Micro-scale fracture toughness of textured alumina ceramics

Enhanced fracture resistance of textured alumina is ascribed to crack deflection along grain boundaries. In this work, we quantify and compare the micro-scale fracture toughness of textured alumina grains and grain boundaries by micro-bending tests. Notched micro-cantilevers were milled from single alumina textured grains (perpendicular to the [0001] direction) and across several textured grains (along the [0001] direction), using a focused ion beam technique. Bending tests were performed with a nanoindenter. A shape function for notched pentagonal-shaped cantilevers was developed using finite element analysis. The critical stress intensity factor at the notch tip was determined based on the measured fracture loads. The micro-scale fracture toughness of the textured alumina grain boundaries (2.3 ± 0.2 MPa m^1/2) was about 30% lower than that of the grains (3.3 ± 0.2 MPa m^1/2). These findings at the micro-scale are paramount for understanding the macroscopic fracture behaviour of textured alumina ceramics.     

Effect of second phase addition of zirconia on the mechanical response of textured alumina ceramics

The effect of second phase addition of zirconia on the mechanical response of textured alumina was analysed. Highly textured monolithic tape-casted alumina was obtained through templated grain growth. Compositions containing 1, 2, 5 and 10 vol% of (i) non-stabilised and (ii) 3 mol% yttria-stabilised zirconia, respectively, were investigated. XRD analyses revealed that the texture degree decreased with increasing second phase content. Microstructural analysis showed zirconia grains inside the textured alumina grains for contents ≤ 5 vol%, affecting the mode of fracture. Fracture toughness of textured alumina significantly decreased with the addition of a second phase. In the case of non-stabilised zirconia, the constraint of the alumina matrix and the small grain size led to a lower fracture toughness in comparison to monolithic textured alumina (K_Ic = 5.1 MPa m^1/2). The fracture toughness of textured alumina with 3 mol% yttria-stabilised zirconia was comparable to equiaxed alumina, independent of the content ratio (K_Ic = 3.5 MPa m^1/2).     

Mechanical properties of ceria-calcia stabilized zirconia ceramics with alumina additions

Ceria-stabilized zirconia-based composites have been developed aiming to obtain ceramic materials with enhanced hardness, strength, fracture toughness, and resistance to low temperature degradation. These composites are based on ceria-calcia stabilized zirconia (10 mol% CeO₂-1 mol% CaO TZP) and α-alumina (0?15 wt%) as a second phase. Raw materials in the form of powders were dispersed through ball milling, dried by slip casting, and subsequently grounded before being pressed and conventionally sintered at 1450 °C. Compared to the strength and hardness of 10Ce-TZP ceramics (typically 500 MPa and 6 GPa), an increase was observed for all compositions, especially for 10Ce-1CaO-5Al₂O₃ (739 MPa and 10.2 GPa). Single Edge V-Notched Beam fracture toughness values ranged from 5.1 to 6.6 MPa?√m, indicating a loss of transformability for all compositions. As in 10Ce-1CaO-TZP co-doped ceramics, the aging resistance of all alumina-containing composites was also excellent.     

Prediction of edge and tunnelling crack formation in layered ceramics using a stress-energy fracture criterion

A coupled stress-energy criterion is utilized to predict initiation of both edge and tunnelling cracks in layered ceramics containing thermal residual stresses. Edge (surface) cracks may originate in layers having high compressive in-plane stresses while tunnelling (internal) cracks may form in layers with high tensile in-plane stresses. This work investigates the influence of both the residual stresses magnitude and layer thickness on the formation of surface cracks and provides a design map defining safe regions where no cracks will be present in the sintered multilayer architecture upon reaching the room temperature. Necessary stress and energy inputs to evaluate the coupled criterion are calculated using the finite element method. Simulation results are validated with experimental observations on sample architectures fabricated with layers of various thicknesses and in-plane thermal residual stresses. The good agreement demonstrates the potential of the stress-energy coupled criterion for designing crack-free multi-layered ceramic architectures.     

