Interphase characterization in polymer composites - monitoring of interphasial behavior in dependence on the mode of loading

Single fiber model composites consisting of epoxy resin matrix and differently sized glass fibers were investigated using pull-out tests, scanning electron microscopy (SEM), scanning force microscopy (SFM) and single fiber dynamic load test (SFDL). The inhomogeneous stress distribution along the embedded fiber length could be visualized by monitoring. SEM images showed either cohesive fracture or adhesive failure on pulled-out fibers with different sizings. The crack initiation and propagation were detected randomly and multiply distributed as the inhomogeneous interphase itself and depending strongly on the fiber-matrix model combination. The meniscus region acts as a material inhomogeneity and its appearence depends on the surface free energies of fiber and matrix and on the curing conditions of the resin. SFM in force modulation mode has visualized different interphase thicknesses and gradients of local stiffness. The SFDL test has been shown as a worthful tool for the comprehensive determination of fiber-matrix interaction.     

Crack propagation in amorphous polymers and their composites

The fracture energy of a polymer depends strongly on the viscoelastic responses of the material, and therefore is a function of temperature and crack velocity. The toughness of a composite is determined by the way in which the reinforcing filler modifies the energy dissipating mechanisms of the polymeric matrix.

The fracture toughness of a variety of polymeric glasses and their composites with glass beads, glass fibers, and rubber particles was measured. The velocity of rapidly moving cracks and the crack propagation rates under controlled loading conditions were also measured.

It was found that the crack propagation velocities in unfilled and glass bead filled materials were controlled by the longitudinal stress waves in the matrix and that the only effects of the glass beads were to blunt the crack tip and limit the viscous deformation. The effect on fracture toughness was relatively small and either positive or negative, depending on which of the above two factors dominated.

The presence of rubber particles as a second phase lowered terminal crack propagation velocities and greatly increased the fracture toughness, indicating a crack retarding effect of the rubber particles. This is related to the induction of crazes in the matrix by the rubber phase.

Glass fibers had a tendency to bridge the tip of a propagating crack, thereby greatly increasing the fracture toughness. In this case the work of fracture comes from a combination of the elastic strain energy stored in the fibers, the energy dissipated in debonding the fibers from the matrix, and the fracture energy of the matrix itself.     

Simulation of fracture behavior of unidirectional SiC/SiC composite exposed in air at 823–1673 K

It is known that SiC/SiC composite has high strength and toughness, but is degraded when exposed in air at high temperatures due to the propagation of the crack made by the premature fracture of the SiO₂ layer. It is also known that the fracture morphology of this composite varies from fiber pull-out type to non pull-out type with progressing oxidation. The present work aimed to describe such a behavior with a computer-aided Monte Carlo shear lag simulation method. The experimentally measured variation of strength of the unidirectional composite as a function of thickness of the SiO₂ layer and also as a function of exposure time and temperature, and the experimentally observed variation of fracture morphology with progressing oxidation, could be reproduced satisfactorily by this method.     

Unstable Fracture Behavior of Rubber Toughened Poly(Styrene-co-Acrylonitrile)

A linear elastic fracture mechanics (LEFM) approach was used to study fracture characteristics of ABS materials. The effects of crack (ligament) length and rubber content on the microscopic deformations taking place at the front of crack tip and in the bulk of the specimens were investigated. The results of fractography studies showed that, in addition to rubber content, the microscopic deformations are influenced by crack length. For some materials this manifests itself as a change in macroscopic response. The ligament length dependent behavior was increased for the samples with higher rubber contents. The results also showed that, although the elastic behavior with unstable crack growth is the dominant micromechanism of deformation, stable crack propagation still occurred in some compositions. All the fracture parameters, including fracture toughness, fracture energy, plastic zone size, and crack tip opening, increased with rubber content. The changes in microscopic and, as a consequence, in the macroscopic deformation behavior of a given specimen with ligament length were attributed to changes in yield stress of the sample and maximum stress on the ligament.     

