氮化硅陶瓷晶界相研究进展

晶界相对氮化硅陶瓷性能有重要作用,研究晶界相的性能对断裂韧性、高温强度的提高有重要意义。介绍了氮化硅陶瓷的显微结构、性能和应用,重点评述了氮化硅陶瓷晶界相的形成、特点、影响因素以及晶界相对力学性能和摩擦磨损性能的影响。提出了当前研究中存在的问题,并展望了未来氮化硅的研究方向。     

Fabrication,formulation, mechanical properties,and oxidation of sintered Si3N4 ceramics using disc specimens

Abstract

The high cost and lengthy preparation time of conventional ceramic bend-bar strength specimens is holding back the development of sintered silicon nitride ceramics having good high–temperature properties. The equipment now available for high–temperature sintering enables discs of high–strength sintered silicon nitride to be fabricated in a wide range of formulations. The use of disc specimens has led to a considerable increase in the rate and volume of research into mechanical properties and behaviour in a high-temperature environment. This research has demonstrated the value of using disc specimens to reduce the time and cost of programmes for developing materials suitable for gas-turbine and other demanding applications.

MST/232     

Fracture Resistance of Ceramics: Edge Fracture Method

Fracture resistance of macrohomogeneous linear elastic yttria, scandia, alumina, zirconia, and silicon nitride ceramics was studied upon flaking of the edges of rectangular specimens with the Rockwell indenter. The correlation between the obtained estimates and fracture toughness test results gained by the single-edge V-notched beam method was demonstrated. Loads giving rise to the flaking of a part of the edge and distances from this edge to the chip scar on the specimen surface were measured. The ratio of those values was considered as a flaking toughness characteristic. The data obtained were statististically reliable (based on more than a hundred determinations). This procedure termed the edge fracture method can be used along with other known fracture toughness test methods for ceramics, its application is especially advantageous when ceramic item sizes are comparable with those of the standard specimens or when expensive materials (e.g., nanoceramics) are tested. __________ Translated from Problemy Prochnosti, No. 5, pp. 84 – 92, September – October, 2005.     

Face/core interface fracture characterization of mixed mode bending sandwich specimens

Debonding of the core from the face sheets is a critical failure mode in sandwich structures. This paper presents an experimental study on face/core debond fracture of foam core sandwich specimens under a wide range of mixed mode loading conditions. Sandwich beams with E‐glass fibre face sheets and PVC H45, H100 and H250 foam core materials were evaluated. A methodology to perform precracking on fracture specimens in order to achieve a sharp and representative crack front is outlined. The mixed mode loading was controlled in the mixed mode bending (MMB) test rig by changing the loading application point (lever arm distance). Finite element analysis was performed to determine the mode‐mixity at the crack tip. The results showed that the face/core interface fracture toughness increased with increased mode II loading. Post failure analysis of the fractured specimens revealed that the crack path depends on the mode‐mixity at the crack tip, face sheet properties and core density.     

Experimental fracture investigation of CNT/epoxy nanocomposite under mixed mode II/III loading conditions

For the first time, the brittle fracture of epoxy‐based nanocomposite reinforced with MWCNTs (multi‐walled carbon nanotubes) and subjected to mixed mode II/III loading conditions is investigated. This experimental investigation is carried out using a newly developed test configuration. Araldite LY 5052 epoxy, which is a resin frequently used in aerospace industry, is utilized to fabricate pure epoxy and nanocomposite test specimens with two different MWCNTs contents of 0.1 and 0.5 wt%. The obtained experimental results reveal that adding MWCNTs to epoxy resin up to 0.5 wt% improves the fracture toughness under pure mode II and pure mode III loading with an increasing trend. This is while the improvement under mixed mode II/III loading is reduced by adding nanotubes more than 0.1 wt%. To justify the variations of fracture toughness in terms of nanoparticles content, SEM (scanning electron microscopy) photographs of the fracture surfaces of the specimens in the vicinity of the initial crack front are prepared. Additional fracture mechanisms caused by adding carbon nanotubes are discussed in detail based on the provided SEM images.     

