Solvent-induced crack growth in rubbery block polymers

The rapid cracking of lightly stressed rubbery block polymers of styrene and isoprene in certain liquids and vapors has been examined experimentally, by using model test pieces containing a single crack. Solvents which preferentially dissolve the rigid molecular end blocks rather than the rubbery center blocks are efficient cracking agents. The stress required for crack growth to occur is shown to be in accord with a simple energy criterion: the stored elastic energy must be sufficient to provide a characteristic energy for the newly formed surface. This characteristic energy ranges from values close to the surface energy of simple liquids up to about 100 times this value for thicker test pieces or slowly diffusing vapors, when some tearing of an incompletely swollen core is inferred. “Induction times,” before the initial crack starts to grow, are shown to be due to a progressive increase in stored energy under a constant stress as the material absorbs solvent and softens until the critical energy criterion is met. Thus, a timedependent fracture process is shown to be in accord with a constant energy criterion. Above the critical condition the rate of crack growth depends strongly upon stress, like tearing of amorphous elastomers, and the crack then accelerates rapidly.     

Experimental and theoretical investigation of stress corrosion crack (SCC) growth of polyethylene pipes

Degradation of polymers is usually manifested in a reduction of molecular weight, increase of crystallinity in semicrystalline polymers, increase of material density, a subtle increase in yield strength, and a dramatic reduction in toughness. Stress corrosion cracking (SCC) results from strongly coupled thermo-mechano-chemical processes, and is sensitive to material composition and morphology. The individual crack propagation stage is critical in determining the lifetime of pipe. Based on author's previous works, crack layer (CL) theory model is adopted in this study to describe the individual stress corrosion (SC) crack propagation kinetics and the time interval from crack initiation to instability and break through. The effect of localized chemical degradation at the crack tip on SC crack growth kinetics is addressed. Typical SC crack growth is presented and discussed as a step-wise manner based on the proposed model. In addition, scanning electron microscopy (SEM) observation and Fourier transform Infrared spectroscopy (FTIR) analysis of failed samples obtained by accelerated SCC tests are applied to validate the proposed model. SEM is useful to identify the change of fracture mechanisms from chemically driven crack to mechanically driven crack by the formation of visible striations. FTIR analysis enables tracking of the accumulation of chemical degradation by detecting the amount of carbonyls on the crack surface. Carbonyl index is defined to compare the amount of chemical degradation quantitatively. The purpose of this paper is to continue to develop the technical theory and understanding behind SCC phenomena to facilitate all polymer pipe industries and in particular the polyethylene pipe industry to design better resins and piping systems.     

Effects of humidity on environmental stress cracking behavior in poly(methyl methacrylate)

Environmental stress cracking (ESC) in poly(methyl methacrylate) under different humidity conditions has been investigated. Constant stress‐intensity factor (K) ring‐type specimens were prepared, and all specimens were equilibrated at five different humidity conditions for about two years. ESC tests were carried out under the same humidity as specimens had been stored. Acoustic emission (AE) signals during ESC tests were also measured to examine the crack‐growth behavior. The threshold K value (K_th) tended to increase with increasing humidity. At a relative humidity (RH) of 11%, crack growth occurred gradually until 40 ks under a K value of 0.70 MPam^1/2, and then the crack‐growth rate began to increase and AE events were observed. A laser microscopic observation indicated that the crack extended by the coalescence between a main crack and a microcrack ahead of the main crack tip. AE signals generated are considered to be associated with the coalescence. At 98% RH, an incubation period where no crack growth was observed existed under a K value of 0.94 MPam^1/2, but the crack began to grow suddenly after that incubation period. This suggests that the craze at the crack tip may become weaker with increasing loading time under high humidity. Although the crack‐growth rate at 98% RH was higher than that at 11% RH, no AE events were observed. This suggests that the crack extended stably in the craze at a crack tip, and sorbed water may make the craze growth easy. All the results suggest that two different ESC mechanisms are activated depending on sorbed water that are varied by humidity. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 40: 1–9, 2002     

Detection of SCC of 304 NG stainless steel in an acidic NaCl solution using electrochemical noise based on chaos and wavelet analysis

The stress corrosion crack (SCC) of 304 nuclear grade (NG) stainless steel (SS) in 0.5 mol/L NaCl+1.5 mol/L H₂SO₄ was monitored using electrochemical noise (EN) based on chaos theory, statistics and wavelet analysis. The results indicated that the SCC process was divided into three stages according to the transient features in the EN. In the beginning, compared with the sample without applied stress, the enhanced fluctuation amplitude in the electrochemical current noise (ECN) of the stressed samples was attributed to stress-enhanced pitting corrosion and uniform corrosion; then the fluctuations of ECN for all the samples decreased due to a coverage by the corrosion products; however, the ECN fluctuations of stressed sample were larger than the unstressed sample, suggesting that the stress enhanced the SCC initiation and propagation. Chaos analysis revealed that the correlation dimensions increase from 2.1 to 2.5 during the corrosion process, and the applied stress seems increase the complexity and uncertainty of the ECN signal.     

