Properties of lead zirconate-alumina ‘nanocomposites’

Microstructures, Vickers hardness and dielectric properties of PbZrO₃ ceramics with co-additions of 0.5-5 vol% Al₂O₃ nanoparticles have been investigated. The additive inhibited grain growth, with average grain size decreasing from ∼13 μm for PbZrO₃ to ∼1 μm for the nanocomposites. The mode of fracture also changed, from predominantly inter-granular in PbZrO₃ to a mixed-mode of intra- and inter-granular fracture in the composite samples. Vickers hardness values increased from 2.9 GPa for PbZrO₃ to 4.1 GPa for the sample with 1 vol% Al₂O₃, but there was a more gradual increase for higher Al₂O₃ contents. Plots of relative permittivity versus temperature indicated subtle differences which were attributed to a chemical reaction between the additive and matrix during sintering. X-ray powder diffraction showed that lead aluminium oxides were the principal products of this reaction.     

Machinable Al2O3/BN composite ceramics with strong mechanical properties

Al₂O₃/BN composite ceramics with nano-sized BN dispersions ranging from 0 to 30 vol.% were successfully fabricated by hot-pressing α-Al₂O₃ powders with turbostratic BN (t-BN) coating, which was prepared through chemical processes using boric acid and urea. SEM observations revealed that the nano-sized hexagonal BN (h-BN) particulates were homogeneously dispersed within Al₂O₃ grains as well as at grain boundaries. Vickers hardness of materials decreased with an increase in BN content. The fracture toughness was improved but the fracture strength had a small decrease, in comparison to Al₂O₃ monolithic ceramics. The nanocomposite ceramics with BN content more than 20 vol.% exhibited excellent machinability, which could be drilled using conventional hard metal alloy drills. Drilling rates and normal forces demonstrate the ease of machining of these materials. The preliminary information on the relationship between microstructures and properties are provided. The mechanism of material removal is also discussed.     

Effect of a new additive on mechanical properties of hot-pressed silicon carbide ceramics

The mechanical properties and microstructure of SiC ceramics, hot pressed by simultaneously adding nano-SiC and oxides (MgO+Al₂O₃+Y₂O₃) or nitrate salts (Mg(NO₃)₂+Al(NO₃)₃+Y(NO₃)₃) as additives, were evaluated. The oxide additives system slightly influenced the mechanical properties of the ceramics, while the addition of nano-SiC lead to finer microstructure, and 5 vol.% nano-SiC changed the fracture mode from intergranular type to transgranular type. The ceramics with nitrate salts had fine, equiaxed grains with an average grain size larger than that of the system added oxides, thus inducing lower Viker’s hardness and flexural strength, while the presence of crystalline YAG phase improved the fracture toughness by 54.7%. Also, an observed increase in grain growth—with decreasing weight fraction of liquid and the grounded grain morphology in this system—confirmed a diffusion-controlled growth mechanism. Although the sample with the least amount of additives has the lowest relative density and largest grain size, its flexural strength did not drastically decrease. The influence of nano-SiC on the fracture toughness in the nitrate additive system was negligible.     

Influence of cobalt phase on thermal shock resistance of Al2O3-TiC composites evaluated by indentation technique

Cobalt-coated Al₂O₃ and TiC powders were prepared using an electroless method to improve resistance to thermal shock. The mixture of cobalt-coated Al₂O₃ and TiC powders (about 70 wt.% Al₂O₃-Co + 30 wt.% TiC-Co) was hot-pressed into an Al₂O₃-TiC-Co composite. The thermal shock properties of the composite were evaluated by indentation technique and compared with the traditional Al₂O₃-TiC composite. The composites containing 3.96 vol.% cobalt exhibited better resistance to crack propagation, cyclic thermal shock and higher critical temperature difference (ΔT_c). The calculation of thermal shock resistance parameters (R parameters) shows that the incorporation of cobalt improves the resistance to thermal shock fracture and thermal shock damage. The thermal physic parameters are changed very little but the flexure strength and fracture toughness of the composites are improved greatly by introducing cobalt into Al₂O₃-TiC (AT) composites. The better thermal shock resistance of the composites should be attributed to the higher flexure strength and fracture toughness.     

Reaction sintering fabrication of (AlN, TiN)-Al2O3 composite

The (AlN, TiN)-Al₂O₃ composites were fabricated by reaction sintering powder mixtures containing 10-30 wt.% (Al, Ti)-Al₂O₃ at 1420-1520°C in nitrogen. It was found that the densification and mechanical properties of the sintered composites depended strongly on the Al, Ti contents of the starting powder and hot pressing parameters. Reaction sintering 20 wt.% (Al, Ti)-Al₂O₃ powder in nitrogen in 1520°C for 30 min yields (AlN, TiN)-Al₂O₃ composites with the best mechanical properties, with a hardness HRA of 94.1, bending strength of 687 MPa, and fracture toughness of 6.5 MPa m^1/2. Microstructure analysis indicated that TiN is present as well dispersed particulates within a matrix of Al₂O₃. The AlN identified by XRD was not directly observed, but probably resides at the Al₂O₃ grain boundary. The fracture mode of these composites was observed to be transgranular.     

