature and Nd₂O₃ co-stabilizer content on the densification, hardness, fracture toughness and bending strength of the composites was investigated. The best combination of properties was obtained for a 1 mol% Y₂O₃ and 0.75 mol% Nd₂O₃ co-stabilized composite densified for 2 min at 1450 °C under a pressure of 62 MPa, resulting in a hardness of 15.5 ± 0.2 GPa, an excellent toughness of 9.6 ± 0.4 MPa.m^0.5 and an impressive 3-point bending strength of 2.04 ± 0.08 GPa. The hydrothermal stability of the 1 mol% Y₂O₃ + 1 mol% Nd₂O₃ co-stabilized ZrO₂-WC (60/40) composites was compared with that of the equivalent 2 mol% Y₂O₃ stabilized ceramic. The double stabilized composite did not degrade in 1.5 MPa steam at 200 °C after 4000 min, whereas the yttria stabilized composite degraded after less than 2000 min. Moreover, the (1Y,1Nd) ZrO₂-WC composites have a substantially higher toughness (~9 MPa.m^0.5) than their 2Y stabilized equivalents (~7 MPa.m^0.5).     

Mechanical properties of Al2O3 and Al2O3 + ZrO2 ceramics reinforced by SiC whiskers

The effect of the SiC whisker content on the mechanical properties of Al₂O₃ and Al₂O₃ + 20 vol% ZrO₂ (2 mol% Y₂O₃) ceramic composites has been investigated. It is shown that the strength and fracture toughness of the composites are increased by the addition of 0–30 vol% SiC whiskers with only one exception that 30 vol% SiC whisker leads to a decrease in the flexure strength. The addition of 20 vol% ZrO₂ (2 mol% Y₂O₃) significantly improves the mechanical properties of the Al₂O₃ + SiC whisker (SiC_w) composites and the t-m phase transformation of ZrO₂ is enhanced by the residual stresses caused by the thermal incompatibility between the SiC_w and the matrix. The toughening effect of both SiC whiskers and the t-m phase transformation of ZrO₂ (2 mol% Y₂O₃) is shown to be additive, but the addition of ZrO₂ decreases the strengthening effect of the SiC whiskers.     

Microstructure and mechanical properties of 3Y-TZP/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites fabricated by liquid phase sintering

3Y-TZP/Al₂O₃ composites were pressureless sintered with the addition of TiO₂-MnO₂ and CaO-Al₂O₃-SiO₂ glass. The densification, microstructure and mechanical properties of the composites were investigated. It was found that the composites could be densified at a temperature as low as 1400^C by liquid phase sintering. The majority of the grain sizes for both Al₂O₃ and ZrO₂ were below 1 m because of the lower sintering temperature. A bending strength of 934 ± 28 MPa and fracture toughness of 7.82 ± 0.19 MPam^1/2 were obtained for 3Y-TZP/Al₂O₃ (20 vol%) composite. Transformation toughening is considered the responsible toughening mechanism.     

Effects of heteroflocculation of powders on mechanical properties of zirconia alumina composites

Zirconia-toughened alumina (ZTA) composites colloidally processed from dense aqueous suspensions (>50 vol% solids) had ZrO₂ content varying from 5 to 30 vol%. Tetragonal zirconia (TZ) was used in the unstabilized, transformable form (0Y-TZ), in the partially transformable form, partially stabilized with 2 mol% yttria (2Y-TZ), and in the non-transformable form stabilized with 3 mol% yttria (3Y-TZ). After sintering in air to 99% theoretical density, the elastic properties, flexure strength and fracture toughness were examined at room temperature. Dynamic moduli of elasticity of fully deagglomerated compositions did not show the effects of microcrack formation during sintering, even for materials with unstabilized zirconia. In all compositions made from submicron powders and with low content of dispersed phase (less than 10 to 20 vol %), the strength increased with increasing ZrO₂ content to a maximum of 1 GPa, irrespective of the degree of stabilization of t-ZrO₂. With increasing content of the dispersed phase (> 20 vol%), heteroflocculation of powder mixtures during wet-processing led to the formation of ZrO₂ grain clusters of increasing size. Residual tensile stresses built within cluster/matrix interfaces upon cooling not only facilitated the t-m ZrO₂ phase transformation in final composites with transformable t-ZrO₂, but also led to lateral microcracking of ZrO₂/Al₂O₃ interfaces. This enhanced fracture toughness, but at larger ZrO₂ contents the flexure strength always decreased due to intensive microcracking, both radial and lateral. The important microstructural aspects of strengthening and toughening mechanisms in ZTA composites are related in discussion to the effects of heteroflocculation of powder mixtures during wet-processing.     