Dislocation-crack interaction

In this paper, recent developments in the understanding of the dislocation-crack interaction and its relationship to the phenomena of crack tip deformation and fracture toughness are reviewed. An enhanced research activity in this area began with successful observations of the behavior of crack tip dislocations by various techniques, namely etch pits technique, X-ray topography and transmision electron microscopy. The advantages and limitations of these techniques are compared and the information obtained from these experiments are discussed. The results show that dislocations are emitted from a crack tip when the applied stress is sufficiently high. During crack propagation, dislocations are also generated from other bulk sources and the number of these dislocations relative to those from the crack tip may be an important parameter. The elastic theory of the interaction between dislocations and a crack is presented by considering the force on the dislocations. The theory is applied to derive a dislocation emission condition, which may be expressed in terms of a critical stress intensity factor. It is concluded that the dislocations emitted from a crack tip are repelled from the crack tip and this repulsive interaction is responsible for the formation of a dislocation-free zone. These dislocations shield the crack tip from the applied stress and hence contribute to an increase in the fracture toughness. The physical origin of the dislocation-free zone lies in the presence of a barrier to dislocation emission from the crack tip. One of the barriers to dislocation emission is the image stress. With the dislocation-free zone, the crack tip can maintain a finite stress intensity factor following crack tip deformation. The lattice theories of dislocation-crack interaction indicate that the results are consistent with those of the continuum theory.     

Caustics method in dynamic fracture problem of orthotropic materials

Caustics method is a powerful optical technique in fracture mechanics because of its high sensitivity to stress gradients. In this paper, it is applied to resolve dynamic fracture problems in orthotropic composites. Considering most orthotropic materials are opaque, reflective caustics method is derived here by combining the fundamental principle of caustics method with the mechanical properties of orthotropic materials. Meanwhile, corresponding experiments are carried out for typical glass fiber-reinforced composites, where mode I and mixed-mode fracture states are taken into account. By recording and analyzing shadow spot patterns during the crack propagation process carefully, crack onset time, dynamic fracture toughness and crack growth velocity of orthotropic composite are determined. These results will be useful to evaluate the dynamic fracture properties of composites and further to optimize their designs.     

In situ observation of interfacial debonding process induced by matrix crack propagation in two-dimensional unidirectional model composites

Interfacial debonding behavior is studied for unidirectional fiber reinforced composites from both experimental and analytical viewpoints. A new type of two-dimensional unidirectional model composite is prepared using 10 boron fibers and transparent epoxy resin with two levels of interfacial strength. In situ observation of the internal mesoscopic fracture process is carried out using the single edge notched specimen under static loading. The matrix crack propagation, the interfacial debonding growth and the interaction between them are directly observed in detail. As a result, the interfacial debonding is clearly accelerated in specimens with weakly bonded fibers in comparison with those with strongly bonded fibers. Secondary, three-dimensional finite element analysis is carried out in order to reproduce the interfacial debonding behavior. The experimentally observed relation between the mesoscopic fracture process and the applied load is given as the boundary condition. We successfully evaluate the mode II interfacial debonding toughness and the effect of interfacial frictional shear stress on the apparent mode II energy release rate separately by employing the present model composite in combination with the finite element analysis. The true mode II interfacial debonding toughness for weaker interface is about 0.4 times as high as that for a stronger interface. The effect of the interfacial frictional shear stress on the apparent mode II energy release rate for the weak interface is about 0.07 times as high as that for the strong interface. The interfacial frictional shear stress and the coefficient of friction for weak interface are calculated as 0.25 and 0.4 times as high as those for strong interface, respectively.     

Characterization of the fracture toughness of micro-sized tungsten single crystal notched specimens

Fracture experiments using micrometer-sized notched cantilevers were conducted to investigate the possibility of determining fracture mechanical parameters for the semi-brittle material tungsten. The experiments were also used to improve the understanding of semi-brittle fracture processes for which single crystalline tungsten serves as a model material. Due to the large plastic zone in relation to the micrometer sample size, linear elastic fracture mechanics is inapplicable and elastic-plastic fracture mechanics has to be applied. Conditional fracture toughness values J _Q were calculated from corrected force vs. displacement diagrams. Crack growth was accessible by direct observation of in-situ experiments as well as with the help of unloading compliances. As a further tool, fracture toughness can be determined via crack tip opening displacement. The micro samples behave more ductile and exhibit higher fracture toughness values compared to macro-sized single crystals and fail by stable crack propagation.     