Scratch behaviour of graphene alumina nanocomposites

The scratch resistance behaviour of alumina-graphene nanoplatelet (GNP) (0.5, 2 and 5?vol.-%) composites was investigated using a Rockwell indenter with normal applied loads ranging from 1 to 200?N. The alumina-GNP composites behaved differently during scratch testing depending on the normal applied load. The coefficient of friction of the composites did not change much at low normal loads but increased with increasing amount of GNP in the alumina matrix for high normal loads. The addition of GNP contributed to improved scratch resistance of alumina nanocomposites only for low loads below ～97?N. This correlates with the mechanical properties of the composites. As the applied load increased, the scratch resistance of the GNP composites decreased due to the presence of weakly bonded grain boundaries in the alumina matrix, which enhanced chipping of material.     

Solid particle erosion behaviour of high purity alumina ceramics

The solid particle erosion behaviour of a high purity, cold isostatically pressed ceramics, CIP-Al₂O₃, is studied in this paper. The influence of particle properties, such as hardness and shape, on erosion is examined, as well as the effect of varying the impingement angle of the erodent stream on the weight loss of alumina ceramics samples. Therefore, the erosive wear behaviour was studied at five different impact angles (30°, 45°, 60°, 75° and 90°), using SiC and SiO₂ particles as erodents.The material loss during solid particle erosion is measured by changes in surface roughness, surface morphology and mass loss.The surface roughness and topography of the eroded Al₂O₃ ceramics were recorded using a profilometer.Scanning electron microscopy (SEM) was used to examine the features of eroded surfaces and to ascertain erosion mechanisms of the tested alumina samples.The results indicate that hard, angular SiC particles cause more damage than softer, more rounded SiO₂ particles. It was found that maximum erosion by both types of particles occurs at an impact angle of 90°.     

92黄色氧化铝陶瓷的研制及其显微结构分析

将ZrO2＋Y2O3复合添加剂加入到92白色氧化铝陶瓷基料中,经常压烧结制备了黄色氧化铝陶瓷。实验结果表明：当添加0．6％（质量分数,下同）ZrO2和0．3％Y2O3时,可以使氧化铝陶瓷呈现均匀的黄色。通过SEM检测对氧化铝陶瓷的显微结构进行了分析。     

Dilatometric study of anisotropic sintering of alumina/zirconia laminates with controlled fracture behaviour

Al₂O₃ and ZrO₂ monoliths as well as layered Al₂O₃/ZrO₂ composites with a varying layer thickness ratio were prepared by electrophoretic deposition. The sintering shrinkage of these materials in the transversal (perpendicular to the layers, i.e. in the direction of deposition) as well as in the longitudinal (parallel with layers interfaces) direction were monitored using high-temperature dilatometry. The sintering of layered composites exhibited anisotropic behaviour. The detailed study revealed that sintering shrinkage in the longitudinal direction was governed by alumina (material with a higher sintering temperature), whilst in the transversal direction it was accelerated by the directional sintering of zirconia layers. For interpretation of such anisotropic sintering kinetics, the Master Shrinkage Curve model was developed and applied. Crack propagation through laminates with a different alumina/zirconia thickness ratio was described with the help of scanning electron microscopy and confocal laser microscopy.     

High-temperature elasticity of fibrous ceramics with a bird's nest structure

New fibrous ceramics with polycrystalline mullite fibers as the matrix and silica–boron sols as the high temperature binder, which was inspired by the bird's nest structure in nature, were synthesized. The most important structure characteristic of this fibrous material is that the silica–boron binder only fixed the fibers at the crossing points rather than filled the pores among the fibers. The elastic behavior was investigated, both at room temperature and elevated temperature. Compared to conventional ceramic matrix composites, the samples show a much higher degree of elasticity because of the bending of the fibers. The rebound resilience decreased slowly with the increase of the temperature, but it still remained 86% of that at ambient temperature at 1000 °C. The sample exhibits good elasticity performance, relatively high strength (2.25 MPa) and high porosity (83%) indicating it is a potential high-temperature seal material.     

