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.     

Evolution of microstructure and residual stresses in gradually ground/polished 3Y-TZP

A comprehensive study of progressively ground/polished 3Y-TZP was performed with the aim of better understanding the mechanisms driving the microstructural modifications observed after such procedures, and identifying the processing parameters leading to optimal microstructures (i.e. ageing-protective and damage-free). Gradually ground/polished surfaces were produced, yielding four different topographies of increasing roughness (grades 1–4) and two different textures (unidirectionally, U, and multidirectionally, M). Phase transformation, microstructure and residual stresses were investigated by means of advanced characterization techniques. It was found that low-roughness mildly ground/polished specimens (i.e. 2-M/U) presented a nanometric layer with the ageing-related protective features generally associated with coarsely ground specimens. A lower limit for grain refinement in terms of surface abrasion was also found, in which partial recrystallization took place (i.e. 1-M/U). A mathematical relation was established between average surface roughness (S_a), monoclinic volume fraction (V_m) and surface compressive residual stresses, demonstrating that if the processing parameters are controlled, both V_m and residual stresses can be predicted by the measurement of S_a.     

Functional gradient coating of alumina on net shaped zirconia implant: Improved strength,aging resistance,and role of residual stress

Aging of zirconia in vivo has been widely discussed as a potential cause of implant degradation over time. Hydrothermal degradation is sensitive to composition, process conditions, and microstructure leading to an emphasis on secondary phases, and grain boundary engineering for aging resistance. However, surface coatings, resultant residual stress, and associated physical constraint for phase stabilization are insufficiently explored. Herein a novel ceramic dough processing facilitated the formation of a functional gradient alumina coating (20–50 µm) below the critical thickness, on net-shaped green zirconia dental implant while preserving the fine machined threads. Residual stress (~ ?0.8 GPa) after sintering improved the characteristic strength by ~ 45% with a simultaneous contribution to profound phase preservation after in vitro aging. Thus, the compositional gradient coating on green zirconia components using alumina-based slurries is a facile surface modification technique to inhibit moisture-induced aging.     

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.     

Thermal residual stresses in bilayered,trilayered and graded dental ceramics

Layered ceramic systems are usually hit by residual thermal stresses created during cooling from high processing temperature. The purpose of this study was to determine the thermal residual stresses at different ceramic multi-layered systems and evaluate their influence on the bending stress distribution. Finite elements method was used to evaluate the residual stresses in zirconia-porcelain and alumina-porcelain multi-layered discs and to simulate the ‘piston-on-ring’ test. Temperature-dependent material properties were used. Three different multi-layered designs were simulated: a conventional bilayered design; a trilayered design, with an intermediate composite layer with constant composition; and a graded design, with an intermediate layer with gradation of properties. Parameters such as the interlayer thickness and composition profiles were varied in the study. Alumina-porcelain discs present smaller residual stress than the zirconia-porcelain discs, regardless of the type of design. The homogeneous interlayer can yield a reduction of ~40% in thermal stress relative to bilayered systems. Thinner interlayers favoured the formation of lower thermal stresses. The graded discs showed the lowest thermal stresses for a gradation profile given by power law function with p=2. The bending stresses were significantly affected by the thermal stresses in the discs. The risk of failure for all-ceramic dental restorative systems can be significantly reduced by using trilayered systems (homogenous or graded interlayer) with the proper design.     

Quantitative analysis of the residual stress and dislocation density distributions around indentations in alumina and zirconia toughened alumina (ZTA) ceramics

Alumina, 10% and 20% ZTA with 1.5 mol% yttria stabiliser were subjected to Vickers indentation testing with loads from 1 to 20 kg. Cr³⁺ fluorescence and Raman spectroscopy were applied to the indent centre and around the indentation in order to investigate the origin of the signal, the effect of indentation loads and zirconia phase transformation on the residual stress and plastic deformation in the plastic zone. The results suggested that with very strong laser scattering, the depth resolution of ZTA materials was very poor, which lead to a very significant amount of the signal being collected from the subsurface regions below the plastic zone. It was also found that zirconia phase transformation reduced the compressive residual stress in the alumina matrix within the plastic zone, except at the indentation centre, due to the tensile residual microstress generated by the zirconia phase transformation. In addition, the dislocation density on the indent surface of the ZTA samples was significantly reduced due to the restriction of crack propagation and energy absorption during the phase transformation process. At the indent centre, the zirconia phase transformation was suppressed by the high compressive stress, therefore, no significant difference between alumina and ZTA in terms of their residual stress and dislocation density were observed. Using TEM observation, it was found that the plastic zone microstructure of pure alumina is different from that of ZTA, which is consistent with the Cr³⁺ fluorescence results.     

