Influence of nano-ZrO2 additive on the bending strength and fracture toughness of fluoro-silicic mica glass–ceramics

Fluoro-silicic mica glass–ceramics were prepared by a sintering process and different proportions of nano-ZrO₂ particles (3Y-TZP) were integrated during the process. Bending strength and fracture toughness were evaluated using a three-point bending test and a Vickers indenter, respectively. The bending strength and fracture toughness improved in significantly with the increase in the quantity of nano-ZrO₂ additives. The highest bending strength of 324.3 ± 12.3 MPa and fracture toughness of 4.2 ± 0.11 MPa m^1/2 were obtained with 30% (wt.) nano-ZrO₂. Good results were also obtained in morphological observations. The glass–ceramic is homogenous and the ZrO₂ grains embed in the lamellar structures of the fluoro-silicic mica homogenously and completely and array well and compactly. On the fracture surface, both the transgranular fracture and the intergranular fracture can be observed clearly.     

Fabrication,characterization and mechanical properties of SiC-whisker-reinforced Y-TZP composites

The microstructure and mechanical properties of hot-pressed yttria-stablized tetragonal zirconia polycrystals (Y-TZP) reinforced with up to 30 vol % SiC whiskers were investigated. The homogeneously dispersed and fully dense SiC whisker/Y-TZP composites were fabricated by wet-mixing the constitutents and uniaxially hot-pressing the resulting powder. The grain size of the matrix depended on the whisker volume fraction and the hot-pressing temperature. The significant increase of fracture toughness of about MPa m^1/2 at 10 Vol % SiC and a small increase in strength were achieved by uniformly dispersing the whiskers in the Y-TZP matrix. Fracture surfaces revealed evidence of toughening by the mechanisms of crack deflection, pullout, and crack bridging by the whiskers and also a phase transformation of ZrO₂. The observed increase in the fracture toughness of Y-TZP due to the addition of SiC whiskers was correlated with existing models of toughening mechanisms. Good agreement was achieved between the theoretical predictions and the experimental toughness values, obtained from the Y-TZP/SiC_w composites.     

Microstructure and mechanical behaviour of 3Y-TZP/Mo nanocomposites possessing a novel interpenetrated intragranular microstructure

Yttria stabilized tetragonal zirconia polycrystal (Y-TZP)/0-100 vol % molybdenum (Mo) composites were fabricated by hot-pressing a mixture of Y-TZP powder containing 3 mol % yttria (Y₂O₃) and a fine Mo powder in vacuum. This composite system possessed a novel microstructural feature composed of an interpenetrated intragranular nanostructure, in which either nanometer sized Mo particles or equivalent sized zirconia (ZrO₂) particles located within the ZrO₂ grains or Mo grains, respectively. The strength and toughness were both greatly enhanced with increasing Mo content for the 3Y-TZP/Mo composites thus breaking through the strength-toughness tradeoff relation in transformation toughened ZrO₂ and its composite materials. They exhibited a maximum strength of 2100 MPa and a toughness of 11.4 MPa·m^1/2 for the composite containing 70 vol % Mo. These simultaneous improvements in strength and toughness were determined to be the result of a decrease in flaw size associated with the interpenetrated intragranular nanostructure, and a stress shielding effect created in the crack tip by the elongated Mo polycrystals bridging the crack tip in addition to the stress induced phase transformation.     

Mechanical properties of Al2O3 particle-Y-TZP matrix composite and its toughening mechanism

Dense Al₂O₃ particle-Y-TZP matrix (Al₂O₃<40 vol%) composite was prepared by pressureless sintering at 1550°C. Composites with 10–30 vol% Al₂O₃ particles showed enhanced fracture toughness, bending strength and Vicker's hardness as compared to single-phase Y-TZP. The highest strength (1150 MPa) and highest toughness (12.4 MPa m^1/2) were obtained for the composite containing 10 vol% Al₂O₃. It was found that, in addition to the contribution by the crack-deflection effect, the enhanced phase transformation from tetragonal to monoclinic during fracture was the main toughening mechanism in operation in the composites.     

