Composites Derived from Zirconia Nanopowders Stabilized with Yttria and Containing Alumina Particles Incorporated Physically or Chemically

Two methods of incorporating Al₂O₃ inclusions into a polycrystalline matrix of tetragonal zirconia stabilized with yttria (3Y-TZP) were used, and their influence on the microstructure and properties of TZP/Al₂O₃ composites has been studied. The first method consisted in the physical mixing of the component powders by means of intensive milling. The second method utilized the possibilities of the coprecipitation method of chemically homogeneous deposits followed by their calcination. An aqueous solution of zirconium, yttrium, and aluminum salts was used. Green compacts were shaped by cold isostatic pressing under a pressure of 300 MPa, and then they were sintered under no pressure for 2 h at 1500–1650°C in air. The powders were also consolidated using hot pressing under 25 MPa in argon and under the same heating cycle as in the case of pressureless sintering. The composites studied contained from 0 to 20 vol % of alumina inclusions, whose sizes depended on the powder preparation method. The morphology and phase composition of the powders and the microstructure of the green compacts and sintered materials were characterized. Bending strength, fracture toughness, and wear were measured. The coprecipitation method enabled us to produce composites that contained nanosize alumina inclusions. The inclusions derived from this method were much smaller than those derived from the physical mixing method (d ₅₀ = 0.21 ± 0.01 and 0.32 ± 0.2 µm, respectively). The reduction in the alumina inclusion size nearly to the nanometer level did not increase the fracture strength and fracture toughness of the composites. The density of the composites and the size of microstructural flaws were the critical factors controlling the fracture strength. The highest strength value, namely, 1.7 ± 0.2 GPa, was measured for the TZP containing 5 vol % of alumina particles incorporated by means of the physical mixing process. The 20 vol % content of alumina particles increased the wear resistance of the 3Y-TZP materials by 51 and 41% for the physical and chemical methods of inclusion incorporation, respectively.Original English Text Copyright © 2005 by Fizika i Khimiya Stekla, W. Pyda, Brzezinska-Miecznik, Bucko, Pedzich, A. Pyda.This article was submitted by the authors in English.     

Fracture behaviour of alumina-YAG particulate composites

Particulate composites of the Al₂O₃–YAG system were produced by precipitation of the yttrium oxide precursor in the aluminium oxide suspension. The solid state reaction took place during thermal treatment of the resulting powder and led to the creation of the YAG phase. This method allowed fine and homogenously distributed YAG inclusions within the alumina matrix to be obtained. The performed investigations involved determining of the critical stress intensity factor (K_IC), Vickers hardness and bending strength of the materials. The composites showed higher hardness (HV) than α-Al₂O₃. The presence of YAG inclusion in the amount higher than 7.5 vol.% improved also fracture toughness when compared to polycrystalline alumina. In the case of the material with the best mechanical properties measurements of subcritical cracking were conducted and the threshold value of K_IC (K_I0) was determined.     

Abrasive wear of Al2O3–SiC and Al2O3–(SiC)–C composites with micrometer- and submicrometer-sized alumina matrix grains

The response of Al₂O₃, Al₂O₃–SiC–(C) and Al₂O₃–C nanocomposites to grinding was investigated in terms of changes of quality of ground surfaces and of the weight losses with time. The study used monolithic polycrystalline aluminas as references, and alumina-based composites with nanosized SiC and C inclusions and with alumina matrix grain size varying from submicrometer to approximately 4 μm. The studied materials can be roughly divided into two groups. Materials with submicrometer alumina matrix grains (Group 1) wear predominantly by plastic deformation and grooving. Coarse-grained materials (Group 2) wear by mixed wear mechanism involving crack initiation and interlinking accompanied by grain pull-out, plastic deformation and grooving. The wear rate of composites increases with increasing volume fraction of SiC. The Group 2 materials wear much faster then those with submicron microstructure. In all cases (with one exception) the wear resistance of composites was higher than that of pure aluminas of comparable grain sizes used as reference materials.     

Toughening of zirconia/alumina composites by the addition of graphene platelets

A study on graphene platelet/zirconia-toughened alumina (GPL/ZTA) composites was carried out to evaluate the potential of the new structural materials. GPL–ZrO₂–Al₂O₃ powders were obtained by ball milling of graphene platelets and alumina powders using yttria stabilized ZrO₂ balls. Samples were sintered at different temperatures using spark plasma sintering. Fracture toughness was determined by the single-edge notched beam method. The results show that the GPLs are uniformly distributed in the ceramic matrix and have survived high temperature sintering processes. Several sintering experiments were carried out. It is found that at 1550 °C, GPL/ZTA composites were obtained with nearly full density, maximum hardness and fracture toughness. A 40% increase in fracture toughness in the ZTA composite has been achieved by adding graphene platelets. The toughening mechanisms, such as pull out, bridging and crack deflection, were observed and are discussed.     