Crack growth in a pipe grade PVC material under static and cyclic loading conditions

The creep crack growth (CCG) and the fatigue crack growth (FCG) behavior of a commercial pipe grade PVC material was studied based on a linear elastic fracture mechanics (LEFM) methodology. The FCG tests were performed under sinusoidal load control at a frequency of 5 Hz and at R-ratios (F_min/F_max) of 0.1, 0.3 and 0.5; the test temperatures were 23°C and 60°C. The creep crack growth behavior (corresponding to R = 1) was studied at a test temperature of 60°C. The results of the FCG tests revealed that fatigue crack propagation is primarily controlled by the cyclic component of the crack tip stress field rather than by the mean stress level. Comparing FCG and CCG data in terms of K_Imax and K_I, respectively, also confirmed the deteriorating effect of the fatigue loading on the crack growth resistance. Fracture surface investigations for both fatigue and static loading were performed to gain insight into the micromechanisms of crack advance.     

Characterization of the Orientation Parameters Around Crack Tips in Unfilled and Nanofilled Poly(propylene) Using in-situ Synchrotron Small and Wide Angle Scanning Scattering Techniques

The fracturing behavior of polymers and polymeric composites is of great interest in the scientific and application community. Especially in the case of silicate-layered nanocomposites the influence of fillers on the fracturing behavior is still fairly unclear. Fractures of semicrystalline polymers are accompanied by various processes of which shearing and cavitations are the most common ones. Nanocomposite deformation due to the delamination of fillers seems to be the most practical way leading to fractures with relatively low strains. With the method of scanning small angle X-ray scattering (SAXS) and wide angle X-ray diffraction (WAXD) it is possible to combine information on the structural details with the position on the sample, with the actual position resolution of the investigation being defined by the size of the X-ray beam used to scan the sample. By means of the application of synchrotron radiation it is nowadays possible to adjust the actual beam size to the dimensions of the region of interest, which is why it is an adequate tool for studying the deformation region near a crack tip. In a native polypropylene sample, the fracturing process was accompanied by shear yielding as well as lamellae fragmentation and reorienting. In the highly deformed material near the crack tip fibrillated material could be found. However, in the polymeric nanocomposites (PNC) shearing, lamellae fragmentation, and fibrillation were hindered by the filler due to which the material did not have so much freedom to dissipate energy and fractures occurred much earlier. In this paper the comparison of a PNC and its native polymer is to provide an overview of the different deformation mechanism and the structural details around the crack tip.     

Crack propagation behavior in rubber materials

Within the linear viscoelastic theory, crack tip fields are calculated at various crack tip velocities. A transition from rubbery to glassy material behavior in the vicinity of the crack tip can be observed. Shear and bulk behavior is analyzed separately. Whereas the increase of tearing energy at higher crack tip velocities can be ascribed to the shear behavior, bulk behavior influences the fracture mechanism. The results support experimental investigations that the instability separating stable from unstable crack propagation is related to a change in the fracture mechanism. At low crack tip velocities, material separation is the result of formation, growth, and coalescence of cavities. At high crack tip velocities, cavitation is suppressed and fracture is driven by a rather brittle mechanism resulting in a decreased amount of energy to propagate the fracture process zone. Published in Russian in Vysokomolekulyarnye Soedineniya, Ser. A, 2008, Vol. 50, No. 5, pp. 882–891. This article was submitted by the authors in English.     

Mechanism of fracture in glassy polymers. III. Direct observation of the craze ahead of the propagating crack in poly(methyl methacrylate) and polystyrene

Observation of optical interference fringes at the tip of a crack in a glassy polymer allows the construction of the configurations of the crack tip and the craze that precedes it. The craze extends 25 μ beyond the crack tip in poly(methyl methacrylate) and 550 μ beyond the tip in the polystyrene studied. The craze at the crack tip in PMMA may be seen to deform elastically as much as 100% under stress before crack propagation recommences. Such deformation is estimated to account for as much as 40% of the nominal Griffith energy of crack propagation.     

Radiation produced traps in crystalline ice

Using the pulse radiolysis method it is found that electron traps are produced in a low temperature crystal of ice by electron irradiation. The optical absorbance per pulse due to the trapped electron is increased by the repeated bombardment of multiple pulses on the same crystal at 106°K, under the condition that trapped electrons produced by the preceding pulses are completely photobleached before the observation pulse. The produced trap disappears on annealing the sample at temperatures below 140°K.     

