硅液相浸渍反应制备TiC/SiC和TiN/SiC复相陶瓷

以滤纸、酚醛树脂和氧化钛为原料,经过模压成型、固化、碳化及不同条件下渗硅制备了TiC/SiC和TiN/SiC复相陶瓷。通过X射线衍射和扫描电子显微镜研究了TiC/SiC和TiN/SiC复相陶瓷的微观结构和物相组成,测量了复相陶瓷的弯曲强度和断裂韧性。结果表明:真空条件下液态渗硅获得的TiC/SiC复相陶瓷具有多孔的微观结构,其弯曲强度和断裂韧性较小。氮气气氛下液态渗硅制备的TiN/SiC复相陶瓷结构致密,有较高的弯曲强度和断裂韧性。不同反应生成的TiC,TiN陶瓷颗粒对液态硅的润湿性不同,使得生成的复相陶瓷具有不同的微观结构。TiN/SiC复相陶瓷中TiN颗粒的引入,在基体与第二相颗粒间的界面上产生拉应力和压应力,使达到这一区域的裂纹偏转,从而获得增韧效果。     

The Influence of Water on the Fracture of Magnesium Aluminate (MgAl2O4) Spinel

The influence of water on the fracture of magnesium aluminate (MgAl₂O₄) ceramics and spinel single crystals is investigated in order to determine whether adsorption plays an important role during subcritical crack growth as it does for MnZn ferrites, a compound with the same spinel structure. The fracture toughness of porous and dense polycrystalline ceramic and single crystal specimens are determined using a single edge notched beam setup at different crosshead velocities and humidities. Furthermore, in order to investigate whether a preferred plane of fracture is present, electron backscattered diffraction (EBSD) has been performed. It is found that the fracture toughness decreases with increasing humidity for dense ceramics, indicating that adsorption plays an important role as it does for MnZn ferrites. However, porous ceramics only show a sharp decrease between 0% and 2–10% relative humidity (RH) and hardly decreases onwards. This implies that the pores inhibit in some way the effect of adsorption during fracture. The exact mechanism remains unclear. EBSD measurements indicated that a preferred plane is absent. Therefore, the fracture of spinel single crystal along the (100) and (111) planes was chosen for further detailed investigation. It is revealed that between 2% and 40% RH both planes show a reduction in fracture surface energy of ∼46%. Using reported computer simulations results, it can be concluded that the surfaces are partially hydrated when being fractured.     

A critical evaluation of indentation crack lengths in air

An extensive overview is presented of Vickers indentation crack lengths in ceramics in air. Measurement of such crack lengths is one of the most common and powerful assessments of the fracture properties of ceramics and the overview provides a critical evaluation of observed behavior as functions of material type and indentation load, and an extensive basis for comparison of results from new materials and analyses. The overview considers single crystals, polycrystals, transforming materials, glasses, and multiphase materials, including cermets, glass-ceramics, and tooth enamel. The coverage extends over structural and electronic ceramics, including oxides, carbides, nitrides, and titanates. The data are presented in a single format for ease of interpretation in terms of idealized indentation fracture and for inter-material comparisons; most data are unique to this work, but the results of selected studies from the published literature are included. The overview considers the precision and accuracy of crack length measurements and demonstrates a simple quantitative evaluation and ranking scheme for ceramic fracture based on load-adjusted crack length and cracking susceptibility. Indentation hardness and cracking threshold are also determined and related to the susceptibility. Material toughness is related to cracking susceptibility by fracture mechanics analyses: typical crack length measurements in air are shown to provide estimates of inert toughness with a relative uncertainty of ±50%.     