Effect of Al<Subscript>2</Subscript>O<Subscript>3</Subscript> on the properties of nanocrystalline ZrO<Subscript>2</Subscript> + 3 mol % Y<Subscript>2</Subscript>O<Subscript>3</Subscript> powder

We have studied the properties of nanocrystalline ZrO₂〈3 mol % Y₂O₃〉 and 90 wt % ZrO₂〈3 mol % Y₂O₃〉-10 wt % Al₂O₃ powders prepared via hydrothermal treatment of coprecipitated hydroxides at 210°C. The results demonstrate that Al₂O₃ doping raises the phase transition temperatures of the metastable low-temperature ZrO₂ polymorphs and that the structural transformations of the ZrO₂ and Al₂O₃ in the doped material inhibit each other.     

A novel method for producing open-cell Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-ZrO<Subscript>2</Subscript> ceramic foams with controlled cell structure

A novel method was introduced to prepare open-cell Al₂O₃–ZrO₂ ceramic foams with controlled cell structure. This method used epispastic polystyrene (EPS) spheres to array ordered templates and centrifugal slip casting in the interstitial spaces of the EPS template to obtain cell struts with high packing density. Aqueous Al₂O₃–ZrO₂ slurries with up to 50 vol.% solid contents were prepared and centrifuged at acceleration of 2,860g. The effect of the solid contents of slurries on segregation phenomena of different particles and green compact uniformity were investigated. In multiphase system, the settling velocities of Al₂O₃ and ZrO₂ particles were calculated. Theory analysis and calculated results both indicated segregation phenomenon was hindered for slurries with 50 vol.% solid content. The cell struts of sintered products had high green density (61.5%TD), sintered density (99.1%TD) and homogeneous microstructures after sintered at 1,550 °C for 2 h. The cell size and porosity of Al₂O₃–ZrO₂ ceramic foams can be adjusted by changing the size of EPS spheres and the load applied on them during packing, respectively. When the porosity increased from 75.3% to 83.1%, the compressive strength decreases from 3.82 to 2.07 MPa.     

Influence of CaTiO3 impurity in SHS-TiN powder on the mechanical properties of ZrO2–TiN composites

Yttria-stabilised tetragonal polycrystalline ZrO₂-based composites with 40 vol.% TiN were hot pressed at 1450 °C for 1 h using a jet-milled thermally synthesized and a self-propagating high-temperature synthesis (SHS) TiN powder. The ZrO₂ phase of the SHS-TiN powder-based composites was found to be substantially coarser than for the jet-milled TiN powder-based ceramics and prone to spontaneous transformation to m-ZrO₂ and microcracking, due to the CaTiO₃ impurity in the SHS-TiN starting powder. In order to prove this, a set of experiments was performed to investigate the effect of the addition of CaO and TiO₂ on an yttria-stabilised tetragonal ZrO₂ polycrystalline (Y-TZP). The addition of 0.2 mol% of CaO to a Y-TZP ceramic was found to destabilise the t-ZrO₂ phase, whereas the addition of 1 mol% TiO₂ results in significant grain growth and the formation of less transformable t-ZrO₂. The CaTiO₃ impurity could be removed from the SHS-TiN powder by hot hydrochloric acid leaching, allowing to obtain a similar microstructure and mechanical properties as with conventional TiN powder.     

Relationship between thermal and sliding wear behavior of Al6061/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> metal matrix composites

Al6061 alloy and Al6061/Al₂O₃ metal matrix composites (MMCs) were fabricated by stir casting. The MMCs were prepared by addition of 5, 10 and 15 wt% Al₂O₃ particulates and the size of particulates was taken as 16 μm. The effect of Al₂O₃ particulate content, thermal properties and stir casting parameters on the dry sliding wear resistance of MMCs were investigated under 50–350 N loads. The dry sliding wear tests were performed to investigate the wear behavior of MMCs against a steel counterface (DIN 5401) in a block-on-ring apparatus. The wear tests were carried out in an incremental manner, i.e., 300 m per increment and 3,000 m in total. It was observed that, the increase in Al₂O₃ vol% decreased both thermal conductivity and friction coefficient and hence increased the transition load and transition temperature for mild to severe wear during dry sliding wear test.     

