An evaluation of Al2O3-ZrO2 composites produced by coprecipitation method

The objective of this work is to produce Al₂O₃-ZrO₂ composite from nano-sized powders processed by coprecipitation method. Al₂O₃ and mixture of Al₂O₃ + 10 wt.% ZrO₂ precipitated successfully by chemical route from aluminum sulfate and zirconium sulfate were pressed under uniaxial compression of 170 MPa and sintered at 1600 °C for 1 h. SEM investigations revealed that, pure alumina sample has a microstructure with coarse grains which anisotropically grown up to 30-40 μm in size. In alumina-zirconia composite, the structure consists of very fine equiaxed grains of typically 2 μm in which zirconia precipitates were uniformly dispersed. By adding zirconia to alumina, hardness and indentation fracture toughness were increased from 11.6 GPa to 16.8 GPa and from 3.2 MPa m^1/2 to 4.9 MPa m^1/2, respectively. Improvement in fracture toughness was attributed to bridging effects of zirconia particles as well as transformation toughening.     

Compressive strength, hardness and fracture toughness of Al2O3 whiskers reinforced ZTA and ATZ nanocomposites: Weibull analysis

The aim of this investigation was to study the variability in compressive strength, fracture toughness and microhardness applying the well-known Weibull statistics and to be able to provide a wide spectrum of mechanical properties in Al₂O₃ whisker reinforced alumina toughened zirconia (ATZ) and zirconia toughened alumina (ZTA) nanocomposites for possible dental applications. Uniaxial compression tests at room temperature of samples 6.35 ± 0.03 mm in diameter and 12.50 ± 0.63 mm in length and Vickers hardness measurements on polished surfaces were carried out. The indentation fracture toughness (K_IC) was derived from the average crack length. Weibull analysis was performed on the data. The ATZ2 (18.0 wt.% Al₂O₃ + 2.0 wt.%_(w) + 80.0 wt.% ZrO₂ (TZ-3Y)) nanocomposite reported the highest average compressive load of 1200 MPa, the highest value of characteristic strength, σ_o, of 1340 MPa with Weibull modulus of 3.25 and relatively high fracture toughness (4.7 ± 0.7 MPa m^1/2), suggesting that with the wide range of mechanical properties obtained in our work, different dental applications could be offered without lead to premature failure.     

Hot isostatic pressing (HIP) of α-Al2O3 submicron ceramics pressureless sintered at different temperatures: Improvement in mechanical properties for use in total hip arthroplasty (THA)

The effect of hot isostatic pressing (HIPing) on as-sintered α-Al₂O₃ ceramics for total hip arthroplasty (THA) was investigated. The sinterability of these powders and the minimum temperature required to obtain closed porosity have been determined by pressureless sintering in air at temperatures between 1280 and 1460 °C for 2 h. Temperatures of 1300 and 1325 °C and applied pressures of 150 MPa for 30 min were utilised in the HIP cycles. Densities >98% of the theoretical density (TD) have been obtained after HIPing, and the grain sizes previously obtained during pressureless sintering increased slightly during the HIP treatment. The microstructures before and after HIP treatments were observed by means of scanning electron microscopy (SEM). The fracture toughness was obtained by the indentation fracture technique using a Vickers hardness tester at a load of 10 N with a dwell time of 15 s for all cases. The ceramics obtained at the lowest HIP temperature (1300 °C) presented a grain size of 0.62 ± 0.04 μm, hardness of 20.5 ± 0.6 GPa, and fracture toughness of 4.8 ± 0.3 MPa m^1/2. The reported values were higher than those obtained by other authors and were in concordance with international standards that could make these ceramics available as a replacement for metal-on-polyethylene in orthopaedic surgery.     

Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.     