Effect of heat transfer on residual stresses in thermal spray coatings

Herein, heat transfer from the coating to the substrate during the thermal spraying process is simplified as one-dimensional heat conduction and a formula to express the temperature distribution in the substrate is provided. To achieve this, the spray process was divided into two stages, namely deposition (coating sprayed onto the substrate) and post-deposition (cooling of coating and substrate to atmospheric temperature). The coating was achieved through a layer-by-layer deposition method. Residual stresses in the system (including both the coating and substrate) following deposition of each layer were calculated, as well as those induced by post-deposition. Finally, the proposed formulae were implemented in a real-case example to illustrate the effect of heat transfer with regards to torch velocity on residual stresses. The simulative results were shown to have a better agreement with experimental results at low rather than at high torch velocities. The residual stresses in the coating surface decreased with the increase in heat transfer time. When the heat transfer time exceeded a certain value, a sharp decline in residual stresses was observed.     

Impact of sandblasting on the mechanical properties and aging resistance of alumina and zirconia based ceramics

Bioinert zirconia and alumina ceramic devices are widely used, both in orthopaedics and in dentistry. In order to improve their bonding with bone tissues or dental resin cements, their surfaces are often roughened at different scales. In this work, we have investigated the effects of the same sandblasting treatment on alumina, zirconia and a zirconia-toughened alumina, focusing on their mechanical performance and the interplay between surface defects and residual stresses. Additionally, we explored the impact of the treatment on the hydrothermal aging of the two zirconia-containing materials. Residual stresses generated during sandblasting were always predominant over surface defects but their effect varied with the material: while they had a weakening effect on alumina, they reinforced both zirconia-containing materials. Finally, we found that the monoclinic grains at the surface of sandblasted zirconia recrystallized into tetragonal nanograins after annealing and this led to an increased resistance to aging.     

High-temperature fracture behaviour of layered alumina ceramics with textured microstructure

Mimicking the damage tolerance of biological materials such as nacre has been realised in textured layered alumina ceramics, showing improved reliability as well as fracture resistance at room temperature. In this work, the fracture behaviour of alumina ceramics with textured microstructure and laminates with embedded textured layers are investigated under uniaxial bending tests at elevated temperatures (up to 1200 °C). At temperatures higher than 800 °C monolithic textured alumina favours crack deflection along the basal grain boundaries, corresponding to the transition from brittle to more ductile behaviour. In the case of laminates, the loss of compressive residual stresses is counterbalanced by the textured microstructure, effective up to 1200 °C. This study demonstrates the potential of tailoring microstructure and architecture in ceramics to enhance damage tolerance within a wide range of temperatures.     

Synthesis and characterization of zirconia toughened alumina ceramics prepared by co-precipitation method

Undoped and 3 mol% yttrium doped ZrO₂–Al₂O₃ composite powders with partially stabilized ZrO₂ (PSZ) content varying from 0 to 30 wt% were prepared by a co-precipitation route using inorganic precursors Al(NO₃)₃, ZrOCl₂ and Y(NO₃)₃. The precipitates were characterized by DTA and subsequently calcined at 1200 °C for 4 h to achieve fine grained composite powders. The calcined powders were characterized by FTIR and XRD. In order to enhance the sinterability, the calcined powders were wet milled in a high energy ball mill. Powders were uniaxially pressed to form pellets and sintered at 1600 °C for 5 h to achieve greater than 96% relative density. Microstructural analysis of the sintered compacts revealed the uniform distribution of the zirconia particles among the alumina matrix. It was also observed that the faceted intergranular zirconia grains were present at the grain boundaries and junctions in the alumina matrix. Vickers indentation was carried out at 1 kgf load for hardness and 2 kgf load for estimating the critical stress concentration factor (K_c). Microscopic studies of the indented samples showed that cracks were propagating around the grain boundaries. Highest K_c ∼8.40 ± 0.4 MPa√m and hardness ∼16.31 ± 0.58 GPa was obtained for the 30 wt% PSZ-Al₂O₃ composite. The sintered density and critical stress intensity factor (K_c) achieved were compararble to that achieved earlier by hot press and SPS.     