Methodology for measuring fracture toughness of ceramic materials by instrumented indentation test with vickers indenter

Virtual crack closure technique and elastoplastic finite element method were employed to calculate the stress intensity factors (SIF) of ceramic materials on the tip of both half‐penny crack (HPC) and radial crack (RC) induced by Vickers indenter and the value of fracture toughness (K_IC) was extracted by the design of equi‐SIF contour of HPC and RC crack front. Through dimensional theorem and regressive analysis, a functional relationship between instrumented indentation parameters, crack length of Vickers impression and fracture toughness of ceramic materials was established, thus a novel methodology has been presented for measuring fracture toughness of ceramic materials by instrumented Vickers indentation. Both numerical analysis and experiments have indicated that this methodology enjoys higher measurement precision compared with other available indentation methods. The methodology is universally suitable for HPC, RC as well as transition cracks and capable of determining fracture toughness and elastic modulus in a single indentation test. In addition, it saves the effort of measuring the diagonal length of Vickers impression in case that the impression remains unclear.     

陶瓷材料断裂韧性测试新技术：静态爆破剂预制裂纹的研究

准确测试陶瓷材料断裂韧性Ｋ１Ｃ的关键是预制具有原生裂纹的试样。本文以单边切口梁法测试Ｋ１Ｃ为基础，提出了一种简便而有效的陶瓷材料原生裂纹的预制方法－静态膨胀法。研究结果表明：静态膨胀法中裂纹的扩展是稳态的；通过调节影响微裂纹产生与扩展的多种因素，可以准确地控制裂纹扩展的深度，预制出合适的原生裂纹，为准确评价结构陶瓷的断裂韧性提供了一种有效可行的方法。     

Fracture Toughness of a Silicon Nitride/Silicon Carbide Nanocomposite at 1350°C

The fracture toughness of a hot-pressed silicon nitride/silicon carbide (Si₃N₄/SiC) nanocomposite and reference monolithic Si₃N₄ has been investigated in four-point bending at 1350°C in air, using different loading rates (0.01-1 mm/min). Single-edge V-notched bend specimens that were prepared by polishing the notch tip to a radius of <10 µm, using 1 µm diamond paste, were used for the fracture toughness measurement. Slow crack growth (SCG) prior to catastrophic failure was detected at all applied loading rates at 1350°C. The fracture toughness at 1350°C, as calculated using the actual crack size measured on the fracture surface after the bend test, increased in both ceramics with decreasing loading rate and increasing area of the SCG region.     

On the Vickers Indentation Fracture Toughness Test

The Vickers indentation fracture toughness test, or VIF, is addressed by considering its origins and the numerous equations that have been applied along with the technique to estimate the fracture resistance, or the K _{I c} of ceramics. Initiation and propagation of cracks during the VIF test are described and contrasted with the pre-cracking and crack growth for internationally standardized fracture toughness tests. It is concluded that the VIF test technique is fundamentally different than standard fracture toughness tests. The VIF test has a complex three-dimensional crack system with substantial deformation residual stresses and damage around the cracks. The VIF test relates to an ill-defined crack arrest condition as opposed to the rapid crack propagation of the standardized fracture toughness tests.
Previously published fracture toughness results employing the VIF technique are reviewed. These reveal serious discrepancies in reported VIF fracture toughness values. Finally, recent fracture resistance measurements by the VIF technique for the Standard Reference Material SRM 2100 are presented. These are compared with standardized test results for the same material. It is concluded that the VIF technique is not reliable as a fracture toughness test for ceramics or for other brittle materials. What the VIF actually measures in terms of fracture resistance cannot be readily defined. It is recommended that the VIF technique no longer be acceptable for the fracture toughness testing of ceramic materials.     

Short-Crack Toughness and Abrasive Machining of Silicon Nitride

Hardness and toughness are often used to analyze the abrasive machining behavior of ceramic materials. However, toughness values of silicon nitride ceramics with microstructures containing elongated grains increase with crack extension. The present study investigates the effect of toughness on the process of abrasive machining to determine which value of toughness should be used in the analysis. The toughness curves (i.e., toughness as a function of crack length) of ten different silicon nitride materials are characterized by an indentation-strength technique and an indentation technique. The forces in surface grinding are measured as a function of the depth of cut. Examination of ground surfaces by scanning electron microscopy indicates that the material-removal processes in grinding follows the formation of short cracks (i.e., microcracks) and grain-scale material dislodgement. An indentation fracture model for material removal in abrasive machining is used to correlate the grinding forces with toughness and hardness of the materials. An agreement is obtained between the experimental results and the indentation model only when the toughness associated with short cracks is used. This study shows the importance of using appropriate toughness values corresponding to the microfracture processes in analyzing abrasive machining results for materials possessing rising toughness curves.     