Microstructure and mechanical properties of 3Y-TZP/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites fabricated by liquid phase sintering

3Y-TZP/Al₂O₃ composites were pressureless sintered with the addition of TiO₂-MnO₂ and CaO-Al₂O₃-SiO₂ glass. The densification, microstructure and mechanical properties of the composites were investigated. It was found that the composites could be densified at a temperature as low as 1400^C by liquid phase sintering. The majority of the grain sizes for both Al₂O₃ and ZrO₂ were below 1 m because of the lower sintering temperature. A bending strength of 934 ± 28 MPa and fracture toughness of 7.82 ± 0.19 MPam^1/2 were obtained for 3Y-TZP/Al₂O₃ (20 vol%) composite. Transformation toughening is considered the responsible toughening mechanism.     

SiC-TiC and SiC-TiB2 composites densified by liquid-phase sintering

Particle-reinforced SiC composites with the addition of TiC or TiB₂ were fabricated at 1850 °C by hot-pressing. Densification was accomplished by utilizing a liquid phase formed with added Al₂O₃, Y₂O₃, and surface SiO₂ on SiC. Their mechanical and electrical properties were measured as a function of TiC or TiB₂ content. Adding TiC or TiB₂ to the SiC matrix increased the toughness, and decreased the strength and electrical resistivity. The fracture toughnesses of SiC-50 wt% TiC and SiC-50 wt% TiB₂ composites were approximately 60% and 50%, respectively, higher than that of monolithic SiC ceramics. Microstructural analysis showed that the toughening was due to crack deflection, with some possible contribution from microcracking in the vicinity of TiC or TiB₂ particles.     

Toughening mechanisms in duplex alumina-zirconia ceramics

A series of Al₂O₃-ZrO₂ ceramics has been fabricated using both conventional sintering and a hot-pressing route, which results in various microstructures including (i) Al₂O₃ with well-dispersed ZrO₂ single crystals; (ii) Al₂O₃ With TZP (tetragonal zirconia polycrystals) agglomerates (20 to 50m); and (iii) Al₂O₃-ZrO₂ duplex structures, in which both well-dispersed ZrO₂ single crystals and TZP agglomerates are dispersed. The fracture strength of the composites has been measured by means of three-point bending and the fracture toughness by means of the micro-indentation technique. The microstructural characterization was carried out using scanning and transmission electron microscopy, and phase analysis of the zirconia by means of X-ray diffraction. The high toughness values of 12 M Pa m^1/2 measured for the duplex structure have been correlated with the toughening mechanisms operative and the fracture strength with the matrix grain size and with larger defects present in the structure. A combined toughening process is proposed to account for the improved properties, including transformation toughening, microcrack toughening and crack deflection, which are discussed in context with the property measurements and the microstructural observations.     

Microstructure and mechanical properties of hot-pressed SiC-TiC composites

Hot-pressed SiC-TiC composite ceramics with 0–100 wt% TiC have been investigated to determine the effect of composition (amount of TiC) on the elastic modulus, hardness, flexural strength and fracture toughness,K _IC. The composites exhibited superior mechanical properties compared to monolithic SiC and TiC, especially in fracture toughness,K _IC, value for 30–50 wt% TiC composite. The maximum values ofK _IC and room-temperature flexural strength were 6 MPa m^1/2 for a 50 wt % TiC and 750 MPa for a 30 wt% TiC composite, respectively. The observed toughening could be attributed to the deflection of cracks due to dispersion of the different particles. Although no third phases were detected by both TEM and XRD studies, an EDAX study and resistivity measurements indicated some possibility of solid solutions being present. The composites containing more than 30 wt% TiC, exhibited resistivity lower than 10^–3 cm which is favourable for electro-discharge machining of ceramics.     

Preparation of zirconia-toughened bioactive glass-ceramics

Bioactive glass-ceramics toughened by tetragonal zirconia polycrystal (TZP) were prepared by hot-pressing mixed powders of the MgO-CaO-P₂O₅-SiO₂ glass and TZP containing 20 to 80% alumina. The bending strength and the fracture toughness of the composite materials were improved compared with those of the material without TZP. These composites showed high bending strengths (400 to 500MPa) and high fracture toughness ( 2.8MPa m^1/2). The existence of a crack deflection mechanism was observed by scanning electron microscopy. After soaking in simulated physiological solution at 100 °C, no phase transformation from tetragonal to monoclinic of TZP in the composites and no degradation in bending strength occurred.     

