Design of damage tolerant and crack-free layered ceramics with textured microstructure

This work demonstrates damage tolerant behavior of ceramic laminates designed with residual stresses and free of surface edge cracks. Non-periodic architectures were designed by embedding 2 textured alumina (TA) layers between 3 equiaxed alumina-zirconia (AZ) layers. Compressive residual stresses of ∼ 250 MPa were induced in the textured layers. Indentation strength tests showed that textured compressive layers arrested the propagation of cracks. Results were compared to periodic architectures with the same volume ratio of TA and AZ materials. Crack propagation was arrested in both periodic and non-periodic designs; the minimum threshold-strength being higher in the latter. Non-periodic architectures with compressive layers as thin as ∼ 200 μm showed no evidence of surface edge cracks, yet still reached minimum threshold strength values of ∼ 300 MPa. In addition, the textured microstructure promoted crack bifurcation in the thin compressive layers and thus enhanced the damage tolerance of the material.     

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).     

Residual stresses in alumina matrix composites reinforced with Ti(C,N)

Ti(C_0.5,N_0.5)-reinforced alumina matrix composites with an addition of 2 wt% ZrO₂ were tested to determine residual stresses of Al₂O₃ and Ti(C_0.5,N_0.5) phases. The advanced sintering technique (spark plasma sintering ―SPS) at various temperatures of 1600°C and 1700°C was used. Vickers hardness HV1, Young’s modulus E, apparent density ρ and indentation fracture toughness K_IC(HV) were evaluated. An indirectly residual stress measurement by the XRD method using the sin² ψ technique was applied. Compressive residual stresses in both phases: α-Al₂O₃ and Ti(C_0.5,N_0.5) were observed. Residual stresses of α-Al₂O₃₍₂₂₆₎ are in the range between ?204 ± 20 MPa and ?120 ± 20 MPa (for 1600 °C and 1700 °C respectively) are lower compared to Ti(C_0.5,N_0.5)_(420), for which the stresses are in the range of between ?292 ± 20 MPa and ?256 ± 20 MPa (for 1600 °C and 1700 °C respectively). The results exhibit the influence of the sintering temperature on the residual stresses of the tested phases. The residual stresses revealed at 1700°C are lower by about 40% for α-Al₂O₃₍₂₂₆₎ and much less for Ti(C_0.5,N_0.5)₍₄₂₀₎, by only about 15%. Microstructure studies using scanning electron microscopy, X-ray and electron diffraction phase analysis were used.     

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.     

Contact damage tolerance of alumina-based layered ceramics with tailored microstructures

This work demonstrates how to enhance contact damage resistance of alumina-based ceramics combining tailored microstructures in a multilayer architecture. The multilayer system designed with textured alumina layers under compressive residual stresses embedded between alumina–zirconia layers was investigated under Hertzian contact loading and compared to the corresponding monolithic reference materials. Critical forces for crack initiation under spherical contact were detected through an acoustic emission system. Damage was assessed by combining cross-section polishing and ion-slicing techniques. It was found that a textured microstructure can accommodate the damage below the surface by shear-driven, quasi-plastic deformation instead of the classical Hertzian cone cracking observed in equiaxed alumina. In the multilayer system, a combination of both mechanisms, namely Hertzian cone cracking on the top (equiaxed) surface layer and quasi-plastic deformation within the embedded textured layer, was identified. Further propagation of cone cracks at higher loads was hindered and/or deflected owed to the combined action of the textured microstructure and compressive residual stresses. These findings demonstrate the potential of embedding textured layers as a strategy to enhance the contact damage tolerance in alumina ceramics.     

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.     

Luminescent Eu3+-doped transparent alumina ceramics with high hardness

The Eu³⁺-doped transparent aluminas were prepared by wet shaping technique followed by pressure-less sintering and hot isostatic pressing. The effect of dopant amount on microstructure, real in-line transmission (RIT), photoluminescence (PL) properties, hardness and fracture behaviour was studied. The RIT decreased with increasing amount of the dopant. The PL emission spectra of Al₂O₃:Eu³⁺ ceramics exhibited predominant red light emission with the highest intensity (under 394 nm excitation) for material containing 0.125 at.% of Eu³⁺ and colour coordinates (0.645, 0.355) comparable with commercial red phosphors. The doping resulted in hardness increase from 26.1 GPa for undoped alumina to 27.6 GPa for Eu-doped sample. The study of fracture surfaces showed predominantly intergranular crack propagation micro-mechanism.     

Effect of residual stresses to the crack path in alumina/zirconia laminates

Laminates with alternating layers are well known from nature. The strongly bonded alumina/zirconia (Al₂O₃/ZrO₂) layers can combine high fracture resistance with high strength and stiffness when properly tailored. The presence of compressive residual stresses formed in Al₂O₃ layers can suppress and deflect cracks propagating through the layers. The crack path is governed by both the elastic properties and the internal stress field of individual layers. The laminates with various layer-thickness ratios ranging from 0.1 to 3 were used to investigate the effect of residual stresses and influence of crack formation pattern on the crack path development. The indentation surface cracks observed in various alumina-zirconia laminates exhibit the same crack deflection independently on the level of internal stresses. The crack deflection observed on the fracture surfaces of bending specimens was related to the indentations cracks. The complicated crack path was explained experimentally by 3D reconstruction with the support of numerical simulations.     

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°.     