Mechanical aspects of ceramic membrane materials

Interest in ceramic transport membrane materials has increased significantly leading also to questions with respect to mechanical reliability and robustness, hence, requiring knowledge of the mechanical properties. The current review focuses on the mechanical properties of such ceramics, emphasizing in particular relationships between mechanical properties, non-elastic effects, phase changes and materials’ stability. Room and elevated temperature application is considered with a main emphasis on elastic and creep deformation as well as fracture. Consideration is given to dense membranes as well as porous substrate materials for advanced asymmetric concepts. Properties are summarized for selected oxygen and proton conductors. Furthermore, mechanical properties of some selected porous ceramic and metallic substrate materials are given. In addition to the failure probability associated with the Weibull distribution of fracture stresses, creep rupture of dense materials and enhanced creep deformation of porous materials are aspects that need special consideration in the application of these materials in gas separation systems.     

Fracture toughness of glasses and hydroxyapatite: A comparative study of 7 methods by using Vickers indenter

Numerous methods have been proposed to estimate the indentation fracture toughness Kic for brittle materials. These methods generally uses formulæ established from empirical correlations between critical applied force, or average crack length, and classical fracture mechanics tests. This study compares several models of fracture toughness calculation obtained by using Vickers indenters. Two optical glasses (Crown and Flint), one vitroceramic (Zerodur) and one ceramic (hydroxyapatite) are tested. Fracture toughness and hardness are obtained by using instrumented Vickers indentation at micrometer scale. Young's moduli are obtained by instrumented Berkovich indentation at nanometer scale. Fracture toughness is calculated with models involving crack length measurements, and by models free of crack length measurements by considering critical force, chipping, pop-in. Finally, method based on the cracking energy, commonly employed for coated materials is also used.The aim of this work is to compare seven methods, which enable the facture toughness determination, on four brittle materials. To do so, it was necessary to determine some specific constant in the case of Vickers tip use.On the one hand, results show that methods using crack length, critical force, edge chipping or pop-in lead to comparable results, and the advantages and drawbacks are highlighted. On the other hand, the indentation energy method leads to underestimated results of about 20%.     

A New Method for Precracking Beam for Fracture Toughness Experiments

A simple and versatile precracking method using a triangular notch as a crack starter in limited bending was developed, which is suitable for both brittle ceramics and quasi-plastic materials that are difficult to precrack by the conventional bridge-indentation technique. Slow growth of large crack in brittle or quasi-brittle ceramics was controlled and observed in situ in this way. The precracking tests performed on various ceramics exhibited high reliability and feasibility. The precracked specimens were subsequently used to measure the fracture toughness, and the resultant data showed that the fracture toughness determined by using the precracked specimens reflected the minimum value of the toughness measured in single edge-notched beam (SENB) tests.     

Effect of pH variation on the subcritical crack growth parameters of glassy matrix ceramics

The goals of our study were to calculate the subcritical crack growth (SCG) parameters of two veneering ceramics stored in water or Streptococcus mutans (S. mutans) biofilm and remineralizing medium, with indentation flaws. Feldspar (VM7) and leucite-reinforced (VM13) glass ceramic disks (Vita Zahnfabrik, Bad Säckingen, Germany) were made according to ISO 6872. Some specimens were indented with a Vickers diamond and the crack dimensions were measured. The specimens were fractured for a calculation of inert strength or further stored in water or submitted to pH variation, under preloading tension. Finally, the SCG parameters were calculated after the specimens were fractured under four stressing rates (MPa/s). Weibull analysis was conducted on non-indented specimens. XPS was performed as qualitative analysis. The subcritical crack of leucite ceramic did not vary with the media storage, but the glass-ceramic experienced a retarded growth after pH variation. The materials presented low Weibull modulus. Qualitative elemental analyses showed chemical modification on both ceramics. Therefore, the crack growth of leucite-reinforced ceramic was less affected by the environment pH than glass-ceramic.     

