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.     

Sandwich materials formed by thick alumina tapes and thin-layered alumina–aluminium titanate structures shaped by EPD

The objective of this work was to analyse the potential of the alumina (Al₂O₃)–titania (TiO₂) system to fabricate laminates with very thin deflecting layers. Alumina–aluminium titanate structures formed by thick self-supported alumina tapes (400 μm) joined together by layered alumina–aluminium titanate structures shaped by EPD have been developed and their mechanical response has been evaluated as a function of the thickness of the layered structures. For this purpose the stability of alumina and alumina–titania suspensions in ethanol was optimized and the EPD parameters to control the growth of layers on non-conductive substrates were analysed. Two different sandwich structures formed by external alumina tapes joined by multilayer systems built by EPD were fabricated. Differences between the multilayer systems were based on the thickness of the layers. Large portions of the central parts of the laminates with thicker layers remained un-fractured while multiple delaminations were observed in the central parts of the specimens with thinner layers that presented wood-like fracture. The fracture modes were reflected in the load-displacement curves as higher loads were needed to fracture the more resistant thicker ligaments whereas larger displacements were admitted by the specimens with thinner layers due to multiple delaminations.     

Improved wear behaviour of alumina-aluminium titanate laminates with low residual stresses and large grained interfaces

The wear behaviour of a monolithic alumina and an alumina-aluminium titanate laminated structure was studied. The laminate, containing surface fine grained alumina layers and internal composite layers with 10 vol.% of aluminium titanate, showed relatively low (≅20 MPa) compressive residual stresses at the surface. Interfaces between layers were constituted by large alumina grains (up to ≅50 μm) that promoted toughening due to crack deflection and branching. Wear tests were performed on square specimens (30 mm × 30 mm × 6 mm) using the pin-on-disc method. The laminates showed higher wear resistance than the monolithic alumina. The analysis of the results together with SEM-EDX observations was performed to identify possible wear mechanisms. The wear resistance improvements are discussed in terms of the residual stresses in the laminate and the properties provided by the special microstructure of the interfaces.     

Edge Stresses in Alumina/Zirconia Laminates

Using the technique of fluorescence piezospectroscopy, we determine the distribution of thermal residual stresses across the edges of three laminated alumina/zirconia composites. We develop a methodology for separating the measured stress state into microstresses that result from grain-to-grain thermal mismatch and macrostresses that result from lamination-induced thermal mismatch between individual plies. Comparison between the measured edge-stress distributions and those calculated based on a simple force-superposition model shows good agreement, indicating that the laminate system is well approximated as linear elastic. Given the experimental confirmation of significant edge stresses in multi-ply laminates, the possibility of failure initiating at composite edges must be considered in the design of surface-compressed laminate structures with the aim of mediating the detrimental effect of surface flaws.     

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.     

Lamination and Sintering Shrinkage Behavior in Multilayered Ceramics

Variations in lamination conditions, such as pressure, temperature, and time, changed the laminated density of multilayered alumina but had no effect on the sintered density. The present results showed that sintering shrinkage values differ with lamination conditions and vary inversely with laminated density. When lamination was accomplished using a press die, the difference in shrinkage between the X-Y and the Z directions was <1%. The effect of the press die could be explained by introducing a new factor, the SDF (shear deformation factor), which represents the ratio of area change in the X-Y direction before and after lamination. The lamination of green sheets exhibited almost the same behavior as did the compression of granules. A linear relationship also was found between laminated density and the logarithm of lamination pressure. Results for sintering shrinkage in the overall range of measured laminated densities showed that sintering shrinkage behavior could be divided into three regions; that is, the laminates had three packing structures with different laminated densities. A new factor ( k ), related to packing structure values before and after sintering, was introduced to explain the sintering shrinkage behavior. Each k value was obtained from the relationship between laminated density and sintering shrinkage. Comparing k factors for the laminated densities ( X-Y and Z ) under various lamination conditions made it possible to systematically analyze variations in the sintering shrinkage behavior of laminates with processing conditions. An estimation of sintering shrinkage was possible from that analysis.     