R-curve measurement of silicon nitride ceramics using single-edge notched beam specimens

R-curve behaviour of three kinds of silicon nitride-based ceramics has been studied using the single-edge notched beam (SENB) technique. If the notch is deep enough, the specimen shows stable fracture during the bending test, even when the sample is a brittle material. The conditions required to obtain stable fracture in the bending test are clarified by the analysis. The crack length of the specimen was also calculated from the changing load during the fracture test. In this study, coarse-grained silicon nitride shows a large increase of theR-curve. On the other hand, silicon nitride with silicon carbide whiskers shows noR-curve increase. The rise of theR-curve should be related to the microstructure of the ceramics, and especially to the grain size of the specimen, because silicon carbide whiskers are not large compared to the silicon nitride grains, and silicon carbide can reduce the grain growth of silicon nitride during sintering.     

Investigation of ductile rupture in U‐notched Al 6061‐T6 plates under mixed mode loading

The aim of the present research is to evaluate ductile failure of U‐notched components under mixed mode I/II loading conditions. For this purpose, first, several rectangular plates made of the aluminium alloy Al 6061‐T6 and weakened by central bean‐shaped slit with two U‐shaped ends are tested under mixed mode I/II loading conditions, and the load‐carrying capacity of the specimens are experimentally measured. Then, using the equivalent material concept, Al 6061‐T6, which is a highly ductile material, is equated with a virtual brittle material, and the load‐carrying capacity of the same U‐notched specimens virtually made of the equivalent material is theoretically predicted by using two well‐known stress‐based brittle fracture criteria. Finally, the theoretical failure loads of the virtual specimens are compared with the experimental ones of the real Al 6061‐T6 specimens. It is revealed that the experimental results could very well be predicted by means of both brittle fracture criteria without conducting time‐consuming elastic–plastic analyses.     

A new fixture for fracture tests under mixed mode I/II/III loading

In this paper, a new loading device for general mixed mode I/II/III fracture tests is designed and recommended. Finite element analyses are conducted on the proposed apparatus to evaluate the fracture parameters of the tested samples under various mixed mode loading conditions. The numerical results revealed that the designed loading fixture can generate wide varieties of mode mixities from pure tensile mode to pure in‐plane and out‐of‐plane shear modes. The accuracy of the proposed fixture is evaluated by conducting a wide range of fracture tests on compact tension shear (CTS) specimens made of polymethyl methacrylate (PMMA). The experimental results are then compared with the theoretical predictions obtained by the Richard criterion. A good consistency is observed between the experimental results and theoretical predictions.     

State‐of‐the‐art review on the local strain energy density concept and its relation to the J‐integral and peak stress method

The local average strain energy density (SED) approach has been proposed and elaborated by Lazzarin for strength assessments in respect of brittle fracture and high‐cycle fatigue. Pointed and rounded (blunt) V‐notches subjected to tensile loading (mode 1) are primarily considered. The method is systematically extended to multiaxial conditions (mode 3, mixed modes 1 and 2). The application to brittle fracture is documented for PMMA flat bar specimens with pointed or rounded V‐notches inclusive of U‐notches. Results for other brittle materials (ceramics, PVC, duraluminum and graphite) are also recorded. The application to high‐cycle fatigue comprises fillet‐welded joints, weld‐like shaped and V‐notched base material specimens as well as round bar specimens with a V‐notch. The relation of the local SED concept to comparable other concepts is investigated, among them the Kitagawa, Taylor and Atzori–Lazzarin diagrams, the Neuber concept of fictitious notch rounding applied to welded joints and also the J‐integral approach. Alternative details of the local SED concept such as a semicircular control volume, microrounded notches and slit‐parallel loading are also mentioned. Coarse FE meshes at pointed or rounded notch tips are proven to be acceptable for accurate local SED evaluations. The peak stress method proposed by Meneghetti, which is based on a notch stress intensity factor consideration combined with a globally even coarse FE mesh and is used for the assessment of the fatigue strength of welded joints, is also presented.     

Investigation of mixed mode brittle fracture in rounded-tip V-notched components

A criterion is proposed for brittle fracture analysis in rounded-tip V-notched components. This criterion, called RV-MTS, is developed based on the maximum tangential stress (MTS) criterion proposed earlier for investigating mixed mode brittle fracture in sharp cracks. Using the RV-MTS criterion, a set of fracture curves is presented based on the notch stress intensity factors (NSIFs) for predicting mixed mode and also pure mode II fracture toughness of rounded-tip V-notches. The criterion is also able to predict fracture initiation angles under mixed mode loading. The validity of the criterion is evaluated by several fracture tests performed on the rounded-tip V-notched Brazilian disc (RV-BD) specimens made of PMMA. A good agreement is shown to exist between the theoretical predictions and the experimental results for various notch opening angles and different notch radii.     