Interfacial adhesion between semi-crystalline polymers (polypropylene and nylon-6): in situ compatibilized interface and fracture mechanism

The interfacial fracture toughness between semi-crystalline polymers (polyamide/polypropylene) were studied to understand the failure mechanisms at the interface, especially when the interface was reinforced by an in situ compatibilizer. Based on the observation of the interface using scanning electron microscopy and wide angle X-ray spectroscopy, it was revealed that crystalline structure of polypropylene was not affected by the in situ compatibilizer at the interface. The reinforcing mechanism could be qualitatively identified by investigating the evolution of fracture toughness as a function of annealing time and temperature. The adhesion strength increased with the annealing time. Depending on the annealing temperature, the fracture toughness passed a peak value and then reached a plateau after some bonding time. As long as the chain length of the compatibilizer is long enough to form entanglements with the molecules at both bulk sides, the fracture at the interface is decided by the balance between adhesion strength at the interface and cohesive strength in the weak modulus side; the failure locus follows the lower one. Thus, adhesive failure occurred first when the reaction at the interface did not occur long enough to provide high adhesive strength at the interface, but the cohesive failure occurred in the crack propagation side after the adhesive strength value became higher than the cohesive strength value.     

Statistical Aspects of Tensile Fracture of Isotactic Polypropylene

The fracture behavior of isotactic polypropylene (iPP) specimen with double-notched shape under a fixed elongation speed at room temperature is described. Over 100 tensile tests were performed, and the statistic fracture data were obtained for the tensile condition. The statistical data of fracture were obtained by examining the time to fracture, the ultimate stress, and the tensile toughness (determined from the area under the nominal stress–strain curve from the origin to the fracture point). The probability density distributions for time to fracture, the ultimate stress, and the tensile toughness approximately followed the normal Gaussian statistics. Using a linear relationship between stress and elongation time near the fracture point, we can apply a static Kalman filter system to the present fracture data to determine a conditional probability density function. As a consequence, this application makes it possible to predict the probability of fracture of iPP under any static condition.     

Atomistic scale fracture behaviours in hierarchically nanotwinned metals

In the present study, a series of large-scale molecular dynamics simulations have been performed to investigate the atomistic scale fracture behaviours along the boundaries of primary twins in Cu with hierarchically nanotwinned structures (HTS), and compare their fracture behaviours with those in monolithic twins. The results indicate that crack propagation along [1?1?2] on the twin plane in monolithic nanotwins is brittle cleavage and fracture, resulting in low crack resistance and fracture toughness. However, the crack resistance along the boundaries of primary twins in HTS is much higher, and a smaller spacing of secondary twins (λ ₂) leads to even higher fracture toughness. With large λ ₂, the crack growth is achieved by void nucleation, growth and coalescence. However, considerable plastic deformation and enhanced fracture toughness in HTS could be achieved by the crack blunting and by the extensive dislocation accommodation ahead of the crack tip when λ ₂ is small.     

Mechanical properties of flat braided composite with flexible interphase

Textile composites have been used extensively as industrial materials because of the excellent mechanical properties resulting from the continuously oriented fiber bundle. In a study of the mechanical properties, it is important to consider the fiber/matrix interface property as for other composite materials. In a recent study, the fiber/matrix interface is regarded as an interphase that has its own material constants and thickness; consequently, the mechanical properties of a composite can be controlled by specifically designing the interphase. In this study, we applied this concept to braided composites with flexible resin as interphase for the purpose of designing the interphase. In a static tensile test, though there were no improvements in Noncut specimens (normal braided composites), but a Cut specimen (each side of the Noncut specimen was cut) with flexible interphase was improved in fracture load and displacement. The observation of the specimen edge was carried out and it was confirmed that the progress of debonding at the fiber bundle intersection was interrupted by a flexible interphase, and a matrix crack did not occur in the Cut specimen with flexible interphase. In a fiber bundle pull-out test, it was confirmed that debonding progressed not into the fiber/resin interface but into the flexible interphase in the specimen with flexible interphase, and the interfacial property at the fiber bundle intersection was improved.     

