Effects of cyclic tensile loading on the rupture behavior of orthogonal 3-D woven SiC fiber/SiC matrix composites at elevated temperatures in air

This study examined the rupture mechanisms of an orthogonal 3D woven SiC fiber/BN interface/SiC matrix composite under combination of constant and cyclic tensile loading at elevated temperature in air. Monotonic tensile testing, constant tensile load testing, and tension–tension fatigue testing were conducted at 1100 °C. A rectangular waveform was used for fatigue testing to assess effects of unloading on the damage and failure behavior. Microscopic observation and single-fiber push-out tests were conducted to reveal the rupture mechanisms. Results show that both oxidative matrix crack propagation attributable to oxidation of the fiber–matrix interface and the decrease in the interfacial shear stress (IFSS) at the fiber–matrix interface significantly affect the lifetime of the SiC/SiC composites. A rupture strength degradation model was proposed using the combination of the oxidative matrix crack growth model and the IFSS degradation model. The prediction roughly agreed with the experimentally obtained results.     

Properties of Multilayered Interphases in SiC/SiC Chemical-Vapor-Infiltrated Composites with "Weak" and "Strong" Interfaces

The interfacial properties of SiC/SiC composites with interphases that consist of (C-SiC) sequences deposited on the fibers have been determined by single-fiber push-out tests. The matrix has been reinforced with either as-received or treated Nicalon fibers. The measured interfacial properties are correlated with the fiber-coatingbond strength and the number of interlayers. For the composites reinforced with as-received (weakly bonded) fibers, interfacial characteristics are extracted from the nonlinear portion of the stress-displacement curve by fitting Hsueh's push-out model. The interfacial characteristics are controlled by the carbon layer adjacent to the fiber. The resistance to interface crack growth and fiber sliding increases as the number of (C-SiC) sequences increases. For the composites reinforced with treated (strongly bonded) fibers, the push-out curves exhibit an uncommon upward curvature, which reflects different modes of interphase cracking and a contribution of fiber roughness.     

纤维增强树脂基复合材料界面粘结强度测试方法探讨

基体和增强材料界面的粘结性能直接影响到复合材料的力学性能，如何测量复合材料界面的粘结强度是界面研究的关键问题之一。本文侧重回顾了目前使用的复合材料界面粘结强度测试方法，如微脱粘、单纤维复合材料断裂、单纤维拔出和压出法，并对相关的计算理论进行了扼要介绍。     

Weak interface dominated high temperature fracture strength of carbon fiber reinforced mullite matrix composites

Weak fiber/matrix interface dominates the toughening properties of ceramic matrix composites. This paper reports a novel sol-gel fabricated carbon fiber reinforced mullite matrix composite, in which the fiber/matrix interface was inherently weak in shear properties (∼25 MPa), measured in-situ by fiber push-in tests. The interface microstructure was chemically sharp, characterized by transmission electron microscopy. The outcome of the weak interface was the full trigger of the toughening mechanisms like crack deflection, etc., leading to significant enhancement of the fracture toughness of the composite (∼12 MPa√m), measured by single edged notch beam method. Finally, due to the weak fiber/matrix interface and large thermal expansion mismatch of the fiber and matrix, the high temperature fracture strength was enhanced in the temperature range from 25 to 1200 °C, which is attributed to the enhancement of the interfacial property at elevated temperatures that favors better load transfers between composite constituents.     

Effect of Interface Roughness on Fiber Push-Out Stress

A theoretical analysis is given for single-fiber push-out with a rough interface whose asperity amplitude can be expressed by a Fourier series that has a good convergence. Based on a three-cylinder model for the single-fiber push-out test, the solutions of the fiber frictional push-out stress and the relative displacement of the fiber to the matrix at the fiber-matrix interface are obtained. A new asperity wear model is introduced in the analysis to simulate the degradation of the asperity amplitude during the fiber push-out process. The interfacial roughness between the fiber and the matrix is found to have a pronounced influence on the fiber sliding behavior.     

The properties of dry-spun carbon nanotube fibers and their interfacial shear strength in an epoxy composite

Continuous fibers composed of carbon nanotubes have been adopted as reinforcements for polymeric composites. This paper presents several fundamental studies relevant to the mechanical behavior of CNT fibers, including fiber tensile behavior; in situ SEM observation of fiber deformation mechanisms; and fiber modulus, ultimate strength and fracture strain measurements. A modified Weibull strength distribution model that takes into account the flaw density variation with fiber diameter has been adopted for the statistical strength analysis. The interfacial shear strength between the carbon nanotube fiber and the epoxy matrix has been measured using fragmentation tests of single-fiber composites.     