Modeling complex crack paths in ceramic laminates: A novel variational framework combining the phase field method of fracture and the cohesive zone model

The competition between crack penetration in the layers and cohesive delamination along interfaces is herein investigated in reference to laminate ceramics, with special attention to the occurrence of crack deflection and crack branching. These phenomena are simulated according to a recent variational approach coupling the phase field model for brittle fracture in the laminae and the cohesive zone model for quasi-brittle interfaces. It is shown that the proposed variational approach is particularly suitable for the prediction of complex crack paths involving crack branching, crack deflection and cohesive delamination. The effect of different interface properties on the predicted crack path tortuosity is investigated and the ability of the method to simulate fracture in layered ceramics is proven in relation to experimental data taken from the literature.     

Distribution of the thermal residual stresses in the WC-Co microstructure by finite element method

A Finite Element Model is used to observe the build-up of residual thermal stresses during the sintering process in two WC-Co samples with different volume fractions of Co. A realistic model of the two phase material is obtained by FIB slicing a real WC-Co sample and reconstituting the morphology. In the finite element model, the WC phase is defined as elastic and the Co phase includes plasticity. Different sets of parameters are considered to model the two phases. The results are compared with experimental data obtained by neutron diffraction. A good agreement is obtained between the experimental data and the simulations. The spatial distribution of the stress in the WC phase is also observed. This observation reveals anisotropy in the microscopic behavior, with the presence of preferential directions for the build-up of stress.     

Selective laser induced autocatalytic metallization of NiO and Cr2O3 doped alumina zirconia ceramic substrates

In this study slip cast alumina-zirconia materials were doped with nickel oxide and chromium oxide and sintered in air. Chromium oxide forms a solid solution while nickel oxide forms spinel with alumina. The sintered substrates were selectively irradiated with a green, ps pulsed Nd:YVO₄ laser. During subsequent autocatalytic plating, copper was deposited selectively on laser-irradiated surfaces. It is assumed that under the irradiation influence at very high temperatures metal or lower valence oxides are produced which initiate the growth of copper crystallites during the plating process. The process offers the opportunity to manufacture 3D integrated circuit carriers with ceramic substrates, which offer superior strength, thermal stability and heat conductivity compared to polymers. Single dopant or co-dopant contents of < 2 wt% are sufficient to induce a reliable laser activation at a broad range of laser parameters which enables the application of very narrow continuous conductor paths.     

Kinetics of the oxidative color removal and degradation of bromophenol blue with hydrogen peroxide catalyzed by copper(II)-supported alumina and zirconia

Copper-supported alumina and zirconia catalysts were prepared and their catalytic activity towards the oxidative color removal and degradation of bromophenol blue with H₂O₂ was investigated. The rate of reaction with alumina is greater than that with zirconia, which ascribed to the increased amount of copper loaded on the catalyst as well as to the increased surface area. A brown intermediate (peroxo-compound), formed at the early stages of the reaction, inhibited the reaction rate. The rate of reaction increased with increase in pH of the medium as well as with added chloride ions. Both catalysts are very stable and can be used for several times without notable loss in their catalytic activities.     

Electroconductive composite of zirconia and hybrid graphene/alumina nanofibers

Novel type of hybrid nanofillers representing graphene encapsulated alumina nanofibres was selected as an additive to develop toughened electroconductive partially stabilized zirconia. The sinterability, mechanical and electrical properties of the produced nanocomposites were studied as function of the filler/graphene content. Composites containing just 0.6 vol.% of graphene corresponding to 3 vol.% of hybrid nanofibres exhibited high electroconductivity of 58 S/m without deterioration of mechanical properties. They also showed a slight toughening effect that is reflected by an increase in the indentation fracture toughness by 20% as compared to monolithic zirconia.     