Effect of initial particle size on grain microstructure of textured ferroelectric ceramics: A phase-field method and brush technique

A phase-field model was employed to simulate the grain microstructure evolution of the textured ceramics. Textured KSr₂Nb₅O₁₅ (KSN) ceramics were chosen as the research object and prepared by using acicular KSN particles as raw materials. A method combining the brush technique with the rolling process was proposed for the directional arrangement of the acicular particles. The effects of the initial particle length distribution and diameter on the grain growth behavior and electrical properties were investigated. It was found the influence of the initial particle length distribution on the grain growth rate mainly depended on its diameter. The use of coarse particles was beneficial to obtain a microstructure with a strongly anisotropic morphology and homogeneous grain size. The obtained KSN ceramics exhibited a high piezoelectric constant d₃₃ of 68 pC/N and Curie temperature of 120 ℃, which was closely related to the grain microstructure.     

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。     

Effects of debinding condition on microstructure and densification of alumina ceramics shaped with photopolymerization-based additive manufacturing technology

Alumina green bodies shaped with digital light processing (DLP) technology were debinded in four atmospheres, including air, argon (Ar), mixture of 95% argon and 5% hydrogen (95% Ar +5% H₂) and vacuum, at different heating rates (0.5 °C/min, 1 °C/min and 3 °C/min), followed by sintering in air at 1650 °C for 3 h. The effects of debinding atmosphere and heating rate on microstructure and densification of the brown bodies and sintered bodies were evaluated via morphology characterization, X-ray computed tomography (CT) reconstructions and other tests. Focusing on the quantitative analysis of the geometric characteristics and distribution of defects in the brown bodies and sintered bodies, it is found that the type (holes, cracks and delamination), content and volume distribution of defects during the debinding in aerobic and anaerobic environments are different. Our study indicates that low-rate vacuum debinding should be adopted as a promising debinding approach for ceramics shaped with photopolymerization-based additive manufacturing technology.     

Continuous alumina fiber-reinforced yttria-stabilized zirconia composites with high density and toughness

Continuous alumina fiber-reinforced yttria-stabilized zirconia (YSZ) composites with a LaPO₄ fiber coating were fabricated by slurry infiltration and spark plasma sintering (SPS). The LaPO₄ coating was deposited on the reinforcement alumina fabrics by a modified sol-gel method. The YSZ slurry with good dispersion and stability was prepared by optimizing the pH value, dispersant addition and ball milling time. The fabricated composite with a high density of ∼ 92 % has a good flexural strength of 277 ± 43 MPa, and a superior fracture toughness of 15.93 ± 0.75 MPa·m^1/2 exhibiting a non-brittle failure behavior. It was found that the LaPO₄ coating reduced the residual stress near the fiber/matrix interface to 131 ± 41 MPa, which was 369 ± 63 MPa in the composite without the fiber coating. The LaPO₄ coating renders a weak interphase to improve the composite toughness by activating several toughening mechanisms including crack deflection, fiber debonding and pullout, and delamination behavior.     

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.     

Dry sliding wear behaviour of ZrB2-based ceramics: Self-mated and cross coupling with alumina

Systematic dry sliding wear tests with monolithic ZrB₂ and Al₂O₃ pins coupled to ZrB₂, ZrB₂-20 vol% SiC and Al₂O₃ discs were carried out in a disc-on-pin configuration. The steady state friction of ZrB₂ self-mated or cross coupled with Al₂O₃ was about 1.1. Self-mated monolithic ZrB₂ discs worn about three orders of magnitude more than self-mated Al₂O₃ discs. ZrB₂ pin wear rate was almost double when coupled to ZrB₂ or ZrB₂-20 vol% SiC discs than when coupled to Al₂O₃ discs. The wear track of ZrB₂-based materials showed an oxygen increment due to humidity-driven tribo-reaction. In all the systems, the main wear mechanisms observed were microfracture and abrasion. Numerical calculations and fracture models were employed to describe the wear mechanisms. By nanoindentation tests on worn and unworn areas, a significant lower hardness of the debris layer formed when ZrB₂ materials were involved.     

Grain orientation evolution and multi-scale interfaces enhanced thermoelectric properties of textured Sr0.9La0.1TiO3 based ceramics

Sr_0.9La_0.1TiO₃ based textured ceramics (SLTT-S3T) with a texture fraction of 0.81 are successfully fabricated by the reactive template grain growth method, in which Sr_0.9La_0.1TiO₃/20 wt%Ti was used as matrix and 10 wt% plate-like Sr₃Ti₂O₇ template seeds were used as templates. The phase transition, microstructure evolution, and the anisotropic thermoelectric properties of SLTT-S3T ceramics were investigated. The results show that the ceramics are mainly composed of Sr_0.9La_0.1TiO₃ and rutile TiO₂ phases. Grains grow with a preferred orientation along (h00). A maximum ZT of 0.26 at 1073 K was achieved in the direction perpendicular to the tape casting direction. The low lattice thermal conductivity of 1.9 W/(m K) at 1073 K was obtained decreased by 34%, 40%, and 38% compared with non-textured, SrTiO₃ and Sr_0.9La_0.1TiO₃ ceramics prepared by the same process, can be attributed to the enhanced phonon scattering by the complex multi-scale boundaries and interfaces. This work provides a strategy of microstructural design for thermoelectric oxides to decrease intrinsic lattice thermal conductivity and further regulate thermoelectric properties via texture engineering.