PBX材料宏细观断裂行为的数字散斑相关法实验研究

 采用半圆盘弯曲实验和数字散斑相关方法,对高聚物粘结炸药（PBX）的宏、细观断裂行为进行了实验研究。宏观上,带有预制裂纹的半圆盘试样发生拉伸破坏,利用数字散斑相关技术得到了试样的应变场和位移矢量场分布,定量分析了试样全场的变形特征,并测得了PBX材料的平面应变断裂韧性;细观上,用配有加载装置的扫描电子显微镜对含预制裂纹的半圆盘试样间接拉伸下的损伤演化和破坏过程进行了实时原位观察,借助于数字散斑相关方法,定量分析了试样损伤局部化特征。结果表明,将数字散斑相关方法用于研究PBX材料宏、细观尺度上的变形破坏问题是有效的。     

Impact toughness of EK-181 ferritic-martensitic chromium (12%) steel under loading by concentrated bending

The low-temperature fracture of a high-temperature low-activated ferritic-martensitic EK-181 chromium (12%) steel (RUSFER-EK-181: Fe-12Cr-2W-V-Ta-B) is studied using impact and static concentrated bending tests as a function of the specimen dimensions (standard, small), the type of stress concentrator (V-shaped notch, fatigue crack), and the temperature (from −196 to +100°C). The ductile-brittle transition temperature falls in the range from −85 to +35°C. The temperature dependences of stress-intensity factor K _Ic and fracture toughness J _Ic are determined. The severest type of impact toughness tests is represented by tests of V-notched specimens with an additional fatigue crack and two lateral V-shaped notches (three-sided V-shaped notch with a central fatigue crack). The fracture energy of the steel depends on the type of stress concentrator and the specimen dimensions and is determined by the elastic energy and the plastic deformation conditions in the near-surface layers of a specimen, which are controlled by the lateral notches. At the same test temperature, the impact toughness and the fracture toughness are interrelated. Irrespective of the type of specimen (including notches and a fatigue crack), the ferritic-martensitic steel exhibits the same fracture mechanism.     

Predicting Interfacial Strengthening Behaviour of Particulate-Reinforced MMC — A Micro-mechanistic Approach

The fracture properties of particulate-reinforced metal matrix composites (MMCs) are influenced by several factors, such as particle size, inter-particle spacing and volume fraction of the reinforcement. In addition, complex microstructural mechanisms, such as precipitation hardening induced by heat treatment processing, affect the fracture toughness of MMCs. Precipitates that are formed at the particle/matrix interface region, lead to improvement of the interfacial strength, and hence enhancement of the macroscopic strength properties of the composite material. In this paper, a micro-mechanics model, based on thermodynamics principles, is proposed to determine the fracture strength of the interface at a segregated state in MMCs. This model uses energy considerations to express the fracture toughness of the interface in terms of interfacial critical strain energy release rate and elastic modulus. The interfacial fracture toughness is further expressed as a function of the macroscopic fracture toughness and mechanical properties of the composite, using a toughening mechanism model based on crack deflection and interface cracking. Mechanical testing is also performed to obtain macroscopic data, such as the fracture strength, elastic modulus and fracture toughness of the composite, which are used as input to the model. Based on the experimental data and the analysis, the interfacial strength is determined for SiC particle-reinforced aluminium matrix composites subjected to different heat treatment processing conditions.     