Improved microstructure of alumina ceramics prepared from DBD plasma activated powders

Submicron Al₂O₃ powders were activated by Diffuse Coplanar Surface Barrier Discharge (DCSBD) plasma. The influence of the plasma treatment on the powder properties and their impact on the microstructure of dry and wet shaped ceramics were investigated. Raman and FTIR analyses of treated powders showed a substantial increase of the powder’s surface hydroxylation, surface cleaning, and the presence of adsorbed NO_x originating from the DCSBD. Sintering of the dry shaped plasma treated powders did not influence sintering behavior. On the other hand, the plasma treated powder was able to form stable water suspension without any chemical stabilization aid. Slip cast samples exhibited finer pore size distribution, a higher sinterability, and a finer final microstructure. The grain size of slip casted plasma treated powder was reduced by a factor of 1.7, which facilitated a grain size of 0.68 μm at the relative density of 99.54% t.d. obtained by pressure-less sintering.     

Novel strategy for the enhancement of anti-counterfeiting ability of photochromic ceramics: Sm3+ doped KSr2Nb5O15 textured ceramics with anisotropic luminescence modulation behavior

Sm³⁺ doped KSr₂Nb₅O₁₅ (KSN-Sm) textured ceramics with anisotropic photochromic and luminescence modulation behaviors provided a new strategy for the enhancement of anti-counterfeiting ability. The KSN-Sm textured ceramics were fabricated by the tape casting technology, which exhibited obvious grain-orientation, with Lotgering factor f_(00l) of 0.62. The textured sample possessed evident difference of reflectivity, photochromic, luminescent and luminescence modulation properties among various grain-orientated directions. The difference of luminescent emission intensity was over than 30 % and the luminescence modulation ratios △R_t are 75.3 % and 63.3 % along paralleled and vertical [00l] orientations, respectively. These optical anisotropies were attributed to the different refractive indexes, distributions of photochromic centers and energy transfer rates at various orientations. This work is hopeful to achieve the multidirectional data recording and enhancement of anti-counterfeiting ability of photochromic ceramics by the anisotropic properties of textured ceramics.     

Effect of substrate temperature on microstructure and optical properties of nanocrystalline alumina thin films

Aluminum oxide (Al₂O₃) thin films were deposited on silicon (100) and quartz substrates by pulsed laser deposition (PLD) at an optimized oxygen partial pressure of 3.0×10^?3 mbar in the substrate temperatures range 300–973 K. The films were characterized by X-ray diffraction, transmission electron microscopy, atomic force microscopy, spectroscopic ellipsometry, UV–visible spectroscopy and nanoindentation. The X-ray diffraction studies showed that the films deposited at low substrate temperatures (300–673 K) were amorphous Al₂O₃, whereas those deposited at higher temperatures (≥773 K) were polycrystalline cubic γ-Al₂O₃. The transmission electron microscopy studies of the film prepared at 673 K, showed diffuse ring pattern indicating the amorphous nature of Al₂O₃. The surface morphology of the films was examined by atomic force microscopy showing dense and uniform nanostructures with increased surface roughness from 0.3 to 2.3 nm with increasing substrate temperature. The optical studies were carried out by ellipsometry in the energy range 1.5–5.5 eV and revealed that the refractive index increased from 1.69 to 1.75 (λ=632.8 nm) with increasing substrate temperature. The UV–visible spectroscopy analysis indicated higher transmittance (>80%) for all the films. Nanoindentation studies revealed the hardness values of 20.8 and 24.7 GPa for the films prepared at 300 K and 973 K respectively.     