Mechanical properties of ultra-fine grained zirconia ceramics

The mechanical properties of tetragonal zirconia (TZP) materials doped with Y, Ce or Ti were studied as a function of temperature and grain size. Fine grained Y-TZP (grain size < 0.3 m) shows values for fracture toughness and strength at room temperature, which are comparable with the coarse grained transformation toughened materials, despite lacking transformation toughening. The morphology of the fracture surface points to crack deflection as the most important toughening mechanism. At 800 °C fracture toughness and strength are higher than in coarse grained Y-TZP materials. Doping Y-TZP with Ce or Ti results in a similar trend in mechanical properties, for fine grained material, as for the Y-TZP materials.     

云母微晶玻璃/Y-TZP复相材料的制备和力学性能

本文用烧结法制备了云母微晶玻璃／－TZP复相材料,用X光衍射分析（XRD）法测定了材料断裂过程中氧化锆的相变体积分数,用拉曼微探针谱测定了相变区宽度,并对增韧机制进行了研究．结果表明：氧化锆的加入可以显著提高材料的力学性能．当加入40vol％ZrO₂时,云母微晶玻璃的强度和断裂韧性分别可达446MPa和4．8MPam^1／2氧化锆的相变分数随氧化锆含量的增加而减小,而相变区宽度随氧化锆含量的增加而增大;氧化锆主要通过应力诱导相交增韧机制来提高云母微晶玻璃的断裂韧性,但随着氧化锆含量的增加,裂纹在氧化锆颗粒附近的偏转会进一步提高材料的断裂韧性．     

Microstructure and mechanical properties of SiC whisker reinforced ZrO2–6 mol.-%Y2O3 composites

Abstract

Microstructure, mechanical properties, fracture behaviour, and toughening mechanisms of hot pressed SiC whisker (SiC_w)

reinforced ZrO₂–6 mol.-%Y₂O₃ composites were investigated via transmission electron microscopy, scanning electron microscopy, X-ray diffraction, and mechanical testing. The experimental results show that there is a continuous increase in the Vickers hardness, elastic modulus, and fracture toughness of the composites with increasing SiC_w content, and an addition of 30 vol.-%SiC_w increases the fracture toughness from 3·42 MN m^?3/2 for the unreinforced matrix to 5·83 MN m^?3/2. The flexural strength is increased from 293 MN m^?2 for the unreinforced matrix to a maximum of 372 MN m^?2 by an addition of 10 vol.-%SiC_w, then it is significantly decreased by further increasing the SiC_w content. Observations via transmission electron microscopy show that no distinct second phase or intermediate layers form at the SiC_w/ZrO₂ interface. Diffusional separation of tetragonal phase from the cubic matrix occurred during cooling after hot pressing. Whisker bridging and crack deflection are the main toughening mechanisms, but whisker pull-out, crack branching, and refinement of the matrix particles also contribute to the improvement in the fracture toughness.

MST/1747     

3Y-TZP/LZAS微晶玻璃功能梯度涂层的微观结构与性能

为了提高钢基体微晶玻璃涂层的韧性, 在Q235钢基体上采用涂搪法制备了钇稳定四方相氧化锆/Li₂O- ZnO-Al₂O₃-SiO₂ (3Y-TZP/LZAS) 微晶玻璃功能梯度涂层。采用XRD、SEM分析了梯度涂层的物相组成和微观结构, 采用压痕法测试并计算了涂层的显微硬度和断裂韧性, 通过粘接-拉伸法测试了涂层的结合强度。结果表明, 3Y-TZP/LZAS微晶玻璃功能梯度涂层各层之间的界面结合紧密; 涂层与钢基体依靠玻璃中的SiO₂与铁的氧化物发生界面反应形成牢固的结合, 反应产物为Fe₂SiO₄和FeSiO₃; 涂层的显微硬度和断裂韧性沿涂层厚度方向逐渐增大, 涂层韧性提高是表面残余压应力增韧、3Y-TZP相变及3Y-TZP的颗粒增韧共同作用的结果; 梯度涂层与Q235的结合强度达16.3 MPa。热震实验表明, 梯度涂层在300℃下经历30余次热循环, 表现出较好的抗热震性能。     

TiC与TiC-WC的添加对FeAl/Al2O3复合材料力学性能的影响

在FeAl/Al2O3复合材料基体中分别加入TiC或TiC-WC固溶体可显著提高其抗弯强度。当添加20％TiC和20％TiC-WC固溶体时，复合材料的抗弯强度分别达到1028．46MPa和1328．72MPa，但其断裂韧性分别降低约40％和30％。当TiC-WC固溶体加入量为5％时，可同时提高复合材料的抗弯强度和断裂韧性。     