Effects of reactive gas on shear and fracture behaviors of plasma-treated polyethylene/steel joints

For this study, we investigated the effects of reactive gases (oxygen, nitrogen, and argon) on the shear behavior and fracture toughness of HDPE/steel joints by treating high-density polyethylene (HDPE) with plasma using a microwave method. We also investigated the effect of plasma treatment on the physical and chemical changes on the surface of HDPE. HDPE/steel joints were fabricated using a secondary bonding process. The results showed that the shear strength and fracture toughness of HDPE/steel joints treated with different reactive gases were ordered as follows, oxygen > nitrogen > argon. Specifically, the shear strength and fracture toughness of oxygen plasma-treated HDPE/steel joints were approximately 7600% and 2400% greater, respectively, than that of untreated HDPE/steel joints. The improvements in shear strength and fracture toughness are attributed to increase in surface roughness and the creation of carbonyl functional groups on the HDPE surface via plasma treatment.     

Effect of surface treatment for steel adherends on static and fatigue crack growth of epoxy adhesives

The fracture toughness of unmodified, glass-bead-reinforced and CNBR-modified epoxy adhesives under mode I loading is not improved by acid surface treatment of steel adherends since cohesive failure always occurs for all adhesives with or without acid surface treatment. On the other hand, the fatigue crack growth resistance greatly increases due to acid surface treatment of steel adherends. Especially, the threshold dramatically increases. The crack grows cohesively at all stages of crack velocity for DCB specimens treated with acids while it grows at the interface between the adherend and the adhesive layer for the specimens whose polished surface of adherends is only decreased with solvent. An optical microscope observation revealed that adherend surfaces treated with acids were rougher than ones without acid treatment, although XPS examination for the surfaces did not show significant difference in their chemical elements among the specimens with and without acid treatment.     

Effect of sizing agent on interfacial properties of aramid knitted structural composites

Tensile tests have been carried out on aramid knitted fabrics/epoxy resin composites in which the aramid knitted fabrics are treated with different sizing agents. Two kinds of surface treatment are performed; one uses an epoxy sizing agent and the other uses a polyethylene sizing agent. Tensile modulus and strength of epoxy-sized composites are higher than those of polyethylene-sized composites. The fracture process is different between epoxy- and polyethylene-sized materials. This difference in fracture process is caused by the different interphase made from either epoxy or polyethylene sizing treatments, resulting in the different tensile performance. Moreover, the tensile properties of the wale specimen are more affected than those of the course specimen by the interphase.     

Crack growth on the basal plane in single crystal zinc: experiments and computations

Crack propagation on the basal planes in zinc was examined by means of in situ fracture testing of pre-cracked single crystals, with specific attention paid to the fracture mechanism. During quasistatic loading, crack propagation occurred in short bursts of dynamic crack extension followed by periods of arrests, the latter accompanied by plastic deformation and blunting of the crack-tip. In situ observations confirmed nucleation and propagation of microcracks on parallel basal planes and plastic deformation and failure of the linking ligaments. Pre-existing twins in the crack path serve as potent crack arrestors. The crystallographic orientation of the crack growth direction on the basal plane was found to influence both the fracture load as well as the deformation at the crack-tip, producing fracture surfaces of noticeably different appearances. Finite element analysis incorporating crystal plasticity was used to identify dominant slip systems and the stress distribution around the crack-tip in plane stress and plane strain. The computational results are helpful in rationalizing the experimental observations including the mechanism of crack propagation, the orientation dependence of crack-tip plasticity and the fracture surface morphology.     

Fracture of ceramics and glasses

The rich variety of fracture behavior exhibited by glasses and ceramic materials is reviewed with particular emphasis on the understanding gained through the use of deliberately introduced, controlled cracks. After a brief summary of the mechanics of indentation cracks four major topics are discussed, the structure of crack tips, environment assisted crack growth, high temperature fracture and the toughening of ceramics. Resolution of the sharp vs blunt crack dilemma is presented together with recent microscopy observations of crack tips in brittle solids. In describing fracture in polycrystalline ceramics we explore some of the complexities beyond the simple Griffith behavior relating strength to flaw size, and show how the scale of the microstructure with respect to the crack length affects the observed toughness. It is shown that the interaction of a crack with the microstructure provides a unifying theme for interpreting much of the current work in the literature and leads to important concepts discussed here, such as the discrete-continuum transition, R-curve behavior, toughening due to crack deflection and crack bridging, transformation toughening and stress-induced microcrack toughening.