Influence of Residual Stresses on the Wear Behavior of Alumina/Alumina–Zirconia Laminated Composites

Symmetric structures of laminated ceramic composites were produced by superimposing alternating layers of Al₂O₃ and Al₂O₃/ZrO₂ composite prepared by tape casting. The composites were designed to have an alumina surface layer on either side. This configuration caused residual compressive stresses to be induced on the surface due to the different thermal expansion coefficients of the various layers, leading to an increase in the apparent surface toughness. The amount of residual stress was determined using the indentation technique. The tribological behavior of these laminated structures was evaluated using the pin-on-disk method for different loads and sliding speeds. Comparison with the results obtained from stress-free alumina showed that, within the range of these experimental conditions, the improvement in surface toughness leads to a reduced friction coefficient and increased wear resistance of the composites. Possible wear mechanisms are proposed.     

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.     

变刚度复合材料层合板的纤维铺放路径设计及屈曲分析

与传统纤维直线铺放的复合材料层合板相比,变刚度层合板可以更好地实现材料的可设计性,并通过铺放路径的优化设计提高层合板的屈曲载荷。首先,对铺放角随坐标轴线性变化的铺放路径进行扩展,提出多种铺放角非线性变化的曲线线型,并以此作为基准轨迹重新设计了四种纤维变角度铺放方式。其次,利用ANSYS软件对上述五种不同铺放路径的变刚度层合板进行建模运算,在单轴和双轴载荷下,对其进行屈曲载荷计算分析并与定角度铺放的层合板对比。计算结果表明,铺放路径优化下的变刚度层合板与纤维直线铺放的层合板相比,其屈曲载荷得以显著提高。     

Residual stresses in alumina–zirconia laminates

Significant residual stresses can arise in hybrid ceramic laminates during the densification and cooling processing cycles. The densification stresses in alumina–zirconia laminates were calculated assuming the layers to be linear viscous with data obtained by cyclic loading dilatometry. These stresses placed the zirconia layers in biaxial tension and even at 1 MPa or less, they were sufficient to cause a type of linear cavitation damage. The methodology was also applied to asymmetric laminates, successfully predicting their observed curling behaviour. Thermal expansion mismatch stresses arise during cooling, again placing the zirconia layers in residual biaxial tension and leading to the formation of transverse (channelling) cracks. The stresses were calculated using both elastic and viscoelastic formulations and were confirmed with indentation measurements. Additions of alumina to the zirconia layers were effective in reducing both sources of residual stress and allowed crack formation during processing to be avoided. Residual stresses were also shown to improve mechanical performance.     

Toughening of Layered Ceramic Composites with Residual Surface Compression

Effects of macroscopic residual stresses on fracture toughness of multilayered ceramic laminates were studied analytically and experimentally. Stress intensities for edge cracks in three-layer, single-edge-notch-bend (SENB) specimens with stepwise varying residual stresses in the absence of the crack and superimposed bending were calculated as a function of the crack length by the method of weight function. The selected weight function and the method of calculation were validated by calculating stress intensities for edge cracks in SENB specimens without the residual stresses and obtaining agreement with the stress-intensity equation recommended in ASTM Standard E-399. The stress-intensity calculations for the three-layer laminates with the macroscopic residual stresses were used to define an apparent fracture toughness. The theoretical predictions of the apparent fracture toughness were verified by experiments on three-layer SENB specimens of polycrystalline alumina with 15 vol% of unstabilized zirconia dispersed in the outer layers and 15 vol% of fully stabilized zirconia dispersed in the inner layer. A residual compression of ∼400 MPa developed in the outer layers by the constrained transformation of the unstabilized zirconia from the tetragonal to the monoclinic phase enhanced the apparent fracture toughness to values of 30 MPa^.m^1/2 in a system where the intrinsic fracture toughness was only 5 to 7 MPa^.m^1/2.     