Effect of microstructure and mechanical properties on wear behavior of plasma-sprayed Cr2O3-YSZ-SiC coatings

In this study, the microstructure and mechanical properties of the atmospheric plasma-sprayed Cr₂O₃ (C), Cr₂O₃-20YSZ (CZ), and Cr₂O₃-20YSZ-10SiC (CZS) coatings were evaluated and also compared with each other, so as to explain the coatings wear behavior. Microstructural evaluations included X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) equipped with energy dispersive X-ray spectroscopy (EDX) and porosity measurements. Mechanical tests including bonding strength, fracture toughness, and micro-hardness tests were used to advance our understanding of the correlation between the coatings properties and their wear behavior. The sliding wear test was conducted using a ball-on-disk configuration against an alumina counterpart at room temperature. Addition of multimodal YSZ and subsequent SiC reinforcements to the Cr₂O₃ matrix resulted in an increase in the fracture toughness and Vickers micro-hardness, respectively. It was found that the composite coatings had comparable coefficients of friction with pure Cr₂O₃ coatings. When compared with the C coating, the CZ and CZS composite coatings with higher fracture toughness exhibited superior wear resistance. Observation of the wear tracks of the coatings indicated that the lower wear rates of the CZ and CZS coatings were due to the higher plastic deformation of the detached materials. In fact, improvement in the wear resistance of the composite coatings was attributed to a phase transformation toughening mechanism associated with tetragonal zirconia which created more ductile tribofilms during the wear test participated in filling the pores of coatings.     

Large-scale fine structural alumina matrix ceramic guideway materials improved by diopside and Fe2O3

Diopside and Fe₂O₃ were introduced in alumina matrix ceramic materials. Large-scale fine structural alumina matrix ceramic guideway materials were fabricated by the technology of pressureless sintering, during which liquid phase sintering took place and new phases such as 3Al₂O₃·2SiO₂, CaO·Al₂O₃·2SiO₂ and CaO·6Al₂O₃ were produced by the chemical reactions taking place among alumina and the additives. The hardness, the fracture toughness and the bending strength of the guideway products were tested. The influences of diopside and Fe₂O₃ additions were studied by microstructural observations and mechanical properties evaluations. Meanwhile, the expected improvement of mechanical properties compared with pure alumina was indeed observed. The fracture mechanism and porosity of large-scale fine structural alumina matrix ceramic guideway materials were analyzed.     

Mechanical properties and sliding wear behaviour of Al2O3-SiC nanocomposites with 3–20 vol% SiC

Al₂O₃/SiC composites containing different volume fractions (3, 5, 10, 15, and 20 vol%) of SiC particles were produced by conventional mixing of alumina and silicon carbide powders, followed by hot pressing at 1740 °C for 1 h under the pressure of 30 MPa in the atmosphere of Ar. The influence of the volume fraction and size of SiC particles (two different powders with the mean size of SiC particles 40 and 200 nm were used), and final microstructure on mechanical properties and dry sliding wear behaviour in ball-on-disc arrangement were evaluated. The properties of the composites were related to a monolithic Al₂O₃ reference. Microstructure of the composites was significantly affected by the volume fraction of added SiC, with the mean size of alumina matrix grains decreasing with increasing content of SiC particles. The addition of SiC moderately improved the Vickers hardness. Fracture toughness was lower with respect to monolithic Al₂O₃, irrespective of the volume fraction and size of SiC particles. Al₂O₃/SiC nanocomposites conferred significant benefits in terms of wear behaviour under the conditions of mild dry sliding wear. Wear resistance of the alumina reference was poor, especially at the applied load of 50 N. The wear rates of composites markedly decreased with increasing volume fraction of SiC. Wear of the composites was also influenced by the material of counterparts, especially their hardness, with softer counterparts resulting in lower wear rates. All composites wore by a combination of grain pull-out with plastic deformation associated with grooving and small contribution of mechanical wear (micro-fracture). No influence of SiC particle size on wear rate or mechanism of wear was observed in the materials with identical volume fractions of SiC.     