应变速率和电位对应力腐蚀裂纹扩展的影响

以滑移-溶解-再钝化模型为基础,推导出应力腐蚀裂纹扩展速率与裂尖应变速率和电位之间的理论公式.计算表明,在裂纹扩展速率与裂尖应变速率的关系曲线中有两个特征区域.裂纹扩展速率在区域I随裂尖应变速率增加而增大,而在区域II不随裂尖应变速率的改变而变化.用慢应变速率拉伸技术（SSRT）测量了304L不锈钢的裂纹增长速率.当电位控制在区域II的阳极区时,理论计算的裂纹扩展速率与实验得到的结果比较吻合.     

Characterisation of the thermo-oxidative degradation of polyethylene pipes by chromatographical,rheological and thermo-analytical methods

In this work the influence of three different stabiliser systems on the stress rupture behaviour of high density polyethylene (PE-HD) pipes under constant internal pressure was examined at 60 and 80°C with special consideration of the quasi-brittle failure by growth of a single crack in the failure regime preceding the global chemical degradation of the pipes. It could be proven that the pipes of the three formulations did not show global molecular and morphological differences in this failure regime and that the stabilisation was still intact. Therefore, the differences in failure times observed for the three formulations are believed to be a result of local ageing around the crack tip related to the combined influence of time, the elevated temperature, the presence of oxygen and water, and the high mechanical stresses in the immediate crack tip region.     

Interferenzoptische Untersuchungen zur Bruchausbreitung unter Wechsellast in PMMA

Zusammenfassung In einem amorphen, transparenten Thermoplasten wurde an einem unter Ermüdungsbelastung sich ausbreitenden Riß das Verhalten des Craze an der Rißspitze untersucht. Dazu wurde eine spezielle Apparatur gebaut, mit der an Miniatur-CT-Proben Ermüdungsbelastungen bis zu 30 N bei Frequenzen bis zu 250 Hz aufgebracht werden können. Der besondere experimentelle Aufbau erlaubt die gleichzeitige Messung der Bruchgeschwindigkeit, der jeweils an der Probe wirkenden Last und des mikroskopischen Interferenzstreifensystems des Craze für jeden beliebigen Zeitpunkt eines Belastungszyklusses.An hochmolekularem PMMA wurden Bruchzähigkeit und Craze-Länge als Funktionen von Bruchgeschwindigkeit und Rißfortschrittsrate in einem weiten Frequenzbereich gemessen.Mit Hilfe des Dugdale-Modells, das die Craze-Zone an der Rißspitze beschreibt, konnte eine neue, charakteristische Materialeigenschaft abgeleitet werden: die Lebensdauer (Zahl der Belastungszyklen) einer Fibrille im Craze als Funktion der lokal am Craze wirkenden Spannung.

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Summary For a propagating crack under cyclic loading conditions the behaviour of the craze at the crack tip in an amorphous transparent polymer has been investigated. A special apparatus has been built to apply a cyclic load up to 30 N at a frequency up to 250 Hz on the cracked sample. The experimental set-up allows the simultaneous measurement of the crack speed, the instantaneous load on the sample and the microscopic interference pattern of the craze at any moment of the cycle.Fracture toughness and craze length as functions of crack speed and fatigue crack growth rate have been measured on PMMA in a wide frequency range.By means of the Dugdale model describing the craze shape at the crack tip, a particular material property could be derived: the lifetime (number of loading cycles) of a fibril in the craze as a function of the local stress applied on the craze.

     

Environmental Stress Cracking of Polymers Monitored by Fatigue Crack Growth Experiments

This article describes fatigue crack growth experiments to investigate the degradation of the durability of polymers due to fluid environments. The degrading effect of media causing stress cracking can be observed on the fracture surfaces of tested samples by scanning electron microscopy. Strategies to improve environmental stress cracking like changes in molecular weight, orientation, toughening with rubber particles of different sizes are discussed. Fatigue crack growth experiments can be employed as a very fast and effective screening method.     

Effect of Fiber Volume Fraction on the Flexural Properties of Unidirectional Carbon Fiber/Epoxy Composites

In this study, the effect of fiber content on the flexural property of continuous carbon fiber/epoxy composites was investigated. Samples with four different fiber volume fractions, 50, 60, 70, and 80 vol.%, were fabricated. For comparisons, cast epoxy resin was also prepared. It was observed that the flexural strength and modulus of this material are enhanced with increasing fiber volume fractions in the range of 50–70 vol.%. Results show that the carbon fiber/epoxy composites possess the largest fracture force and displacement when the fiber volume fraction is 70 vol.%, which is mainly attributed to the effective stress transfer of fibers. This can restrict crack tip propagation and blunt the crack tip, then consume abundant deformation energy and result in an increase of fracture work. On the other hand, poor flexural property was observed when the sample with high fiber volume fraction (80 vol.%) was tested. Three different types of failure modes were observed according to the fiber content.     