Microstructure and mechanical properties of titanium carbonitride whisker reinforced β-sialon matrix composites

The microstructure, hardness, fracture toughness and thermal shock resistance were investigated for 15 vol.% TiC_0.3N_0.7 whisker reinforced β-sialon (Si_6−zAl_zO₂N_8−z with z=0.6) composites with additions of three different volume fractions 2, 5 and 20 vol.%, of an yttrium-containing glass oxynitride phase. The composites were prepared by hot pressing at 1750°C for 90 min under a uniaxial pressure of 30 MPa in nitrogen atmosphere. The TiC_0.3N_0.7 whiskers were found to survive without deteriorating in morphology or reacting with the β-sialon matrix and/or the glass phase. The TiC_0.3N_0.7 whiskers had no obvious influence on the matrix microstructure, but their presence improved both the hardness and the fracture toughness of the composites. The highest hardness was obtained for the whisker composite with 2 vol.% glass phase (H_v=18.6 GPa). The fracture toughness and thermal shock resistance improved with increasing glass content. The whisker reinforced composite containing 20 vol.% glass showed the highest fracture toughness (K_1C=6.8 MPa m^1/2). No unstable crack extension occurred during the thermal shock test of the obtained composites in the temperature interval 90-700°C, but above 700°C severe oxidation of the whiskers precludes further evaluation of thermal shock properties by the indentation-quench method applied.     

Synthesis of submicron-sized spherical Y2O3 powder for transparent YAG ceramics

Spherical monodispersed, submicron-sized Y₂O₃ powder was prepared via a homogeneous precipitation method using nitrate and urea as raw materials. The structure, phase evolution and morphology of Y₂O₃ precursor and the calcined powder were studied by FTIR, TG/DTA, XRD and SEM methods. The sphere size of the precursor was about 250 nm and that of Y₂O₃ powder calcined at 800 °C for 2 h was about 200-210 nm. With the spherical Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder, high transparent YAG ceramics was fabricated by vacuum sintering at 1780 °C for 6 h through a solid-state reaction method. The in-line transmittances of the as-fabricated YAG ceramics at the wavelength of 1064 nm and 400 nm were 82.8% and 79.5%, respectively, which were much higher than that of the YAG ceramics with a commercial Y₂O₃ powder and a commercial Al₂O₃ ultrafine powder directly. The superior properties are attributed to the good morphology, dispersibility and uniform grain size of the as-prepared spherical Y₂O₃ powder, which matches that of the commercial Al₂O₃ powder.     

Microstructure and mechanical properties of small amounts of In2O3 reinforced Pb(ZrxTi1−x)O3 ceramics

Piezoelectric Pb(Zr_xTi_1−x)O₃ (PZT) ceramics with small amount (0.5-2.0 wt.%) of In₂O₃ are prepared by conventional sintering method. Based on X-ray diffraction analysis, the tetragonality of PZT matrix decreases with In₂O₃ content, indicating that In₂O₃ diffuses into PZT matrix. The microstructure of PZT matrix is significantly refined by doping small amounts of In₂O₃. The grain size reduction and the matrix grain boundary reinforcement are the probable mechanism responsible for the high strength and hardness in the PZT/In₂O₃ materials. The enhancement in Young’s modulus is attributed to In³⁺ substitution. The decreased tetragonality with In₂O₃ addition results in less crack energy absorption by domain switching and, hence, causes the small reduction in fracture toughness.     

The production of grain oriented lanthanum titanate (La2Ti2O7) ceramics by uniaxial hot-forging process for improved fracture toughness

The layered-structural ceramics, such as lanthanum titanate (La₂Ti₂O₇), have been known for their good electrical and optical properties at high frequencies and temperatures. However, few studies have been conducted on the mechanical properties of these ceramics. The interest in ceramic hot-forging (HF) has been greatly increased recently due to the enhancement in fracture toughness via bridging effect of oriented grains. In this study, grain oriented lanthanum titanate was produced by the hot-forging process. The characterizations of the samples were achieved by density measurement, scanning electron microscopy (SEM), optical microscopy, X-ray diffraction (XRD), Vickers indentation and three-point bending test. According to X-ray diffraction patterns, the orientation factor (f) was found to be 0.73 for certain hot-forging conditions resulting an improved fracture toughness. The improved fracture toughness of La₂Ti₂O₇ (3.2 MPa m^1/2) reached to the value of monolithic alumina (Al₂O₃) between 3 and 4 MPa m^1/2.     