Effect of yttria doping on the microstructure and mechanical properties of Al2O3–FeAl2O4 nanocomposites developed via solid state precipitation

We have recently reported the production of Al₂O₃-matrix nanocomposites via solid state precipitation of nanosized FeAl₂O₄ particles within the matrix grains during aging of Al₂O₃–10 wt.% Fe₂O₃ solid solutions in a reducing atmosphere (N₂ + 4% H₂). In addition to these nanoparticles, however, coarse micron-sized FeAl₂O₄ particles were present along the matrix grain boundaries. In the present work, we show that the addition of ～250 ppm yttria to the solid solutions suppressed the development of these intergranular particles, reducing their size by a factor of ～2 with optimum aging. A fracture toughness improvement by 45% and flexural strength improvement by 50% with respect to monolithic Al₂O₃ were recorded with the yttria-containing nanocomposite developed by aging for 20 h at 1450 °C. Aging also improved the hardness with respect to the solid solution. The change in fracture mode in the presence of the nanosized intragranular particles was believed to be the major contributing factor towards the improvement in toughness and therefore the strength. The higher strengths obtainable in the presence of yttria were attributed to the reduction of intergranular precipitate size relative to yttria-free nanocomposites.     

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.     

Wear properties and microstructures of alumina matrix composite ceramics used for drawing dies

The alumina matrix ceramics used for drawing dies were prepared by hot-press sintering method. The ceramics materials were made of Al₂O₃/TiC, Al₂O₃/(W,Ti)C and Al₂O₃/Ti(C,N). Mechanical and friction properties of these materials were tested and measured. The experiments for testing friction properties were carried on wear and tear machine. Mechanisms of frictions were analyzed with scanning electron microscope. Results showed that the alumina matrix composite ceramics have good physical and mechanical properties for used as drawing dies. Measured friction coefficients of alumina matrix composite ceramics showed a trend of decline and kept the value of 0.4–0.5 with the rotating speed of 550 rpm. Alumina matrix composite ceramics have smaller wear rate, while the wear rates of Al₂O₃/TiC and Al₂O₃/(W,Ti)C decrease gradually with a rising rotation speed. The wear of alumina matrix ceramics was severe at deformation zone. The primary wear behaviors of alumina matrix ceramics are scraping and furrowing. Even though the mechanisms for wear different, abrasive and adhesive wear were found to be the predominant wear mechanisms for the ceramic drawing die.     

Processing and mechanical properties of Al2O3–5 vol.% Cr nanocomposites

The use of chromium (III) acetylacetonate as a source of nanometre sized chromium particles for the production of Al₂O₃–5 vol.% Cr nanocomposites has been investigated. The details of the processing procedure are crucial in determining the mechanical properties of the composite. The highest strength and fracture toughness, 736±29 MPa and 4.0±0.2 MPa m^1/2, respectively, were obtained for the nanocomposite hot pressed at 1450 °C. It is shown that the strengthening in Al₂O₃–5% Cr nanocomposites mainly results from microstructure refinement in that the mean alumina matrix grain size in the optimum composite was 0.68 μm compared with a grain size of 3.6 μm in the monolithic alumina hot pressed under identical conditions. Crack bridging and crack deflection by the nano-sized Cr particles did not occur to any significant extent. The slight improvement in fracture toughness may result from the observed change in fracture mode from intergranular fracture for monolithic alumina to transgranular failure for the nanocomposites.     

Mechanical properties of SiCp/Al2O3 ceramic matrix composites prepared by directed oxidation of an aluminum alloy

Silicon carbide particulate reinforced alumina matrix composites were fabricated using DIrected Metal OXidation (DIMOX) process. Continuous oxidation of an Al-Si-Mg-Zn alloy with appropriate dopants along with a preform of silicon carbide has led to the formation of alumina matrix surrounding silicon carbide particulates. SiC_p/Al₂O₃ ceramic matrix composites fabricated by the DIMOX process, possess enhanced mechanical properties such as flexural strength, fracture toughness and wear resistance, all at an affordable cost of fabrication. SiC_p/Al₂O₃ matrix composites were investigated for mechanical properties such as flexural strength, fracture toughness and hardness; the composite specimens were evaluated using standard procedures recommended by the ASTM. The SiC_p/Al₂O₃ ceramic matrix composites with SiC volume fractions from 0.35 to 0.43 were found to possess average bend strength in range 158-230 MPa and fracture toughness was found to be in range of 5.61-4.01 MPa√m. The specimen fractured under three-point loading as observed under scanning electron microscope was found to fail in brittle manner being the dominant mode. Further the composites were found to possess lower levels of porosity, among those prepared by DIMOX process.     