Interface structure and mechanical properties of Al2O3-20 vol% ZrO2-20 vol% SiCW ceramic composite

The microstructure, mechanical properties, fracture behaviour and toughening mechanisms of Al₂O₃-20 vol% ZrO₂ (2 mol% Y₂O₃)-20 vol% SiC_W ceramic matrix composite were investigated by X-ray diffraction, scanning and transmission electron microscopies, energy dispersive analysis of X-rays, high-resolution electron microscopy techniques and three-point bending tests. The results show that the Al₂O₃ matrix is simultaneously strengthened and toughened by both ZrO₂ particles and SiC whiskers. The interfacial amorphous layers between SiC whiskers and ZrO₂, and Al₂O₃ grains were observed by both TEM dark-field and high-resolution electron microscopy techniques.     

Thermal stability and mechanical properties of yttria-doped tetragonal zirconia polycrystals with dispersed alumina and silicon carbide particles

Yttria-doped tetragonal zirconia polycrystals in which were dispersed various amounts of Al₂O₃ and SiC particles were sintered at 1500° C for 3 h, and the mechanical properties and the thermal stability of the sintered bodies were evaluated. Dispersion of Al₂O₃ caused no significant effect on sinterability, and increased the hardness and elasticity of the composites. Dispersion of SiC particles decreased the relative density and the grain size of composites. Elasticity and hardness increased by dispersing less than 10 vol% SiC, but decreased above 10 vol% SiC due to the decrease of relative density. Dispersion of both Al₂O₃ and SiC particles slightly increased the fracture toughness of ZrO₂-3 mol% Y₂O₃ ceramics but significantly decreased that of ZrO₂-2 mol% Y₂O₃ ceramics. The rate of the tetragonal-to-monoclinic phase transformation decreased by dispersing both Al₂O₃ and SiC particles. The transformation depth increased rapidly and then slowly with increasing the annealing time. The rate of increase in the transformation depth greatly decreased by dispersing Al₂O₃ particles.     

Texture development in 3 mol% yttria-stabilized tetragonal zirconia

We have developed a method of forming textured tetragonal zirconia. A suspension containing 10 vol% solid loading of monoclinic ZrO₂ mixed with 3 mol% Y₂O₃ was prepared, and then a bead-milling process was performed using 50 μm diameter zirconia beads resulting in a well-dispersed suspension. The mixture suspension of monoclinic zirconia and yttria nanoparticles was slip cast under a magnetic field of 12 T to produce oriented monoclinic zirconia with yttria. The reaction sintering between yttria and the oriented monoclinic zirconia produces a final 3 mol% Y₂O₃ doped tetragonal zirconia that remains oriented.     

Effects of TiO<Subscript>2</Subscript>, ZrO<Subscript>2</Subscript> and Al<Subscript>2</Subscript>O<Subscript>3</Subscript> dopants on the compressive strength of tricalcium phosphate

Tricalcium phosphate (TCP) powders synthesised using the Ca(NO₃)₂ and Ca(OH)₂ routes were doped with TiO₂, ZrO₂ and Al₂O₃ in order to increase their compressive strength. An ultimate compressive strength (UCS) of 255 ± 6 MPa was achieved for approximately 10 vol% TiO₂ doping compared to 30 ± 3 MPa for an un-doped control processed and tested in the same manner. Higher levels of TiO₂ doping resulted in smaller increases in UCS with 30 and 50 vol% achieving 213 ± 9 and 178 ± 15 MPa, respectively. Very small amounts of Al₂O₃ doping (< 0.5 vol%) also resulted in a stronger materials. However, under the processing conditions employed, higher levels of Al₂O₃ and ZrO₂ doping resulted in no beneficial effect on the UCS. Polyvinyl alcohol (PVA) was used as binding agent to facilitate processing. As expected, higher levels of PVA were associated with smaller increases in UCS. Powders synthesised using the Ca(OH)₂ route had smaller particle size and resulted in larger increases in UCS compared to the Ca(NO₃)₂-synthesised powders. Although some powders contained α and β-TCP phases, no other calcium phosphate, CaO, CaTiO₃ or CaZrO₃ phases were detected. In conclusion, a significant increase in the UCS of TCP was achieved by doping with approximately 10 vol% TiO₂ which is expected to have little or no effect on the bioactivity or bioresorbability of the material.     