Fracture mechanics properties of fused silicas used for international space station windowpanes

The fracture toughness and slow crack growth (SCG) parameters of a quartz-based silica and a high-purity fused silica were measured as part of a program to review the reliability of the International Space Station windows. The materials exhibit the same fracture toughness (.75 MPa m^1/2 in N₂) and very similar SCG parameters. The literature on fused silica indicates excellent agreement of fracture toughness, but a very wide range of SCG parameters, even from the same institution, with strength-based methods usually yielding a lower power law exponent than direct crack velocity measurements. Use of the exponential function is shown to provide better agreement between test methods, with velocity curves derived from strength tests of bare fiber and polished or ground test specimens paralleling those from wide-range, direct crack velocity observations, implying that constant stress rate tests can predict long lifetime via the exponential function. However, much variation still exists. SCG parameters for soda–lime silicate are much less sensitive to the test method than fused silica. Static load tests and stress intensity measurements resulted in a fatigue threshold of .3 MPa m^1/2 for fused silica.     

Elastic/Plastic Indentation Damage in Ceramics: The Median/Radial Crack System

A theory for describing the evolution of the median/radial crack system in the far field of sharp-indenter contacts is developed. Analysis is based on a model in which the complex elastic/plastic field beneath the indenter is resolved into elastic and residual components. The elastic component, being reversible, assumes a secondary role in the fracture process: although it does enhance downward (median) extension during the loading half-cycle, it suppresses surface (radial) extension to the extent that significant growth continues during unloading. The residual component accordingly provides the primary driving force for the crack configuration in the final stages of evolution, where the crack tends to near-half-penny geometry. On the hypothesis that the origin of the irreversible field lies in the accommodation of an expanding plastic hardness impression by the surrounding elastic matrix, the ensuing fracture mechanics relations for equilibrium crack growth are found to involve the ratio hardness-to-modulus as well as toughness. Observations of crack evolution in soda-lime glass provide a suitable calibration of indentation coefficients in these relations. The calibrated equations are then demonstrated to be capable of predicting the widely variable median and radial growth characteristics observed in other ceramic materials. The theory is shown to have a vital bearing on important practical areas of ceramics evaluation, including toughness and strength.     

Measurement of the Fracture Toughness of Ceramic Materials Using a Miniaturized Disk-Bend Test

The fracture toughness of several ceramic materials has been measured using a miniaturized disk-bend test apparatus and methodology based on small disk-shaped samples 3 mm in diameter. The method involves the Vickers indentation of specimens ranging in thickness from 300 to 700 μm, and testing them in a ring-on-ring bending mode. New experiments on a glass-ceramic (GC) and Si₃N₄ have been performed to demonstrate the validity of the technique, supplementing the original work on ZnS. The fracture resistances of these materials increase with increasing crack length ( R -curve behavior). The data are analyzed using a specific model for the relationship between fracture resistance and crack length; this model enables the R -curve behavior to be treated analytically, and the fracture resistance at "infinite" crack length to be evaluated using a straightforward graphical procedure. The resulting values of the fracture toughness for ZnS, GC, and Si₃N₄ are 0.74 ± 0.02, 2.18 ± 0.09, and 4.97 ± 0.07 MPa-m^1/2, respectively, which are all in very good agreement with values obtained from conventional fracture toughness tests on large specimens. The results verify the utility of the miniaturized diskbend method for measuring the fracture toughness of brittle materials.     