Effect of CrB2 addition on densification, properties and oxidation resistance of TiB2

This paper presents the results of detailed studies carried out on the densification of TiB₂ with CrB₂ as sinter additive by hot pressing. The dense compacts were characterized by measurement of hardness, indentation fracture toughness, flexural strength, coefficient of thermal expansion and electrical resistivity. Oxidation characteristics were investigated between 600 °C and 1000 °C and isothermal oxidation kinetics at 850 °C. Phase identification and surface morphology analysis of hot pressed and oxidized samples were done using XRD and SEM. A high density of 96.61% Τ.D was obtained with the addition of 2.5% CrB₂ by hot pressing at 1750 °C under 35 MPa pressure. Hardness values of composites with 2.5–10% CrB₂ were close to 24 GPa and fracture toughness in the range of 3–5 MPa m^1/2. Coefficient of thermal expansion of the composite with 10% CrB₂ was measured in the range of 6.21–7.43 × 10⁻⁶/K from room temperature to 1000 °C. Electrical resistivity of TiB₂ + 10%CrB₂ was measured as 32.83, 75.97 and 120 μΩ cm at 25 °C, 500 °C and 900 °C, respectively. Observed nature of oxidation was parabolic for all composites. Formation of continuous and thick glassy film was observed with increased CrB₂ content in the composite. TiO₂ and CrBO₃ phases were identified on the oxidized surface which are responsible for the improved oxidation resistance of this composite.     

Toughening and strengthening mechanism of plasma sprayed nanostructured Al2O3–13 wt.%TiO2 coatings

The starting materials of Al₂O₃, TiO₂, ZrO₂ and CeO₂ nanoparticles were agglomerated into sprayable feedstock powders and plasma sprayed to form nanostructured coatings. There were net structures and fused structures in plasma sprayed nanostructured Al₂O₃–13 wt.%TiO₂ coatings. The net structures were derived from partially melted feedstock powders and the fused structures were derived from fully melted feedstock powders. The nanostructured Al₂O₃–13 wt.%TiO₂ coatings possessed higher hardness, bonding strength and crack growth resistance than conventional Metco 130 coatings which were mainly composed of lamellar fused structures. The higher toughness and strength of nanostructured Al₂O₃–13 wt.%TiO₂ coatings were mainly related to the obtained net structures.     

Mechanical properties improvement related to the isothermal holding time in Si3N4 ceramics sintered with an alternative additive

In the present work, the influence of the isothermal holding time on the physical (relative density and mass loss), chemical (α–β transformation and intergranular phase crystallization) and mechanical (hardness and fracture toughness) properties of Si₃N₄ ceramics with Al₂O₃ and CTR₂O₃ as additives has been studied. CTR₂O₃ is a natural rare earth oxide mixture, produced at DEMAR-FAENQUIL from the mineral xenotime, consisting mainly of Y₂O₃, Yb₂O₃, Er₂O₃ and Dy₂O₃. The increase in hardness and fracture toughness with increasing duration of isothermal sintering is discussed in regard of densification, α–β Si₃N₄ phase transformation and microstructure. The microstructural variations were decisive for the increase of fracture toughness, because larger grains (>4 μm) with higher aspect ratios (>6) developed during increased sinter periods, enhancing crack deflection and crack-bridging mechanism. In this way longer isothermal holding times contribute to the improvement of the physical and mechanical properties of silicon nitride based ceramics.     

Low temperature sintering and properties of CaO–B2O3–SiO2 system glass ceramics for LTCC applications

The P₂O₅ + ZnO, ZrO₂ + TiO₂, B₂O₃ and a low-melting-point CaO–B₂O₃–SiO₂ glass (LG) are selected as the sintering additives, and the effect of their additions on the microwave dielectric properties, mechanical properties and microstructures of CaO–B₂O₃–SiO₂ system glass ceramics is investigated. It is found that the sintering temperature of pure CBS glass is higher than 950 °C and the sintering range is about 10 °C. With the above additions, the glass ceramics can be sintered between 820 °C and 900 °C. The dielectric properties of the samples are dependent on the additions, densification and microstructures of sintered bodies. The major phases of this material are CaSiO₃, CaB₂O₄ and SiO₂. With 10 wt% B₂O₃ and LG glass additions, the CBS glass ceramics have better mechanical properties, but worse dielectric properties. The _r values of 6.51 and 7.07, the tan δ values of 0.0029 and 0.0019 at 10 GHz, are obtained for the CBS glass ceramics sintered at 860 °C with 2 wt% P₂O₅ + 2 wt% ZnO and 2 wt% ZrO₂ + 2 wt% TiO₂ additions, respectively. This material is suitable to be used as the LTCC material for the application in wireless communications.     