Multifunctional performance of Ti2AlC MAX phase/2D braided alumina fiber laminates

The processing and characterization of laminates based on Ti₂AlC MAX phase, as matrix, and triaxial alumina braids, as reinforcing phase, are presented. Ti₂AlC powders with a mean particle size below 1 µm are synthesized, while commercial 3M Nextel 610 alumina fibers are braided in a three-stage process consisting of spooling, braiding with an angle of 0° and ±60° and the separation to single-layer fabric. The laminates are processed by layer-by-layer stacking, where 3 two-dimensional alumina braids are interleaved between Ti₂AlC layers, followed by full densification using a Field-Assisted Sintering Technology/Spark Plasma Sintering. The multifunctional response of the laminates, as well as for the monolithic Ti₂AlC, is evaluated, in particular, the thermal and electrical conductivity, the oxidation resistance, and the mechanical response. The laminates exhibit an anisotropic thermal and electrical behavior, and an excellent oxidation resistance at 1200℃ in air for a week. A relatively lower characteristic biaxial strength and Weibull modulus (i.e., σ₀ = 590 MPa and m = 9) for the laminate compared to the high values measured in the monolithic Ti₂AlC (i.e., σ₀ = 790 MPa and m = 29) indicates the need but also the potential of optimizing MAX-phase layered structures for multifunctional performance.     

Al2O3-3YTZP-Graphene multilayers produced by tape casting and spark plasma sintering

This work aims to establish a colloidal route to obtain laminates of alumina–zirconia combining layers with and without graphene. Green tapes of alumina, alumina with 5 vol.% of 3Y-TZP and alumina with 5 vol.% of 3Y-TZP and graphene-oxide (2 vol.%) were obtained by aqueous tape casting. It is possible to design materials for different structural applications with a controlled microstructure with a high number of different layers. The tapes were punched into 20-mm discs, joined to form laminates alternating up to 18-layers, and sintered in one-step by spark plasma sintering (SPS) at 1400 °C. It has demonstrated that there is a significant graphite diffusion provoked by the required graphite holders into the SPS-furnace. Dense laminates with layer thicknesses ∼100 μm and good cohesion between layers were obtained. Nanoindentation results showed that hardness and elastic modulus values were higher than 27 GPa and 300 GPa, respectively, and similar for all layers.     

Surface Properties of Ceramic Laminates Fabricated by Die Pressing

The simple die-pressing technique has been used to fabricate thick-layer zirconia/alumina ceramic laminates in the forms of film/substrate and multilayer systems. A "vibration sieve" method is used to achieve uniform layer thickness. In order to suppress surface crack initiation and propagation, the laminates are designed to retain residual compressive stresses in the surface layers. As a result, the surface fracture/fatigue resistance has been significantly improved, and the microhardness of the surface layer has also been increased to a certain degree.     

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.     

High-Strength Alumina/Alumina:Calcium-Hexaluminate Layer Composites

The strength degradation of alumina/alumina:calcium-hexaluminate/alumina trilayers, after damage from Hertzian contacts, is evaluated. Relative to the monolithic alumina and alumina:calcium-hexaluminate constituent layer materials, the trilayers show markedly improved strength retention in the damaged state at high contact loads. The outer, fine-grained alumina layers are classically brittle, characterized by cone cracking, whereas the inner alumina:calcium hexaluminate layer is essentially quasi-plastic, with a well-defined "yield" zone that consists of distributed microdamage. The improved strength behavior of the trilayer composite is rationalized in terms of a synergistic interaction between the contact-induced deformation modes in the two layers, with each mode partially ne-gating the effectiveness of the other as a source of failure. This result offers the prospect of hybrid structures with hard outer layers, to provide wear resistance, and soft, tough underlayers, to inhibit brittle fracture.     