A novel fixture for mixed mode I/II/III fracture testing of brittle materials

A novel test‐loading device was suggested in order to study the fracture behavior of brittle materials under mixed mode I/II/III loading conditions. A version of the compact tension shear specimen was used as the test configuration. Using a three‐dimensional finite element analysis, the influence of mode mixity on the stress intensity factors, the T‐stress, and 3‐D plastic zone around the crack tip was investigated. In addition, an experimental study was performed on an epoxy polymer using the proposed setup. Finally, the fracture toughness of pure epoxy was measured under several loading conditions. The numerical and experimental results manifested that the proposed setup is able to determine a full range of mixed mode I/II/III fracture properties. At the end, the fracture envelope obtained using the practical study was compared with various three‐dimensional fracture criteria. A negligible discrepancy was concluded between the practical data and the theoretical data estimated by the maximum mean principle stress criterion.     

水溶性胶态成型工艺制备氮化硅耐磨结构陶瓷

以氮化硅粉末为原料, 采用水溶性胶态成型工艺制备高耐磨氮化硅陶瓷. 采用正交设计的方法来优化制备高品质注浆料, 并研究了掺杂分散剂后Zeta电位的变化. 同时, 还对氮化硅陶瓷烧结体的显微结构、力学性能和耐磨性能进行了研究. 结果表明: 当氮化硅浆料中固相体积分数为45%时, 可制得体积密度较高的精细氮化硅陶瓷材料, 断裂韧性可达7.21MPa·m^1/2, 硬度为9.30GPa. 通过抗耐磨损实验研究表明: 干摩擦条件下, 氮化硅陶瓷发生了晶粒脆性断裂和脱落; 水润滑条件下, 摩擦表面产生了氢氧化硅 反应膜, 降低了磨损, 主要是化学腐蚀磨损.     

Wide range data for crack tip parameters in two disc-type specimens under mixed mode loading

Disc-type specimens are among favorite test samples for determining mode I and mixed mode fracture toughness in brittle materials like rocks, brittle polymers, ceramics, etc. In this research, the finite element method is used to analyze two disc-type specimens: a semi-circular disc specimen containing an edge crack and subjected to three-point-bend loading (SCB specimen), and a centrally cracked circular disc subjected to diametral compressive loading, often called the Brazilian disc specimen. The crack parameters K_I, K_II and T are calculated for different mode mixities from pure mode I to pure mode II. Although the stress intensity factors K_I and K_II are presented mainly for validation of the analyses, they are also used for determining the crack angle corresponding to pure mode II for each specimen. It is shown that in general the T-stress increases for larger crack angles. While the T-stress in the Brazilian disc specimen is always negative for any combinations of mode I and mode II, the sign of T-stress in the SCB specimen depends on the mode mixity. A very good agreement is shown to exist between the calculated results for T and those very limited data presented in other papers.     

A material model to reproduce mixed‐mode fracture in concrete

This paper presents a material model to reproduce crack propagation in cement‐based material specimens under mixed‐mode loading. Its numerical formulation is based on the cohesive crack model, proposed by Hillerborg, and extended for the mixed‐mode case. This model is inspired by former works by Gálvez et al but implemented for its use in a finite element code at a material level, that is to say, at an integration point level. Among its main features, the model is able to predict the crack orientation and can reproduce the fracture behaviour under mixed‐mode fracture loading. In addition, several experimental results found in the literature are properly reproduced by the model.     

Fracture Toughness of Advanced Ceramics at Room Temperature

This report presents the results obtained by the five U.S. participating laboratories in the Versailles Advanced Materials and Standards (VAMAS) round-robin for fracture toughness of advanced ceramics. Three test methods were used: indentation fracture, indentation strength, and single-edge pre-cracked beam. Two materials were tested: a gas-pressure sintered silicon nitride and a zirconia toughened alumina. Consistent results were obtained with the latter two test methods. Interpretation of fracture toughness in the zirconia alumina composite was complicated by R-curve and environmentally-assisted crack growth phenomena.     