Pulsed electric current sintered Fe3Al bonded WC composites

WC based composites with 5, 10 and 20 vol.% Fe₃Al binder were consolidated via pulsed electric current sintering (PECS) in the solid state for 4 min at 1200 °C under a pressure of 90 MPa. Microstructural analysis revealed a homogeneous Fe₃Al binder distribution, ultrafine WC grains and dispersed Al₂O₃ particle clusters. The WC-5 vol.% Fe₃Al composite combines an excellent Vickers hardness of 25.6 GPa with very high Young’s modulus of 693 GPa, a fracture toughness of 7.6 MPa m^1/2 and flexural strength of 1000 MPa. With increasing Fe₃Al binder content, the hardness and stiffness decreased linearly to 19.9 and 539 GPa, respectively with increasing binder content up to 20 vol.%, while the fracture toughness and flexural strength were hardly influenced by the binder content. Compared to WC–Co cemented carbides processed under exactly the same conditions, the WC–Fe₃Al composites exhibit a substantially higher hardness and Young’s modulus.     

Synthesis and characterization of Al2O3-Ce0.5Zr0.5O2 powders prepared by chemical coprecipitation method

Al₂O₃-Ce_0.5Zr_0.5O₂ catalytic powders were synthesized by the coprecipitation (ACZ-C) and mechanical mixing (ACZ-M) methods, respectively. As-synthesized powders were characterized by XRD, Raman spectroscopy, surface area and thermogravimetric analyses. It was found that the mixing extent of Al³⁺ ions affected the phase development, texture and oxygen storage capacity (OSC) of the Ce_0.5Zr_0.5O₂ powder. Single phase of ACZ-C could be maintained without phase separation and inhibit α-Al₂O₃ formation up to 1200 °C. The specific surface area value of ACZ-C (81.5 m²/g) was larger than that of ACZ-M (62.1 m²/g) and Ce_0.5Zr_0.5O₂ (17.1 m²/g) powders, which were calcined at 1000 °C. In comparison with ACZ-C and Al₂O₃, which were calcined at high temperature (900–1200 °C), it was found that the degradation rate of specific surface area of ACZ-C was lower than that of Al₂O₃. ACZ-C sample showed a higher thermal stability to resist phase separation and crystallite growth, which enhanced the oxygen storage capacity property for Ce_0.5Zr_0.5O₂ powders.     

Effect of Al2O3 content and swaging on microstructure and mechanical properties of Al2O3/W alloys

Al₂O₃-reinfored tungsten alloys were fabricated by powder metallurgy method and hot swaging technology. The investigation was made on the microstructure, relative density, nano-hardness and fracture toughness (K_IC) of the sintered and swaged Al₂O₃/W alloys. The swaging process and addition of Al₂O₃ are beneficial to comprehensive properties of the sintered and swaged alloys. After swaging, the Al₂O₃/W alloys can achieve the full density. According to the nano-indentation test and three-point bend test, the swaged W-0.25 wt% Al₂O₃ alloy possesses the highest hardness of 7.02 GPa, the greatest modulus of 435.09 GPa and the maximum fracture toughness of 21 MPa·m^1/2. The observation of fracture morphology shows that the recrystallization behavior and grain growth occur above 1400 °C in the swaged pure W alloy, which leads to recrystallization brittleness. At the same time, the microstructure of the swaged W-0.25 wt% Al₂O₃ alloy does not change apparently.     