Determining specimen thickness limit in fracture toughness tests applied to dental ceramics and metal alloy interfaces

The aims of the current study are to present computational simulations based on the finite element method in order to determine the lowest viable thickness of materials used to make ceramic samples based on the interface of groups of materials (Ni–Cr/ceramics, alumina/ceramics), and samples made of each of these materials, alone; as well as to report the effect of variation in the stress intensity factor of these interfaces (β). Test conditions were simulated in Abaqus CAE software and mesh features focused the crack tip. Fracture toughness analysis was carried out by simulating the three-point bending test (SEVNB specimen of the Fracture Mechanic standards). Based on the present results, the lowest material thickness necessary to meet the stress intensity requirement at the crack tip was 8 mm of each material, under symmetry condition, for sandwich composition. Such a thickness included fracture process zone (FPZ) size and plastic zone (PZ). Sandwich thickness was enough to maintain the test conditions established for the standards. Samples produced in the present study met the requirements of the fracture toughness test, based on the ASTM E?399 standard - specimens with the lowest possible sandwich thickness were obtained and they met the stress intensity requirements of the crack tip. This finding pointed towards a sample based on using a reduced amount of test materials - such as those used for dental restoration. The lowest material thickness in the sandwich was 8 mm, for all groups of materials, under symmetry conditions. This thickness includes fracture process zone size and plastic zone size. The herein proposed sandwich thickness was enough to maintain the test conditions established by fracture mechanic standards.     

Biaxial strength and slow crack growth in porous alumina with silica sintering aid

Biaxial strength, fracture toughness and subcritical crack growth are reported for coarse grained porous alumina ceramics. The materials were prepared with a varying amount of a silica sintering aid, which resulted in the formation of a glassy secondary phase at the grain boundaries. Crystalline mullite was additionally found in the material with the highest silica content. The biaxial strength, measured by Ball-on-Ring and Ball-on-3-Balls, was highest for the material without mullite at the grain boundaries, and the biaxial strength decreased with increasing porosity. The fracture toughness of the materials was in the range of 1.7–1.9 MPa m^0.5. Measurements of subcritical crack growth by a modified lifetime method in air and aqueous environments demonstrated a higher crack growth rate in water and acid relative to in air. The effect of porosity and grain boundary phase were discussed in relation to subcritical crack growth and fracture mode in the coarse grained alumina ceramics.     

Temperature dependent fracture toughness model for whisker-reinforced ceramic matrix composites

A temperature dependent fracture toughness model for whisker-reinforced ceramic matrix composites was developed in this study, which considers the effects of matrix fracture toughness, residual thermal stress, crack bridging, crack deflection, and their temperature dependence. Its predicted results were compared with the fracture toughness of six types of whisker-reinforced ceramic matrix composites at different temperatures, and good agreement between predicted results and experimental results is obtained. Furthermore, based on this model, we systematically analyzed the effects of the volume fraction and aspect ratio of whisker, Young's modulus of matrix and whisker, thermal expansion coefficient difference, stress-free temperature, the ratio between the fracture energy of matrix and that of interface, on their temperature dependent fracture toughness for the first time. Finally, insights and suggestions which could help to optimize and improve the composite fracture toughness at different temperatures are provided.     

Prediction of crack deflection in porous/dense ceramic laminates

The arrangement of ceramic layers in laminated structures is an interesting way to enhance the flaw tolerance of brittle ceramic materials. The interfaces are expected to deflect cracks, increasing the fracture energy of the laminate compared to a monolithic material and thus raising the toughness.Laminates have been fabricated with alternating dense and porous layers of the same material, i.e. SiC or B₄C, in order to obtain a good chemical compatibility between the laminas and almost no thermal residual stresses. Porosity, in the porous layers, is achieved by incorporating organic particles which are removed during the debinding step. In this context, the target of this study is to predict the volume fraction of pores, in the porous layer, required to cause crack deflection.The proposed criterion derives from an energy balance. It relies on a two-scale analysis taking into account the laminated structure of the material. It can be written in terms of two relevant material parameters: the ratio of Young's moduli of the dense and porous materials and toughness ratios. A unique function depending on the volume fraction of pores can be used to express the two above-mentioned ratios. Assuming a cubic lattice of spherical voids, the parameters of the porous ceramic depend linearly on the porosity and vanish at the point of percolation of pores. As a consequence, the criterion can be rewritten in term of a single parameter: the porosity.Crack deflection is permitted only for very high values of the porosity. Predicted values agree satisfactorily with experiments on SiC and B₄C. The comparison with the He and Hutchinson criterion shows that this latter underestimates the correct value.