Impact of characteristic length and loading rate upon dynamic constitutive behavior and fracture process in alumina ceramics

Understanding the impact performance of ceramic materials requires accurate corresponding relationship between mechanical response and fracture behavior. In this study, constitutive behaviors of alumina ceramics were successfully determined via split-Hopkinson pressure bar (SHPB) system coupled with high-speed camera to track the deformation and failure process. Failure strength of alumina demonstrated a strong dependency on strain rate beyond a critical value (namely transition strain rate). Inelastic deformation in the dynamic stress-strain curves implied that degradation of modulus does occur. The incorporating such degradation (damage evolution) in modulus enabled a more accurate evaluation of transition strain rate as a function of characteristic length of specimen. On-line observation revealed that longitudinal cracks dominated the failure process of alumina with negligible interfacial friction. However, interfacial friction became significant with the decreased characteristic length, thus the inclined cracks dominated fracture in alumina. It was found that the effect of interfacial friction can be minimized by lowering the impact velocity to maintain the uniaxial loading status in SHPB loads. Finally, it is suggested that an aspect ratio of 1.0 for the specimen should be suitable for alumina due to its insensitivity to interfacial friction within the achievable strain rate.     

A novel approach to fabricate porous alumina ceramics with excellent properties via pore-forming agent combined with sol impregnation technique

An innovative approach for fabricating porous alumina ceramics (PACs) with improved mechanical and thermal properties using walnut shell powders as pore-forming agent combined with alumina sol impregnation is reported in the present work. It is demonstrated that uniform distribution of spherical pores can be observed in as-prepared PACs by using above technical route. The decrease of walnut shell powder sizes significantly promotes the enhancement of crushing strength and reduction of thermal conductivity of the PACs. Meanwhile, the impregnated alumina sol is favoring for the formation of spherical micro-pores, then further improves their mechanical and thermal insulation performances. The lowest thermal conductivity and highest crushing strength of resulting sample reach 0.16?W/m?K and 29.2?MPa, respectively. This novel method offers new possibilities to fabricate high-quality PACs.     

Optimized etching of porcelain and polycrystalline alumina with a glass phase

Chemical and thermal etching techniques are commonly used in ceramography to enhance microstructural features. While thermal etching works well for high purity ceramic systems, this technique may not be appropriate where glass is present. Porcelain and industrial alumina both contain a glass phase, typically 40?60 vol% and 4?30 vol%, respectively, and these glass chemistries are proposed to be similar. Chemical etching of porcelain is common, but the images published in the literature are frequently over-etched. When glass is present in the grain boundaries of alumina, thermal etching can cause the glass to disappear or to recrystallize, obscuring the microstructure. Because of this, it is proposed that both chemical and thermal etching are necessary to prepare an industrial alumina microstructure for grain size measurements. In addition, it was observed that chemical etching is sensitive to the residual stress in the glass phase, becoming more aggressive when there is residual tension in the glass.     

Effect of starch addition on microstructure and properties of highly porous alumina ceramics

Porous alumina ceramics with ultra-high porosity were prepared through combining the gel-casting process with the pore-forming agent technique. Porosity and pore size distribution of the sintered bulks were evaluated with and without adding starch, respectively. In particular, the influences of starch addition on the properties, including thermal conductivity and compressive strength were studied. It was found that the incorporation of starch increased the nominal solid loading in the suspension and subsequently promoted the particle packing efficiency. The porosity is raised with increasing starch content from 0 to 30 vol%, which brings the decrease in thermal conductivity, whereas the compressive strength isn't seriously degraded. The further higher starch addition (40 vol%), however, would deteriorate the performance of the alumina porous ceramics. It is believed that the appropriate starch amount (lower than 30 vol%), working as a pore-forming agent, suppresses the driving force of densification without affecting the connections of neighboring grains while excessive starch amount would lead to the collapse of the porous structure.     