Estimate of the Hall-Petch and Orowan effects in the nanocrystalline Cu with Al2O3 dispersoid

Nanocrystalline (nc) Cu materials with Al₂O₃ dispersoid (Cu-4 vol. % Al₂O₃) were successfully produced by a simple cryo-milling at 210 K with a mixture of Cu₂O, Al, and Cu ingredient powders, followed by hot pressing at 1123 K. The results of microstructural analysis showed that the hot pressed material was comprised of a mixture of Cu matrix (25.1 nm) with a homogeneous size distribution of the Al₂O₃ dispersoid (4 nm in radius). Grain size of Cu was measured by XRD (Scherrer's formula); dispersoid size of Al₂O₃ was confirmed by STEM-EDS (Scanning Transmission Electron Microscopy-Energy Dispersive Spectroscopy) and TEM (Transmission Electron Microscopy). Result of micro hardness tests indicated that the hot pressed materials have a significantly high hardness (265 ± 8, VHN; 2.6 GPa, SI units) at room temperature. Two strengthening mechanisms are considered for high hardness: strengthening by grain refinement and dispersion hardening. An estimate of the individual strengthening effect to total strength of the material at room temperature, based on the Hall-Petch and Orowan equations, is presented.     

Influence of liquid nitrogen quenching on the evolution of metastable phases during plasma spraying of (ZrO2–5 wt.% Y2O3)–20 wt.% Al2O3 coatings

The preparation of nanostructured (ZrO₂–5 wt.% Y₂O₃)–20 wt.% Al₂O₃ coatings by atmospheric plasma spraying of commercially available micron-scale powders is reported. Materials were prepared by means of a standard spraying technique and by using an improved technique that allows for the quenching of the material using liquid nitrogen-cooled substrates. Quenching leads to the controlled formation of metastable phases. The influence of liquid nitrogen cooling on the formation of the metastable phases was studied by X-ray diffraction under a grazing incidence angle of 1°. A significant increase in the amount of the metastable zirconia phase and a more homogeneous composition along the thickness were found compared to the regularly sprayed coatings. All materials were subjected to a thermal treatment for 1 h at 1400 °C to study the evolution of stable phases.     

Effect of rare earth La2O3 on the microstructure and mechanical properties of TiC/W composites

In this study, La₂O₃ was investigated as an additive to TiC/W composites. The composites were prepared by vacuum hot pressing, and the microstructure and mechanical properties of the composites were investigated. Experimental results show that the grain size of the TiC/W composites is reduced by TiC particles. When 0.5 wt.% La₂O₃ is added to the composites, the grain size is reduced further. According to TEM analysis, La₂O₃ can alleviate the aggregation of TiC particles. With La₂O₃ addition, the relative density of the TiC/W composites can be improved from 95.1% to 96.5%. The hardness and elastic modulus of the TiC/W + 0.5 wt.% La₂O₃ composite are little improved, but the flexural strength and the fracture toughness increase to 796 MPa and 10.07 MPa·m^1/2 respectively, which are higher than those of the TiC/W composites.     

Improved high-Q microwave dielectric resonator using ZnO-doped La(Co1/2Ti1/2)O3 ceramics

The microwave dielectric properties and the microstructures of ZnO-doped La(Co_1/2Ti_1/2)O₃ ceramics prepared by conventional solid-state route have been studied. Doped with ZnO (up to 0.75 wt%) can effectively promote the densification of La(Co_1/2Ti_1/2)O₃ ceramics with low sintering temperature. At 1320 °C, La(Co_1/2Ti_1/2)O₃ ceramics with 0.75 wt% ZnO addition possesses a dielectric constant (_r) of 30.2, a Q × f value of 73,000 GHz (at 8 GHz) and a temperature coefficient of resonant frequency (τ_f) of −35 ppm/°C.     

Effect of ZrO2 and MgO added in alumina on the physical and mechanical properties of spark plasma sintered nanocomposite