Preparation and properties of negative thermal expansion Zr2WP2O12 ceramics

Using solid-state reaction method, Zr₂WP₂O₁₂ powder was synthesized for this study. The optimum heating condition was 1200 °C for 4 h. The obtained powder was compacted and sintered. The relative density of the Zr₂WP₂O₁₂ ceramics with no sintering additive was 60%. That of samples sintered with more than 0.5 mass% MgO was about 97%. The average grain size (D₅₀), as estimated from the polished surface of a sample sintered at 1200 °C for 4 h was about 1 μm. The obtained ceramics showed a negative thermal expansion coefficient of about −3.4 × 10⁻⁶ °C⁻¹. Young's modulus, Poisson's ratio, three-point bending strength, Vickers microhardness, and fracture toughness of the obtained ceramics were, respectively, 74 GPa, 0.25, 113 ± 13 MPa, 4.4 GPa and 2.3 MPa m^1/2.     

Effect of liquid-forming additives on the sintering and mechanical properties of Al2O3/3Y-TZP (30 vol.%) composite

Al₂O₃/3Y-TZP (30 vol.%) composite was pressurelessly sintered with addition of TiO₂MnO₂ and/or CaOAl₂O₃SiO₂ glass. It was found that TiO₂MnO₂ addition greatly enhanced the densification of the composite by the formation of a low-viscosity liquid at sintering temperature. In contrast, the high-viscosity liquid formed by CaOAl₂O₃SiO₂ glass improved mechanical properties because of its repressing effect on grain growth. The composite could be obtained at a temperature as low as 1400°C by co-doping with TiO₂MnO₂ and CAS glass. Bending strength of 552±64 MPa and fracture toughness of 6.03±0.22 MPa m^1/2 were obtained with a doping level of 2 wt.% TiO₂MnO₂ and 2 wt.% CAS glass.     

Mechanical properties and microstructure of Al2O3/TiAl in situ composites doped with Cr2O3

Al₂O₃/TiAl composites were successfully fabricated from powder mixtures of Ti, Al, TiO₂ and Cr₂O₃ by a hot-press-assisted exothermic dispersion method. The effect of the Cr₂O₃ addition on the microstructures and mechanical properties of Al₂O₃/TiAl composites was characterized, and the results showed that the Rockwell hardness, flexural strength and fracture toughness of the composites increased as the Cr₂O₃ content increased. When the Cr₂O₃ content was 2.5 wt%, the flexural strength and the fracture toughness attained peak values of 925 MPa and 8.55 MPa m^1/2, respectively. This improvement of mechanical properties was due to the more homogeneous and finer microstructure developed from the addition of Cr₂O₃ and an increase in the ratio of α₂-Ti₃Al to γ-TiAl matrix phases.     

Synthesis of CuCr and CuCrAg alloy with nano-ceramic dispersion by mechanical alloying and consolidation by laser assisted sintering

Cu-4.5Cr and Cu-4.5Cr-3Ag (in wt%) alloys without or with 10 wt% nanocrystalline Al₂O₃ and ZrO₂ dispersion have been synthesized by mechanical alloying or milling and consolidated by laser assisted sintering in Ar atmosphere. Microstructural characterization by scanning and transmission electron microscopy and phase analysis by X-ray diffraction suggest that the alloyed matrix undergoes significant grain growth after sintering while the dispersoids retain their ultrafine size and uniform distribution in the matrix. The dispersion of nano-Al₂O₃ is more effective than that of nano-ZrO₂ in enhancing the mechanical properties due to the smaller initial particle size of Al₂O₃ than that of ZrO₂. In general, laser sintering of mechanically alloyed Cu-4.5Cr and Cu-4.5Cr-3Ag alloys with 10 wt% nanocrystalline Al₂O₃ at 100 W laser power and 1-2 mm s⁻¹ scan speed yields the optimum combination of high density (7.1-7.5 mg m⁻³), hardness (165-225 VHN), wear resistance and electrical conductivity (13-20% IACS).     

On structure and mechanical properties of ultrasonically cast Al-2% Al2O3 nanocomposite

An investigation on the structure of an ultrasonically cast nanocomposite of Al with 2 wt.% nano-sized Al₂O₃ (average size ∼10 nm) dispersoids showed that the nanocomposite was consisting of nearly continuous nano-alumina dispersed zones (NDZs) in the vicinity of the grain boundaries encapsulating Al₂O₃ depleted zones (ADZs). The mechanical properties were investigated by nanoindentation and tensile tests. The nano-sized dispersoids caused a marginal increase in the elastic modulus, and a significant increase in the hardness (∼92%), and tensile strength (∼48%). Subsequent cold rolling to achieve a reduction ratio of 2 resulted in an appreciable increase in the hardness due to change in morphology of the microstructure. Estimation of the strength on the basis of inter-particle spacing, which was measured by transmission electron microscopy, could not be accounted for on the basis of Orowan mechanism, and therefore, strengthening mechanisms like local climb and/or cross slip might have a role in this room temperature (0.32T_M) deformation process.     