An experimental and theoretical comparison of CCNBD and CCNSCB specimens for determining mode I fracture toughness of rocks

The cracked chevron notched Brazilian disc (CCNBD) specimen, suggested by the International Society for Rock Mechanics for testing mode I fracture toughness of rocks, usually yields rather conservative toughness measurements, and the reasons have not been fully explored. In this study, the CCNBD method is compared with the cracked chevron notched semicircular bending (CCNSCB) method in the fracture process zone (FPZ) and its influence on the fracture toughness measurement. Theoretical analysis reveals that the FPZ is longer in the CCNBD specimen than in the CCNSCB specimen using a relatively large support span, the toughness measurement using the former is affected more seriously by the presence of FPZ, and thus the CCNBD method is usually, more or less, conservative compared with the CCNSCB method. These inferences are further validated by experimental results, which indicate that the CCNBD test indeed produces much lower fracture toughness values and even the results of 75‐mm radius CCNBD specimens are still lower than those of 25‐mm radius CCNSCB specimens. Consequently, due to smaller FPZ, the CCNSCB specimen with a relatively large span is more likely to produce comparably accurate or representative toughness value, and it may be more suitable than the CCNBD specimen for the engineering applications that require more representative or less conservative fracture toughness.     

Fracture toughness testing of materials by the EF method

Experimental evidence is presented that fracture toughness testing of ceramics by the EF method (fracture of the edge of a rectangular specimen as a result of indentation), which does not rely on modern fracture mechanics concepts, in contrast to its conventional analogs, is easy to implement and can be used under standard laboratory conditions. Testing results for yttria, alumina, zirconia, and silicon nitride ceramics confirm that this method is suitable for practical application. The EF method is well suited for testing nanostructured, dental, and other ceramics, as well as semiconductors, and is capable of providing reliable fracture toughness data even if the amount of material for testing is limited.     

The structure of slow crack interfaces in silicon nitride

Fracture interfaces formed in silicon nitride at high temperatures were studied using light and electron microscopy. The structure of the fracture interface depended on the type of silicon nitride fractured. High-purity, reaction-bonded silicon nitride always formed flat, relatively featureless, fracture surfaces. Fracture occurred by a brittle mode even at the highest temperature (1500° C) studied. The critical stress intensity factor for reaction-bonded silicon nitride ( 2.2 MN m^–3/2) is relatively low and is insensitive to temperature. By contrast, hot-pressed silicon nitride gave evidence of plastic flow during fracture at elevated temperatures. Crack growth in magnesia-doped, hot-pressed silicon nitride occurs by creep, caused by grain boundary sliding and grain separation in the vicinity of the crack tip. As a consequence of this behaviour, extensive crack branching was observed along the fracture path. The primary and secondary cracks followed intergranular paths; sometimes dislocation networks, generated by momentary crack arrest, were found in grains bordering the crack interface. As a result of the high temperature, cracks were usually filled with both amorphous and crystalline oxides that formed during the fracture studies. Electron microscopy studies of the compressive surfaces of fourpoint bend specimens gave evidence of grain deformation at high temperatures by diffusion and dislocation motion.     

Mixed Mode Brittle and Ductile Fracture of a High Strength Rotor Steel at Room Temperature

The mixed mode fracture of a high strength rotor steel has been investigated at room temperature using single edge notched specimens. In mode I, and for limited amounts of shear loading, the steel exhibited cleavage fracture. For conditions near mode~II ductile fracture occurred. A transition from brittle to ductile fracture occurred for mixed mode loading. Finite element analysis provided estimates of the extent of near crack tip yielding and elastic-plastic stress intensity factors. Test results agreed with the maximum tensile stress (MTS) criterion for small scale yielding for limited amounts of shear loading. The load for mode II fracture was lower than predicted from the MTS criterion, but higher than predicted from plastic collapse predictions. Observed fracture angles where in broad agreement with the predicted fracture mechanisms. The load for the transition from brittle to ductile fracture was found to agree approximately with the predicted load. This revised version was published online in July 2006 with corrections to the Cover Date.     

A hybrid approach to determine fracture resistance for mode I and mixed‐mode I and II fracture specimens

This paper proposes a hybrid approach to determine the fracture resistance for mode I and mixed‐mode I and II fracture specimens, combining both numerically computed and experimentally measured load (P) versus load‐line displacement (LLD or Δ) relationships for metallic fracture specimens. The hybrid approach predicates on the same principle as the conventional, multiple‐specimen experimental method in determining the energy release rate. The hybrid method computes the P–Δ curves from multiple finite element (FE) models, each with a different crack depth. The experimental procedure measures the P–Δ curve from a standard fracture specimen with a growing crack. The intersections between the experimental P–Δ curve and the numerical P–Δ curves from multiple FE models dictate the LLD levels to compute the strain energy (U) using the area under the numerical P–Δ curves. This method provides accurate estimates of the J resistance data for both SE(B) specimen under mode I loading and single‐edge notched specimens under mixed‐mode I and II loading.