Microstructure and mechanical behavior of TiO2-MnO-doped alumina/alumina laminates

Tapes of TiO₂-MnO-doped alumina (d-Al₂O₃) and pure alumina (Al₂O₃) were shaped via tape casting. Laminates with three different layer numbers and respective thicknesses were produced and sintered at 1200°C. The microstructure and mechanical behavior of laminates were investigated and compared to the respective monolithic references (d-Al₂O₃ and Al₂O₃). The use of dopants in alumina decreased the initial sintering temperature, leading to higher densification at 1200°C (~98% theoretical density (TD)) when compared to Al₂O₃ (~73% TD). The higher density was reflected in a higher Young's modulus and hardness for doped alumina. A region of diffusion of dopants in pure alumina layers was observed along the interface with doped layers. The mechanical strength of d-Al₂O₃ samples sintered at 1200°C was not statistically different from Al₂O₃ samples sintered at 1350°C. The strength of laminates composed of doped layers with undoped, porous interlayers did not change. Nevertheless, as the thickness of these porous interlayers increases, a loss of strength was observed. Monolithic references showed constant values of fracture toughness (K_IC), ~2 MPa·m^1/2, and linear crack path. On the other hand, K_IC of laminates increases when the crack propagates from weak Al₂O₃ layers to dense d-Al₂O₃ layers.     

Ceramic laminates with improved mechanical reliability by tailoring the porosity of the constituting layers

Two different ceramic laminates composed of porous alumina and alumina/zirconia layers were designed and produced in the present work. The two symmetrical architectures were selected whose fundamental difference is the presence on the surface of a porous layer in the first and a compact alumina/zirconia composite layer in the second. The residual stress profile and corresponding fracture toughness were tailored to promote the stable growth of surface defects prior to final failure to increase the mechanical reliability of the material. The laminates were realized by stacking together different green laminae (containing specific pore former content) in a specific order, thermo-compression and co-sintering. The results point out an important reduction of the strength scatter and a clear insensitivity to surface damage. It is also shown that the mechanical performances are strictly related to the specific architecture of the laminate, this allowing to tailor a priori the mechanical performances of the composite.     

Alumina/NiCu Laminate under Thermal Shock up to 1000°C: I, Experimental

The mechanical behavior of an alumina/NiCu laminate under thermal shock loading was investigated. The maximum thermal shock temperature was 1000°C. The laminate architecture was the cause of a basic change in the cracking mechanisms, manifested in a dramatic increase in the mechanical residual strength over that of monolithic alumina. The laminated system was constructed by alternating alumina layers coated with copper films with nickel interlayers and joining them by a combination of liquid-state (brazing) and solid-state (diffusion) bonding. The material system was tested by water quenching square-shaped laminated specimens initially at temperatures of up to 1000°C. Three-point bending tests revealed the mechanical strength before and after thermal shock, and SEM analysis described the damage mechanisms and the extent of debonding at the alumina/NiCu interfaces.     

Improving energy dissipation and damage resistance of CFRP laminates using alumina nanoparticles

ABSTRACT

In this paper, the effect of a toughened epoxy matrix on the damage evolution, energy dissipation, and permanent indentation of composite laminates under out-of-plane (transverse) loading is presented experimentally. The epoxy matrix was toughened by 3% alumina nanoparticles with sizes less than 200?nm. A quasi-static indentation test was exploited to characterise the damage modes and evaluate the dissipation of energy of the composite laminate. The dissipated energy was evaluated as the enclosed area between the loading and unloading curves, while the damage resistance was expressed as the number of delaminations and their size. The results showed that epoxy toughened by alumina nanoparticles, showed an improvement in the damage threshold load by 27.3% and higher ultimate load under indentation. Regarding the damage resistance, the toughened laminates showed lower number of delaminated interfaces and lower projected delamination area than untoughened laminates. This is due to the localised damage under the indenter, the matrix cracks at low indentation energy and fibre breakages occur at high indentation energy.