The effect of carbon nanotubes microstructures on reinforcing properties of SWNTs/alumina composite

Alumina reinforced with 1 wt% single-wall carbon nanotubes (SWNTs) was fabricated by hot-pressing. The fracture toughness of SWNTs/Al₂O₃ composite reaches 6.40 ± 0.3 MPa m^1/2, which is twice as high as that of unreinforced alumina. Nanoindentation introduced controlled cracks and the damage were examined by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SWNTs reinforcing mechanisms including CNT pullout, CNT fracture, CNT bridging and crack deflection were directly observed, and the relationship between carbon nanotubes microstructures in the matrix and mechanical properties was also discussed in detailed.     

Preparation of AlON-TiC composites via reaction-bonding

AlON-TiC composites were fabricated via a reaction-bonding technique, using Al, Al₂O₃ and TiC powders as the starting materials. A composite sample sintered at 1850 °C after nitriding is highly densified and the Vickers hardness and fracture toughness of the sample are about 1751.1 kg/mm² and 5.3 MPa m^1/2, respectively. The composition and microstructure of the sample are characterized by means of XRD and SEM/EDX.     

Improvement of dielectric thermal stability of BST ferroelectric material for tunable applications

100(1 − y)wt%(Ba_0.6Sr_0.4)(Ti_0.8Zr_0.2)O₃-100y wt%MgO (BSTZ20-MgO, y = 0.4, 0.5, 0.6, 0.7) composite ceramics were synthesized via a solid-state reaction route, aiming at improving the dielectric thermal stability of BST for tunable applications. Excellent dielectric thermal stability (low temperature coefficient of permittivity value) was gained in this system. According to our experiment, diffuse phase transition (DPT) induced by Zr ion substitution, ferroelectric-dilution effect of MgO phase and grain size refinement were considered as contributions to this good dielectric thermal stability.     

Pretreatment and sintering of Si3N4 powder synthesized by the high-temperature self-propagation method

Self-propagation high-temperature synthesis (SHS) was applied for the synthesis of low-cost Si₃N₄ powder. The powder was purified and ground until its particle size reached submicron levels and its purity reached 98%. Using this pretreated powder, with α/β = 60/40 content, fully dense Si₃N₄ ceramics, having improved mechanical properties, were obtained by liquid-phase sintering in the presence of (Y, La)₂O₃-AlN. The mechanical properties achieved finally were as follows: strength, 784 MPa; hardness, 15.1 GPa; and fracture toughness, 5.2 MPa m^0.5. The behaviors of the SHS-Si₃N₄ powders before and after the pretreatment were compared. The relation between microstructure and mechanical properties of the sintered specimens and the effect of different β content in the powder on the sintering process of Si₃N₄ were also studied.     

Mechanical and thermal properties of LaMgAl11O19

Lanthanum magnesium hexaaluminate (LaMgAl₁₁O₁₉) powders were synthesized successfully at 1300 °C for 4 h by solid-state reaction, and LaMgAl₁₁O₁₉ ceramic was prepared at 1700 °C for 6 h by pressureless sintering. Phase composition, microstructure, mechanical and thermophysical properties of LaMgAl₁₁O₁₉ ceramic were investigated. Results show that the flexural strength and fracture toughness of LaMgAl₁₁O₁₉ ceramic are 353.3 ± 12.5 MPa and 4.60 ± 0.46 MPa m^1/2. Young's Modulus and Poisson ratio is 295 GPa and 0.23, respectively. The linear thermal expansion coefficient of LaMgAl₁₁O₁₉ ceramic from 473 K to 1473 K is 9.17 × 10⁻⁶/K, and thermal conductivity at 1273 K is 2.55 W/m K.     

Ca3Co4O9 ceramics consolidated by SPS process: Optimisation of mechanical and thermoelectric properties

Ca₃Co₄O₉ (349) thermoelectric (TE) oxide ceramics were successfully prepared by Spark Plasma Sintering process. The effects of the uniaxial pressure (30-100 MPa), the dwell temperature (700-900 °C) and the cooling rate were investigated. Microstructure analyses have revealed strong enhancements of the bulk density as the pressure level and the applied temperature during the SPS process are increased. Mechanical properties were investigated by using instrumented nanoindentation and three point bending tests. Hardness, elastic modulus, strength and fracture toughness were shown to improve drastically and depend on the processing parameters. Thermal expansion measurements reveal a noticeable anisotropy induced by unidirectional hot pressing. The mechanical, thermal and thermoelectric properties were correlated to the microstructure and crystallographic texture of the resulting ceramics.