Slip casting of Al2O3 and Al2O3/ZrO2 composites

Al₂O₃ and Al₂O₃/ZrO₂ composites have been fabricated by slip casting from aqueous suspensions. The physical and structural characteristics of the starting powders, composition of the suspensions, casting behaviour, microstructure of the green and fired bodies and the mechanical properties of the products were investigated. The addition of ZrO₂ to Al₂O₃ leads to a significant increase in fracture toughness when ZrO₂ particles are retained in the tetragonal form (transformation-toughening mechanism) but when microcracking (due to the spontaneous transformation of ZrO₂ from the tetragonal phase to the monoclinic one) is dominant, an excellent toughness value is accompanied by a drastic drop in strength and hardness.     

Effect of graphite flake on the mechanical properties of hot pressed ZrB2-SiC ceramics

A ZrB₂ ceramic containing 20 vol.% SiC and 10 vol.% graphite flake (ZrB₂-SiC-G) was fabricated by hot pressing. It was shown that the fracture toughness was improved due to the introduction of graphite flake, whereas the flexure strength and hardness decreased slightly. The fracture toughness of ZrB₂-SiC-G composite was 6.1 ± 0.3 MPa·m^1/2, which was much higher than that of monolithic ZrB₂, ZrB₂-SiC composite and similar ZrB₂-SiC-C composite. The toughening mechanisms are crack deflection and branching as well as stress relaxation near the crack tip. The results here pointed to a potential method for improving fracture toughness of ZrB₂-based ceramics.     

Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

Effect of chemical modification conditions on the sintering behavior of TiC powders

Dense ceramics have been produced from a chemically modified titanium carbide powder. Chemical modification was carried out by siliciding titanium carbide powder in a gaseous SiO atmosphere at 1350°C. This treatment produced a Ti₃SiC₂ layer (up to 19 wt %) on the surface of the TiC particles. Hot pressing at a temperature of 1600°C and pressures from 10 to 20 MPa ensured effective densification of the modified powders. The density of the resultant material reaches 4.8 g/cm³, with a residual porosity under 2%. Its bending strength and fracture toughness are 330 ± 50 MPa and 6.2 ± 0.6 MPa m^1/2, respectively.     

Microstructure and mechanical properties of ZrB2-SiC composites

A ZrB₂-based composite containing 20 vol.% nanosized SiC particles (ZSN) was fabricated at 1900 °C for 30 min under a uniaxed load of 30 MPa by hot-pressing. The microstructure and mechanical properties of the composite were investigated. It was shown that the grain growth of ZrB₂ matrix was effectively suppressed by submicrosized SiC particles located along the grain boundaries. In addition, the mechanical properties of ZSN composite were strongly improved by incorporating the nanosized SiC particles into a ZrB₂ matrix, especially for flexural strength (925 ± 28 MPa) and fracture toughness (6.4 ± 0.3 MPa•m^1/2), which was much higher than that of monolithic ZrB₂ and ZrB₂-based composite with microsized SiC particles, respectively. The formation of intragranular nanostructures plays an important role in the strengthening and toughening of ZrB₂ ceramic.     

Feasibility study of a tungsten wire-reinforced tungsten matrix composite with ZrOx interfacial coatings

Brittleness problem imposes a severe restriction on the potential application of tungsten as high-temperature structural material. In this paper, a novel toughening method for tungsten is proposed based on reinforcement by tungsten wires. The underlying toughening mechanism is analogous to that of fiber-reinforced ceramic matrix composites. Strain energy is dissipated by debonding and frictional sliding at engineered fiber/matrix interfaces. To achieve maximum composite toughness fracture mechanical properties have to be optimized by interface coating. In this work, we evaluated six kinds of ZrO_x-based interface coatings. Interfacial parameters such as shear strength and fracture energy were determined by means of fiber push-out tests. The parameter values of the six coatings were comparable to each other and satisfied the criterion for crack deflection. Microscopic analysis showed that debonding occurred mostly between the W filament and the ZrO_x coating. Feasibility of interfacial crack deflection was also demonstrated by a three-point bending test.