Corrosion- and wear-resistant properties of Ni–Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composite coatings containing various forms of alumina

This article describes the effect of the addition of different phases of alumina particles on the properties of electrodeposited Ni–Al₂O₃ composite coatings. The corrosion- and wear-resistant properties of Ni–Al₂O₃ composite coatings electrodeposited from a nickel sulfamate bath containing (i) alpha-alumina particles (Ni–Al₂O₃-1), (ii) gamma-alumina particles (Ni–Al₂O₃-2), and (iii) mixture of alpha, gamma, and delta alumina particles (Ni–Al₂O₃-3) have been studied. The potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) studies showed superior corrosion resistance of Ni–Al₂O₃-2 composite coatings compared with other two coatings. The SEM images and EDAX spectra also corroborated well with the observed corrosion results. The pin-on-disk wear studies showed improved wear resistance of Ni–Al₂O₃-1 composite coating containing alpha alumina compared with other two coatings. The transfer of material from the pin onto the disk was evident from the optical microscopy images of the wear tracks and Raman spectra of the wear track. This study shows that the addition of pure gamma-alumina particles enhances the corrosion resistance, and that pure alpha-alumina particles enhance the wear resistance of Ni composite coatings to a greater extent.     

Zirconia-strengthened yttria ceramics for plasma chamber applications

Yttria (Y₂O₃) is the most popular lining material for the inner walls of plasma chambers, owing to its well-known resistance against corrosion by reactive fluorinated plasma. Yttria has a relatively lower toughness and strength compared to alumina (Al₂O₃) and zirconia (ZrO₂). The present work aims to explore the strengthening and toughening of yttria by doping with zirconia, while retaining its good corrosion resistance. Ceramics with zirconia to yttria molar ratios of 2:8 and 5:5 (named 20ZY and 50ZY, respectively) were fabricated by pressure sintering in Ar atmosphere. The corrosion of the prepared ceramics in reactive fluorinated plasma (C₄F₈/CHF₃/Ar) was investigated and compared with that of yttria as a control. The results indicated that 20ZY exhibited excellent corrosion resistance, comparable to that of yttria, while the fracture toughness and flexural strength showed increases of 87% and 44%, respectively. 50ZY exhibited a further improvement in fracture toughness and flexural strength, but at the price of a much lower resistance against plasma corrosion. A percolation model was proposed to interpret the observed plasma corrosion behaviors.     

In situ Incorporation of Sintering Additives in Si3N4 Powder by a Combustion Process

A novel approach for in-situ incorporation of Al₂O₃ and Y₂O₃ additives into Si₃N₄ powder by a combustion technique is described. A suspension is made by mixing an alcoholic solution of Al/Y nitrates and citric acid with Si₃N₄ powder. The suspension forms a gray precipitate upon heating at 60°C. This precipitate undergoes a combustion reaction upon heating at 200°C and produces an amorphous phase of Al₅Y₃O₁₂ (YAG) on the Si₃N₄ powder. The amorphous YAG phase shows a homogeneous distribution on the Si₃N₄ powder. Pellets of the composite powder are fabricated by cold isostatic pressing and sintered at 1750°C for 2 h at 5 bar of nitrogen pressure. The microstructure of the sintered body prepared by this method reveals a high density, the fracture toughness (K_1C) is increased by 13·4%, compared to that of a sintered Si₃N₄ body formed with identical amounts of alumina and yttria additives prepared by planetary milling.     

Slow crack growth and hydrothermal aging stability of an alumina-toughened zirconia composite made from La2O3-doped 2Y-TZP

A very tough zirconia matrix is interesting to fabricate alumina-toughened zirconia (ATZ) and composites generally processed from 3Y-TZP do not exhibit very high toughness. The strategy of lowering the yttria content to increase toughness however is normally associated with an increased hydrothermal aging susceptibility. In this work, a 0.4 mol% La₂O₃ doped 2Y-TZP matrix was investigated to realize a 20 wt.% alumina toughened zirconia composite with a substantially high aging resistance. The higher transformation toughening in the composite shifted the V-K_I towards higher K_I values, while preserving the slope of the curve, resulting in a threshold K_I0 of 4.0 MPa m^1/2 and fracture toughness (K_IC) of 7.1 MPa m^1/2. These composites can offer a better compromise between aging and crack resistance than traditional 3Y-TZPs and plain ATZ composites without La₂O₃ doping.     