Preparation and properties evaluation of zirconia-based/Al2O3 composites as electrolytes for solid oxide fuel cell systems

Yttria-doped zirconia powders containing 3 to 8 mol% Y₂O₃ and 0 to 20 wt% Al₂O₃ were prepared by both mixing commercial oxides and a coprecipitation method, and the mechanical and electrical properties have been examined as a function of the Al₂O₃ content. The bending strength of the composite at room temperature increased with increasing Al₂O₃ content. In the temperature range 500–1000 °C the bending strength increased with Al₂O₃ content up to 10 wt% and then decreased, the measured value at 1000 °C (200 MPa) being higher than those at lower temperatures for cubic zirconia materials. Fracture toughness (K_IC) decreased with increasing Y₂O₃ content in the Al₂O₃-free zirconia materials. Al₂O₃ additions enhanced the fracture toughness and this was maximum (7 MPa m^1/2) for the composite ZrO₂-3 mol% Y₂O₃/10 wt% Al₂O₃. The electrical conductivity of cubic ZrO₂/Al₂O₃ composites decreased monotonically with Al₂O₃ content, but in tetragonal ZrO₂/Al₂O₃ composites hardly varied or apparently increased up to 10 wt% Al₂O₃. At 1000 °C the highest electrical conductivity was 0.30 S cm^–1 for ZrO₂-8 mol% Y₂O₃, and this decreased up to 0.10 S cm^–1 for the composite ZrO₂-8mol% Y₂O₃/20 wt% Al₂O₃.     

Production of opaque frits with low ZrO<Subscript>2</Subscript> and ZnO contents and their industrial uses for fast single-fired wall tile glazes

The amounts of zirconium and zinc oxides, which raise the production costs of ceramic glazes, were decreased in fast single-fired wall tile frit compositions and an industrial frit production was conducted. Opacity of the fired frit-based glazes was accomplished by compositional modifications of frits with no other nucleating agent. It was determined that the ratios of Al₂O₃/ΣR₂O, Al₂O₃/ΣRO, and Al₂O₃/B₂O₃ have significant effects on decreasing ZrO₂ and ZnO levels in the frit composition. A reduction of 25% in both zirconia and zinc oxide contents of frit batches, with respect to the reference frit (R) containing 6–10% ZrO₂ and 6–10% ZnO for a glossy white opaque wall tile glaze, was achieved in the ZD glaze consisting of 4.5–7.5% zirconia and 4.5–7.5% ZnO in its frit composition. It was concluded that zircon was the main crystalline phase of the glaze contributing the opacity. The ZD frit-based glaze has a thermal expansion coefficient value of 61.13 ± 0.32 × 10⁻⁷ °C⁻¹ at 400 °C which well matches to that of the wall tile body. TS EN ISO 10545 standard tests were also applied to the final ZD glaze. It is confirmed that the production cost of a fast single-fired wall tile glaze can be decreased by 15–20% with the successful new frit developed.     

Mechanical properties of bovine hydroxyapatite (BHA) composites doped with SiO<Subscript>2</Subscript>, MgO,Al<Subscript>2</Subscript>O<Subscript>3</Subscript>, and ZrO<Subscript>2</Subscript>

Biologically derived hydroxyapatite from calcinated (at 850 °C) bovine bones (BHA) was doped with 5 wt% and 10 wt% of SiO₂, MgO, Al₂O₃ and ZrO₂ (stabilized with 8% Y₂O₃). The aim was to improve the sintering ability and the mechanical properties (compression strength and hardness) of the resultant BHA-composites. Cylindrical samples were sintered at several temperatures between 1,000 and 1,300 °C for 4 h in air. The experimental results showed that sintering generally occurs at 1,200 °C. The BHA–MgO composites showed the best sintering performance. In the BHA–SiO₂ composites, extended formation of glassy phase occurred at 1,300 °C, resulting in structural degradation of the resultant samples. No sound reinforcement was achieved in the case of doping with Al₂O₃ and zirconia probably due to the big gap between the optimum sintering temperatures of BHA and these two oxides.     

Properties of nanocrystalline ZrO<Subscript>2</Subscript>-Y<Subscript>2</Subscript>O<Subscript>3</Subscript>-CeO<Subscript>2</Subscript>-CoO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> powders

We have studied the properties of nanocrystalline ZrO₂-Y₂O₃-CeO₂-CoO-Al₂O₃ powders prepared via hydrothermal treatment of a mixture of coprecipitated hydroxides at 210°C. A number of general trends are identified in the variation of the properties of the synthesized powders during heat treatment at temperatures from 500 to 1200°C. Our results demonstrate that the addition of 0.3 mol % CoO to nanocrystalline ZrO₂-based powders containing 1 to 5 mol % Al₂O₃ allows one to obtain composites with good sinterability at a reduced temperature (1200°C).     