Processing and properties of tape-cast alumina/zirconia laminates composites

In the present work, laminar ceramic structures formed by layers of alumina and partially stabilized zirconia were fabricated by water-based tape casting. Rheological, physical and mechanical properties of slurries and laminates were evaluated. The laminates consisted of stacked alumina and zirconia green tapes produced by thermopressing. Pyrolysis was carried out at 450 °C and sintering at 1500 °C. The alumina/zirconia laminates were studied for a better understanding of the formation behavior and crack propagation at the laminate interface. The flexural strength values of laminates depend on the stress state on their surface. The laminates with the highest amount of zirconia layers presented low strength values (6.7 MPa), while the laminates with more alumina layers had a higher strength level (57.7 MPa). This is because these laminates have alumina layers on the surface which are in a state of residual compressive stress.     

Tape casting of alumina/zirconia suspensions containing graphene oxide

The introduction of carbon derivatives (nanotubes, graphene, etc.) as a second phase in ceramic matrices has limitations arising from their difficult processing. This paper studies the colloidal stability and the rheological behaviour of concentrated suspensions of alumina with 5 vol.% Y-TZP (AZ) and the effect of the addition of 2 vol.% of graphene oxide (AZGO) on the suspension stability, rheological behaviour and tape casting performance. The colloidal stability was studied using zeta potential measurements in terms of concentration of deflocculants and pH and homogenisation was optimised adjusting the sonication mode and time. The best results were obtained for pulsed mode. The optimum rheological properties were obtained for solid loadings of 53 vol.% and 40 vol.% for AZ and AZGO. Homogeneous, flexible tapes with thickness of ∼120 μm were obtained reaching densities of >60% of theoretical density in which secondary phases are well dispersed.     

Thermomechanical simulations of the transient coupled effect of thermal cycling and oxidation on residual stresses in thermal barrier coatings

Failures in thermal barrier coatings (TBCs) are associated with the build-up of residual stresses that result from thermal cycling, growth strain, and stress relaxation associated with high temperatures. To address these highly coupled processes, three aspects were examined. The first was concerned with the effect of thermal cycling and thermal gradients on the resulting residual stress fields. The second with the dynamic growth of thermally grown oxide (TGO) layer using novel finite volume-finite element algorithms. In the third, we examined the effect of stress relaxation on the (TC/TGO) interface. We modelled these highly coupled processes using transient thermomechanical finite element simulations. The temperature profile and state of oxidation variation with time were imported as a predefined field and solved in ANSYS nonlinear platform. Our results revealed that stress relaxation of the TGO stresses at high temperatures leads to a reduction in the TC/TGO interfacial stresses. They also revealed that the use of the isotropic hardening rule limits the increase in plastic deformation of the bond coat (BC), while the use of kinematic hardening rule leads to ratcheting. Furthermore, we highlighted the importance of considering uneven growth of TGO on the resulting stress field.     

Effect of substrate curvature on residual stresses and failure modes of an air plasma sprayed thermal barrier coating system

A set of aerofoil shaped air plasma sprayed thermal barrier coated (APS-TBC) specimens were adopted in this paper to investigate the stress distributions in the ceramic top coat (TC) and the thermally grown oxide (TGO), the mechanism of local crack generation and propagation at the TC/BC (bond coat) interface. The failure mode of the TBC system, the distribution of asperities at TC/BC interface, thickness of the TC and BC, and the TC microstructure were found to be influenced by substrate curvature. Residual stress was therefore measured across the thickness of the TC, along the undulating TGO and mapped at locations of asperities where failure tended to occur to interpret the initiation of local failure. The role of the TGO was investigated via its chemical bonding with the TC and the decohesion occurring at the TGO/BC interface. The crack propagation at the interface has been discussed with respect to the macro-failure of the TBC system.