Monte Carlo model of the temperature rise at a GaAs surface under an electron beam

Scanning electron microscopy (SEM) has frequently been used to study semiconductor materials. It offers the possibility of obtaining reliable qualitative and quantitative information on relevant local material parameters. The temperature rise due to electron‐beam bombardment can influence some semiconductor parameters, which then will influence the SEM information. In this work we propose a model calculation based on the Monte Carlo (MC) method to calculate the temperature rise due to electron‐beam heating. The results show that the temperature rise increases with increasing numbers of electrons (electron‐beam current), and the inverse behavior is observed with respect to the electron energy (electron‐beam voltage). The decrease in temperature rise with depth is also obtained. Copyright © 2006 John Wiley & Sons, Ltd.     

Environmental stress cracking of low-density polyethylene in normal alcohols

Fracture mechanics was used to investigate the environmental stress cracking of low-density polyethylene with 4.0 melt flow index. Annealed samples were prepared; a single edge notch was made and then the samples were fractured under constant load in four different liquid alcohols. The relation between the stress intensity factor K and the crack speed a˙ has been investigated. The log a˙ vs. logK curves are influenced not only by temperature but also by the alcohol used as the environment. This influence has been studied in detail. The conclusions are as follows: the crack speed at high K is determined by the diffusion mechanism, and this mechanism cannot be explained in terms of hydrodynamics but can be explained in terms of thermally activated molecular motion. On the other hand, the crack speed at low K is strongly related to the plasticization and the stress relaxation of the crack tip material.     

Fracture surface of polystyrene: Mackerel pattern

Characteristic markings of concentric bands are formed on the fracture surface of tensile specimens under certain loading conditions. The marking form in the fast crack growth region of the mirror area of fracture. Optical and electron optical microscope techniques have been used to study the morphology of the markings. It is shown that in this region the crack propagates along the interface between the craze, in which the crack nucleated, and the bulk material. The mackerel pattern is caused by the crack jumping from one craze–matrix interface to the other.     

Fracto-emission from neat epoxy resin

Fracto-emission is the emission of particles (e.g. electrons, photons, ions, neutral species) due to crack growth in materials. These emissions can be related to a number of fracture related phenomena including microcracking, crack speed of dynamic crack growth, locus of fracture (in filled materials), and potentially the extent of crack branching. Here, we examine the emission of electrons, positive ions, and photons during and following the fracture of a neat epoxy resin subjected to tensile and tensile impact loading in vacuum. Experiments which detect correlations of crack tip position and emission intensity show that the emissions occur during and following fracture. We also illustrate that observed variations of the fracture surface morphology under different loading conditions correlated with characteristics of the photon and charged particle emission. For example, regions of the surface exhibiting the highest degree of surface roughness resulted in more intense emission.     

Mechanisms and micromechanics of fatigue crack propagation in glassy thermoplastics

An iterative approach is used to estimate, from interference optics measurements, the variation of refractive index and, hence, extension ratio along the length of a craze at the tip of a fatigue crack. The finite element method is used to compute craze surface stress distributions which are found to be similar to those obtained for static loading. High extension ratios, in the range 6 to 8 for retarded fatigue crack growth in poly(vinylchloride), are attained in the craze fibrils at the crack tip before crack jump occurs. The craze thickens primarily by surface drawing during the early stages of its growth but in the later stages the fibril creep mechanism predominates. The critical fibril extension ratio is not reached in a single cycle, as in normal fatigue crack propagation, and crack jump does not occur until, typically, after several hundreds of cycles during which the fibrils accumulate considerable damage.Presented in part at the 7th Int. Conference Deformation, Yield and Fracture of Polymers, Cambridge, UK, 11–14 April 1988.     

Experimental approach for microscale mechanical characterization of polymeric structured materials obtained by additive manufacturing

In this paper, an original experimental method is developed for local strain characterization at the surface of additively manufactured polymeric materials. The process used herein is material extrusion. This experimental method is based on the use of microscopic speckle pattern deposited at the surface of micro single edge notched specimen (μ_SENT) made of acrylonitrile butadiene styrene (ABS). Two configurations of filament orientation were used for the specimen manufacturing. Images of the μ_SENT specimen surface were recorded during in-situ tensile test. The quantitative analysis of images was made by digital image correlation (DIC). The evolutions of the local strain heterogeneities and the crack tip are evidenced on the kinematic fields. It is shown that the crack propagates in the low resistance path which is the interface area between filaments. It is also evidenced that the intersection of perpendicular filaments in two adjacent layers blocks crack growth. The local strain evolutions at the surface of the specimen are compared to the macroscopic response of the material. The method developed herein allows the determination of the materials mechanical properties. The identification of the crack tip location using digital image correlation (DIC) and J-integral calculation lead to plot the J-R curve. The J-R curves comparison of the two specimen configurations shows that the fracture toughness is directly related to the material structure.