Influences of ZrO<Subscript>2</Subscript> nanoparticles on the microstructure and mechanical behavior of Ce-TZP/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposites

Influences of ZrO₂ nanoparticles on the mechanical properties and microstructure of hot-pressing Ce-TZP/Al₂O₃ ceramics were investigated. Meanwhile, t-ZrO₂ to m-ZrO₂ transformation toughening mechanism was investigated by X-ray diffractometry (XRD) method, and deflection of samples under applied stress were recorded too. The results show that when the percentage of ZrO₂ was 20%, the mechanical properties and microstructures of materials are optimum. Moreover, TEM observation show dislocation structures formation both in the Al₂O₃ and on the grain boundary. Because the dislocation agglomeration and fixation by ZrO₂ nanoparticles could deflect cracking or stop cracking development, a strengthening and toughening effect could be achieved.     

Fabrication of carbon nanofiber(CNF)-dispersed Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites by pulsed electric-current pressure sintering and their mechanical and electrical properties

Dense Al₂O₃-based composites (≥99.0% of theoretical) dispersed with carbon nanofibers (CNFs) were fabricated using the pulsed electric-current pressure sintering (PECPS) for 5 min at 1300°C and 30 MPa in a vacuum. The dispersion of CNFs into the matrix depended much on the particle size of the starting Al₂O₃ powders. Mechanical properties of the composites were evaluated in relation with their microstructures; high values of three-point bending strength σ_b (∼800 MPa) and fracture toughness K _IC (∼5 MPa·m^1/2) were attained at the composition of CNF/Al₂O₃ = 5:95 vol%, which σ_b and K _IC values were ∼25% and ∼5%, respectively, higher than those of monolithic Al₂O₃. This might be due to the small Al₂O₃ grains (1.6 μm) of dense sintered compacts compared with that (4.4 μm) for the pure Al₂O₃ ceramics, resulting from the suppression of grain growth during sintering induced by uniformly dispersed CNFs in the matrix. Electrical resistivity of CNF/Al₂O₃ composites decreased rapidly from >10¹⁵ to ∼2.1 × 10⁻² Ωm (5vol%CNF addition), suggesting the machinability of Al₂O₃-based composites by electrical discharge machining.

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Crack propagation in layered Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/ZrO<Subscript>2</Subscript> composites prepared by electrophoretic deposition

Crack propagation through layered Al₂O₃/ZrO₂ composites was studied. The specimens were prepared via electrophoretic deposition of alumina and zirconia powders from suspensions with monochloroacetic acid and isopropanol. The kinetics of electrophoretic deposition could be described fully if the electrophoretic mobility and conductivity of suspensions were known. The conductivity of suspensions increased in the course of deposition. Adjusting to properly controlled kinetics of deposition and sintering, deposits were prepared with strongly bonded layers of different pre-defined thicknesses and, consequently, with different magnitudes of residual stress. Cracks, produced by an indentation technique, propagated askew towards layer interfaces deflected towards the interface in the Al₂O₃ layers and away from the interface in the ZrO₂ layers. Changes in the direction of crack propagation were described for the whole range of angles of incidence (0°–90°). The biggest change in the crack propagation was observed for the angle of incidence 45° and was ca. 15°, irrespective of the magnitude of residual stress in the layers.     

Phase stability,microstructure and high-temperature properties of NbSi<Subscript>2</Subscript>- and TaSi<Subscript>2</Subscript>-oxide conducting ceramic composites

NbSi₂- and TaSi₂-based electroconductive ceramic composites with the addition of 40–70 vol% Al₂O₃ and ZrO₂ particles were fabricated by high-temperature sintering (1400–1600 °C) under argon. Their phase stability, microstructural evolution, oxidation kinetics and electrical properties were studied at high temperatures. The densification of the composites was improved by increasing the oxide phase content and sintering temperature. The interaction of the starting metal disilicides with residual oxygen sources resulted in the formation of the hexagonal-structured 5–3 metal silicide (Nb₅Si₃ and Ta₅Si₃) phases. The increasing sintering temperature and volume percentage of the oxide phase reduced the pest oxidation, particularly for the silicide–alumina composites, which exhibited lower oxidation-induced mass changes than their dense monolithic metal silicides. Depending on the silicide–oxide volume percentage, their electrical conductivities ranged from 5.3 to 111.3 S/cm at 900 °C. Their phase stability, reduced oxidation rates and high electrical conductivities at high temperatures show promise for future high-temperature applications in advanced sensing.