Oxidation and Temperature Effects on the Interfacial Shear Strength in SCS-6 Fiber-Reinforced Reaction-Bonded Silicon Nitride

The fiber/matrix interfacial shear strength of Textron SCS-6 SiC-fiber-reinforced reaction-bonded Si₃N₄ (RBSN) was studied as a function of temperature after oxidation for 24 h at 600°C. Fiber push-out experiments were conducted using a diamond indenter in a high-temperature micro-hardness tester under vacuum. The interfacial shear strength increased with temperature because of the relief of residual tensile stresses arising from the difference in thermal expansion coefficients between the fiber and the matrix. Most of sublayer 2 of the fiber outer coating, which mainly consisted of carbon in the form of BSU (basic structure unit) aggregates, had disappeared after the heat treatment of the composite. Oxidation resulted in severe changes in the fiber outer coating and caused a lower interfacial shear strength with respect to that of the unoxidized composite.     

Statistically sound application of fiber push-out method for the study of locally non-uniform interfacial properties of SiC-SiC fiber composites

Push-out tests were performed on SiC-SiC fiber composites with single- and multi-layered pyrolytic carbon fiber-matrix interphases. It is shown that experimental scatter is significant and a large number of tests is necessary in order to obtain statistically relevant values of interfacial shear strength. A difference between the regions of an individual fiber tow is observed, linked to local porosity. Interfacial debonding occurs along the boundary between the fiber and the first carbon layer, regardless of the structure of the interphase, and therefore interfacial shear strength is not directly linked to the structure of the interphase.     

The Effect of Nitric Acid Oxidization Treatment on the Interface of Carbon Fiber-Reinforced Thermoplastic Polystyrene Composite

The quality of interfacial interaction is dictated by the surface chemistry of the carbon fibers and the composition of the matrix. The composition of polystyrene was modified by the addition of maleic anhydride (MAH) grafted polystyrene. The surface properties of the various matrix formulations were characterised by contact angle. Carbon fibers were modified by oxidation in nitric acid. The surface composition of the carbon fibers was characterized. The interaction between modified polystyrene and the carbon fibers was studied by single fiber pull-out tests. The best adhesion behavior was achieved between polystyrene containing grafted MAH and nitric acid oxidation carbon fibers. The addition of MAH-grafted polystyrene to the unmodified polystyrene caused the interfacial shear strength to increase. The apparent interfacial shear strength of this fiber-matrix combination allowed for the utilisation of 100% of the yield tensile strength of polystyrene.     

Carbon fiber-reinforced (YMAS) glass-ceramic matrix composites. III. Interfacial aspects

Unidirectional continuous carbon fiber-reinforced glass-ceramic matrix composites have been fabricated for dry sliding applications. Different fracture behaviors have been observed (three-point bend test and fracture surfaces observation). Besides, the distance between next microcracks, which have appeared in the matrix on cooling after hot-pressing of the composites, changes with the sintering temperature, suggesting fiber–matrix reactions. The nature of the fiber–matrix interface is observed in Transmission Electronic Microscopy and the interfacial shear stress is determined by push-in tests. ©     

Mechanical properties and interfacial characteristics of 2.5D SiNOf/BN wave-transparent composites

2.5D SiNO_f/BN wave-transparent composites were fabricated by borazine infiltration and pyrolysis route at 800 °C?1400 °C. The fracture behavior of the composites was investigated on the basis of the retained fiber strength, in-situ fiber and matrix mechanical properties, and fiber/matrix bonding strength. Nano-indentation were employed to determine the in-situ elastic modulus and hardness of the fiber and BN matrix, and single-fiber push-out experiments were performed to quantify the fiber/matrix bonding strength. The interfacial characteristics of the 800 °C?1200 °C fabricated composites were further studied in terms of physical bonding and chemical reaction. Physical bonding was resulted from thermal mismatch between the fiber and matrix, which induced compressive radial stress at the interface. The radial stress increased continuously with increasing fabrication temperature. Meanwhile, the TEM analysis confirmed chemical diffusion at the fiber/matrix interface, which further improved the interfacial bonding strength. The chemical reaction mechanism was proposed.     