The aim of the present research work was to investigate the effect on the properties such as density, surface roughness, microhardness, fracture toughness and microstructure added with MgO and ZrO₂ in an alumina matrix. The magnesia-zirconia toughened alumina spark plasma sintered nanocomposite samples were developed successfully and found the suppressing grain growth and crack free microstructure. No damage was found due to thermal shock up to 1350 °C. The amount of ZrO₂was added with 5 vol%, 10 vol% and 15 vol%, while MgO added with 0.5 vol%, 1 vol% and 2 vol% in an aluminamatrix. Each composition was weighed and mixed together. After that, the powders were pressed under the rapid heating at the sintering temperature of 1250 °C, 1300 °C and 1350 °C and for 5 min holding time under pressure of 60 MPa simultaneously. The optimum properties were found with the compositions of 10 vol% of ZrO₂, 1 vol% of MgO in the Al₂O₃ matrix. It showed highest relative density (99.68%), minimum surface roughness (1.123 μm), highest microhardness (19.46 GPa) and minimum average grain size (0.595 μm). The highest fracture toughness was found to be 6.7 MPa.m^1/2 the added with 15 vol% of ZrO₂,1 vol% of MgO in the Al₂O₃ matrix for the holding time 5 min and a sintering temperature of 1300 °C. The X-ray diffraction analyses indicate the presence of major phases were ZrO₂, α-Al₂O₃, MgO, magnesia phase with minor peaks of the secondary phase MgAl₂O₄. This was found due to chemical reactions between the composite constituents present in the matrix during the sintering. Uniform microstructure was observed using a field emission scanning electron microscope and obtained the sub-micron level of grain size without any significant increases of grain size. The developed compositehas high hardness and toughness to make it more suitable for applications such as ballistic armor and thermal barrier coating.     

The effect of particle size,sintering temperature and sintering time on the properties of Al–Al2O3 composites,made by powder metallurgy

Al₂O₃ is a major reinforcement in aluminum-based composites, which have been developing rapidly in recent years. The aim of this paper is to investigate the effect of alumina particle size, sintering temperature and sintering time on the properties of Al–Al₂O₃ composite. The average particle size of alumina were 3, 12 and 48 μm. Sintering temperature and time were in the range of 500–600 °C for 30–90 min. A correlation is established between the microstructure and mechanical properties. The investigated properties include density, hardness, microstructure, yield strength, compressive strength and elongation to fracture. It has been concluded that as the particle size of alumina is reduced, the density is increased followed by a fall in density. In addition, at low particle size, the hardness and yield strength and compressive strength and elongation to fracture were higher, compared to coarse particles size of alumina. The variations in properties of Al–Al₂O₃ composite are dependent on both sintering temperature and time. Prolonged sintering times had an adverse effect on the strength of the composite.     

Stress analysis of ceramic insulation coating on Cu/MgB2 wires for W&R MgB2 coils

Ceramic insulation coatings were produced on Cu/MgB₂ wires, which were fabricated by Hyper Tech Research Inc., using Continuous Tube Forming and Filling (CTFF) process, from the solution of Zr, and Y based organometalic compounds, solvent and chelating agent using reel-to-reel sol–gel technique for MgB₂ coils. Y₂O₃–ZrO₂/Cu/MgB₂ wires were annealed at 700 °C for 30 min with 5.8 °C/min heating rate under 4% H₂–Ar gas flow. Residual stresses were examined for Cu/MgB₂ wire and YSZ coatings with varying thicknesses. It was observed that displacement values are independent from YSZ thicknesses and the maximum effective stress value is in the Cu region. The surface morphologies and microstructure of samples were characterized using SEM. SEM micrographs of the insulation coatings revealed cracks, pinholes and mosaic structure.     

Electrochemical behavior and localized corrosion associated with Al7Cu2Fe particles in aluminum alloy 7075-T651

Initiation of localized corrosion upon high strength aluminum alloys is often associated with cathodic intermetallic particles within the alloy. Electrochemical measurements and metallurgical characterization have been made to clarify and quantify the physical properties of Al₇Cu₂Fe particles in AA7075-T651. Prior studies regarding either the stereology or electrochemical properties of Al₇Cu₂Fe are scarce. Quantitative microscopy revealed a significant population of Al₇Cu₂Fe in the alloy; comprising up to 65% of the constituent particle population and typically at a size of 1.7 ± 1.0 μm. It was determined that Al₇Cu₂Fe may serve as a local cathode in the evolution of localized corrosion of AA7075-T651 and is capable of sustaining oxygen reduction reactions at rates of several hundreds of μA/cm² over a range of potentials typical of the open circuit potential (OCP) of AA7075-T651 in NaCl solution of various concentrations and pH. The presence of Al₇Cu₂Fe leads to the development of pitting at the particle–matrix interface.