Effect of yttria on crystallization and microstructure of an alumina–YAG fiber prepared by aqueous sol–gel process

Continuous fiber development is needed for high performance and high temperature composites. Various methods have been used to make ceramic fibers. In this research, composite fibers (yttrium aluminum garnet (YAG)/Al₂O₃) were prepared by a sol–gel method using aqueous solution. They were synthesized from aluminum salt, aluminum metal, yttrium oxide and water used as solvent. Transparent gel fibers were obtained by immersing a thin wire into the viscous sol, then pulling it out by hand. The obtained fibers contained very fine grains with diameter ranging from 10 to 80 μm after heat treatment. When yttria content was increased, the crystallization of YAG shifted to a lower temperature, whereas the transformation temperature to α-Al₂O₃ shifted to a higher temperature. Nevertheless, the fibers with different amounts of yttria contained alumina and YAG after heat treatment at 1400 °C. The composite fibers had vermicular structure and were denser than alumina fibers. The yttria percent concerning the limits of this study (≤10 wt%) effected on fiber diameter. As the yttria content was increased, the fiber diameter increased, whereas grain size and densification of the composite fibers decreased.     

Effect of Y2O3 addition on tribological properties of plasma sprayed Al2O3-13% TiO2 coating

The effect of Y₂O₃ addition on structure, mechanical properties and tribological properties of Al₂O₃-13 wt% TiO₂ coating was investigated. The addition of 20 wt% Y₂O₃ resulted in better densification, stabilization of alpha (α) alumina phase and improvement in fracture toughness of Al₂O₃-13 wt% TiO₂ coating. Abrasive wear tests were performed over a range of loads and sliding speeds. The stabilization of α alumina phase further increased with an increase in severity of wear test conditions, as noted from X-Ray Diffraction (XRD) and X-Ray Photoelectron Spectroscopy (XPS) analysis of worn coatings. Al₂O₃-13 wt% TiO₂-20 wt% Y₂O₃ coating displayed lower friction coefficient and lower abrasive wear rate than Al₂O₃-13 wt% TiO₂ coating, which was due to synergistic effect of α alumina phase and formation of magneli phase oxide of titanium; Ti₂O₃. Friction energy map was used to rationalize observed wear rates, to identify different regimes of wear and degradation modes of coatings.     

Phase and microstructural evolution of yttrium-doped nanocrystalline alumina: A contribution of advanced microscopy techniques

Well-dispersed nano-crystalline transition alumina suspensions were mixed with yttrium chloride aqueous solutions, with the aim of producing Al₂O₃-Y₃Al₅O₁₂ (YAG) composite powders. DTA analysis allowed to highlight the role of yttrium on the α-phase crystallization path. Systematic XRD and HRTEM analyses were carried out in parallel on powders calcined in a wide temperature range (600-1300 °C) in order to follow phase and microstructural evolution. A thin, homogeneous yttrium-rich layer was yielded on the alumina particles surface; yttrium diffusion into the alumina matrix was negligible up to 1150 °C whereas, starting from 1200 °C, aggregates of partially sintered alumina particles appeared, stuck together by yttrium-rich thin films. Moreover, in the yttrium-richer zones, such as alumina grain boundaries and triple joints, yttrium-aluminates precipitated at alumina particles surface. Finally, at 1300 °C, alumina-YAG composite powders were produced, in which YAG was homogenously distributed among the alumina grains.     

Mechanical alloying of alumina–yttria powder mixtures

Mechanical alloying has been used to prepare powder mixtures of alumina and yttria as a means to create composites with a dominant matrix phase together with small particles of a dispersed second phase. The yttria–alumina system, containing five possible phases, has the potential for creating eight combinations of matrix and dispersed phases. Here compositions designed to give YAlO₃ (YA) dispersed in Y₃Al₅O₁₂ (Y₃A₅ i.e. YAG) or Y₄Al₂O₉ (Y₂A) were studied. After milling with steel tools for times up to 8 h, the powders were subjected to thermal cycles up to 1500°C during which the phase evolution was monitored using X-ray diffractometry (including high-temperature XRD) and differential thermal analysis. During milling the original crystal structures were quickly broken down, in some cases partially replaced by an intermediate structure after milling. Upon subsequent heating the milled mixtures crystallized to give the expected phases, YA in Y₃A₅ and YA in Y₂A respectively, but the reaction route was seen to be different depending on the amount of amorphization of the yttria. Contamination by iron was seen to affect the phase distribution and the lattice parameters.