Compressive strength of three-dimensionally reinforced carbon/carbon composite

Compressive behavior of three-dimensionally reinforced carbon/carbon composite (3D-C/C) was examined from room temperature to elevated temperatures up to about 3000 K. Three-dimensionally reinforced C/C was found to have an inclination to induce kinks at the ends of specimens due to extremely low shear strength. In order to avoid this type of premature fracture and to conduct high-temperature tests, discussion was made on specimen geometry and testing procedure, and the combination of a dumbbell-shape specimen and test configuration without a supporting jig were found to be suitable for the present study. Using this set-up, the compressive strength of a 3D-C/C was evaluated as a function of temperature up to about 3000 K. The compressive strength of the 3D-C/C monotonically increased with the increase in temperature up to 2300 K, but decreased above this temperature. The strength enhancement was suggested to be caused by improvement in the fiber/matrix interfacial bonding, and the degradation over 2300 K was by softening of the matrix at high temperatures.     

Measuring Interphase Recession by Fiber Push-In Testing

A novel technique for measuring interphase recession in ceramic-matrix composites (CMCs) due to oxidation is described. The technique involves fiber push-in testing and analysis of the load–displacement curves. Fiber push-in tests were conducted on carbon-coated Hi-Nicalon SiC fibers in a CVI SiC matrix, where the carbon interphase had recessed due to oxidation. Estimates of interphase recession distances from analysis of fiber push-in tests are in reasonable agreement with measurements made by optical microscopy. Besides measuring the recession distance, the fiber push-in test can be used to investigate environmental effects on fiber bridging.     

Utilizing Vacuum Bagging Process to Prepare Carbon Fiber/CNT-Modified-epoxy Composites with Improved Mechanical Properties

In this work, the effects of carbon nanotube-modified epoxy and carbon nanotube-enriched sizing agent on the tensile properties and failure mode of unidirectional carbon fiber/epoxy composites were investigated. Laminates of carbon fiber/epoxy composites at different concentrations of carbon nanotube and sizing agent were fabricated by hand layup vacuum bagging process. Scanning electron microscopy analysis was conducted to unveil the relation between the macroproperties and the composites’ microstructure. Experimental results showed that the carbon nanotube-modified epoxy/carbon fiber composite showed 20% enhancements in the Young’s modulus compared to the pristine epoxy/carbon fiber composite. The scanning electron microscopy analysis of the fracture surfaces revealed that incorporating carbon nanotube into the epoxy matrix with utilizing the vacuum improves the interfacial bonding and minimizes the voids that act as crack initiators. This microstructure enhances the interfacial shear strength and load transfer between the matrix and the fabrics and consequently the tensile characteristics of the formulated composite.     

Sharp indentation behavior of carbon/carbon composites and varieties of carbon

Sharp indentation tests on carbon fiber and carbon matrix composites (C/C composite) were carried out over a wide load range from 0 to 2 N on three different cross sections: normal, parallel and inclined to the fiber axis. For comparison purposes, a variety of carbons including HOPG, glassy C, and pyrocarbon films was also examined. Both the fibers and the matrices displayed first a purely elastic response and second crack-induced damage. A purely elastic behavior was also observed with most of the varieties of carbon considered. Young’s modulus was extracted from the indentation curves either at maximum or at various forces, using the Sneddon equation of elastic response on loading (elastic indentation) or a classical equation based on elastic recovery on unloading (elastoplastic indentation). Results are discussed with respect to features of structure and heterogeneity of material in the stressed volume.     

The effects of surface treatments of fibers on the interfacial properties in single-fiber composites

The interfacial properties between fibers and the matrix contribute to the overall properties in high performance composites. Plasma treatments (Ar, O₂, CF₄/O₂, N₂/H₂) have been performed on carbon fibers to improve the fiber-matrix interaction. The treatment efficiency was checked by the single-fiber technique, while the surface chemistry and morphology were characterized by X-ray photoelectron spectroscopy (XPS), static secondary ion mass spectroscopy (SSIMS), and scanning electron microscopy (SEM). The O₂- and N₂/H₂-plasma treatments proved most effective both for introducing oxygen-containing functionalities at the fiber surface and for improving the interfacial shear strength of carbon fiber/epoxy composites. A relationship between the oxygen concentration at the fiber surface and the interfacial shear strength is demonstrated.     