Influence of fibers on the microstructure and compressive response of directional ice-templated alumina ceramics

Directional ice-templated ceramics have unique lamellar porous channels between ceramic walls which run from bottom to top of the samples. This highly oriented morphology results in the anisotropy in mechanical properties both parallel and perpendicular to freezing direction. In this research, fiber-enhanced ice-templated porous ceramics were fabricated by introducing fibers into alumina slurry for freezing. The trans-lamellar fiber bridges connecting adjacent ceramic walls were formed by adjusting the aspect ratio of fibers and freezing velocity, which greatly enhanced the compressive response in two directions and weakened the anisotropy in mechanical properties of the directional ice-templated ceramics. The results showed that the of fiber bridges increased with the increase of fiber aspect ratio and the longitudinal and transverse mechanical properties increased by 73.5% and 232.6%, respectively.     

Effect of sintering temperature on microstructure and mechanical properties of zirconia-toughened alumina machinable dental ceramics

This study investigated the effect of sintering temperature on the microstructure and mechanical properties of dental zirconia-toughened alumina (ZTA) machinable ceramics. Six groups of gelcast ZTA ceramic samples sintered at temperatures between 1100 °C and 1450 °C were prepared. The microstructure was investigated by mercury intrusion porosimetry (MIP), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques. The mechanical properties were characterized by flexural strength, fracture toughness, Vickers hardness, and machinability. Overall, with increasing temperature, the relative density, flexural strength, fracture toughness, and Vickers hardness values increased and more tetragonal ZrO₂ transformed into monoclinic ZrO₂; on the other hand, the porosity and pore size decreased. Significantly lower brittleness indexes were observed in groups sintered below 1300 °C, and the lowest values were observed at 1200 °C. The highest flexural strength and fracture toughness of ceramics reached 348.27 MPa and 5.23 MPa m^1/2 when sintered at 1450 °C, respectively. By considering the various properties of gelcast ZTA that varied with the sintering temperature, the optimal temperature for excellent machinability was determined to be approximately 1200–1250 °C, and in this range, a low brittleness index and moderate strength of 0.74–1.19 µm^−1/2 and 46.89–120.15 MPa, respectively, were realized.     

A urea crystal templating method for the preparation of porous alumina ceramics with the aligned pores

A novel process for the preparation of porous alumina ceramics with an aligned pore structure has been reported. The urea dissolved in the aqueous alumina slurry at higher temperature formed rod shaped crystals aligned in the direction of gravity when cooled to room temperature. The gelatin used to set the slurry, controls the crystallization of urea such that the urea crystals produced in the suspension containing the gelatin had much lower width and thickness compared to that produced in the suspension without the gelatin. The alumina powder catalyzed the thermal decomposition of urea that enabled the removal of the majority of the urea crystals from the alumina green body by isothermal heating at temperature much lower than the melting point of urea. The void space created by the removal of the urea crystals remained as pores in the sintered ceramics.     

Effects of B4C addition on the microstructure and properties of porous alumina ceramics fabricated by direct selective laser sintering

Direct selective laser sintering (dSLS) is a promising method for the fabrication of complex-shaped ceramic parts. In this paper, boron carbide (B₄C) was used as an inorganic additive to improve the laser sintering behavior of alumina. The effects of B₄C addition on the microstructure and mechanical properties of porous alumina ceramics were investigated. Mixture of alumina powders and different amount of B₄C were directly sintered using different SLS parameters. Results indicated that the process window of alumina could be expanded by the addition of B₄C. Furthermore, the amount of B₄C played an important role in surface morphologies of alumina ceramics. It could be explained by the increase of mass transfer due to the addition of B₄C, which enhanced the densification process. The compressive strength of sintered samples increased with the increase of B₄C, which reached its maximum value when the content of B₄C was 7?wt% and the density of the samples after post treatment could reach 1.4?g/cm³. In addition, a size expansion phenomenon was observed. The size expansion could reach 5% after SLS, which could be attributed to the pin effects and oxidation behavior of B₄C particles.