Raman spectroscopy study of high-modulus carbon fibres: effect of plasma-treatment on the interfacial properties of single-fibre-epoxy composites: Part II: Characterisation of the fibre-matrix interface

High-modulus carbon fibres from different precursors were submitted to an oxygen plasma-treatment under similar conditions. Single-fibre epoxy composites were prepared from them, and fragmentation tests were performed in order to characterise fibre-matrix interfacial adhesion. Raman spectroscopy has been used in the present work to map the strain along the fibre during tensile loading of the matrix. The strain distributions obtained agreed well with the prediction of analytical models used conventionally to describe load transfer at interfaces. Interfacial shear stress distributions were then obtained from these distributions according to the conventional force-balance concept. The interfacial shear strength (IFSS) and frictional shear stress (τ_f) values were calculated to quantify the degree of fibre-matrix adhesion. It was found that both parameters increased dramatically after the surface treatment, confirming the ability of cold plasma oxidation to improve the adhesion of carbon fibre to epoxy matrices. A dependence of the IFSS on the degree of surface order, as given by the structural order parameter I_D/(I_D+I_G), calculated from the relative intensities of the D and G bands of Raman spectra, was found. This supports the role played by the graphitic structure in fibre-matrix adhesion.     

Adhesion characteristics of oxygen plasma-treated rayon fibers

The effect of oxygen plasma treatment of fiber on the adhesion between regenerated cellulose fiber and polyethylene (PE) was investigated using the single-fiber fragmentation test. In addition to allowing the determination of the interfacial shear strength, the fragmentation test provided a great deal of useful information on shear stress transfer and failure mechanisms in the systems. It was found that oxygen plasma treatment considerably enhanced the interfacial adhesion, as established by both the shear strength values that were measured and the birefringence patterns observed. The influence of the duration of treatment on adhesion was studied and found to be a very important parameter. The roles of surface chemistry, surface energetics, and surface topography of fiber in the interaction balance were investigated using electron spectroscopy for chemical analysis (ESCA), contact angle measurements, and scanning electron microscopy (SEM). It was seen that neither the plasma-induced changes in the surface energetics nor those in the surface topography could have exerted a positive effect on adhesion. Instead, the improved adhesion was ascribed to covalent bonds formed between the fiber and the matrix, as hydroperoxides, which were created on the fiber surface by the plasma treatment, decomposed during the fabrication of single-fiber specimens.     

Fiber bundle push-out test and image-based finite element simulation for 3D carbon/carbon composites

The interfacial properties such as debond strength, fracture energy release rate in Mode-II and coefficient of friction play important roles in determining the mechanical properties and strength of carbon/carbon (C/C) composites. Push-out tests were conducted on 3D C/C composites and the experimental results were fitted to the shear lag model to determine these interfacial properties. X-ray tomography was used to explore the internal material structure of the composite. The fiber bundle and matrix interfaces were observed as being partially damaged in the tomographic images and the crack network was explored in detail. The tomographic images were also used to reconstruct a finite element (FE) mesh for simulating push-out tests. The interface of the fiber bundle and matrix in the FE mesh was represented by cohesive surfaces with frictional contact. The cohesive surface properties were obtained by matching FE results with the experimental results. The simulations had a good agreement with experiments and values of 0.75 for coefficient of friction, 2–5 N/mm² for debond stress, 1–4 N/mm² for clamping stress and 3–6 N/m for fracture energy release rate were obtained as interfacial parameters for the composite.     

Test methods for bond strength of glass fiber posts to dentin: A review

ABSTRACT

In this paper, a review of the test methods for bond strength of glass fiber posts to dentin is presented. The main variables that influence the bond strength tests are related to substrate, to specimen properties, specimen preparation, and test methodology. The impact of these variables on the test outcome is analyzed. The search was performed on studies published between 2007 and 2015. Most of the tests carried out, in the literature, were the push-out (75%), pull-out (13%), and microtensile (11.9%) tests, showing an inversion compared to the results found in studies published between 2005 and 2010, when push-out test was used in a proportion of 2% and microtensile test in a proportion of 67%. The push-out test emerged as a practical tool for evaluating the interfacial shear strength between fiber post and root canal walls.