Stability of crack propagation in epoxy resins

The propagation of cracks in epoxy resins has been studied using a linear elastic fracture mechanics approach and a double torsion testing geometry. Under constant crosshead displacement rate conditions cracks are found to propagate in an unstable ‘stick-slip’ manner at high temperatures and with low rates of testing whereas at lower temperatures and using higher rates of loading propagation is more stable and cracks propagate in a continuous manner. The presence of liquid water tends to cause a transition from stable to unstable propagation at room temperature. The influence of specimen geometry upon crack stability is also discussed.     

The effect of microstructure on the slow crack growth resistance in polyethylene resins

The slow crack growth (SCG) in high density polyethylene (HDPE) is a phenomenon dominated by crazing. In this work, the crazing was analyzed from a microstructural point of view. PENT (Pennsylvania Edge Notched Tensile) test was chosen to study the evolution of the craze with time for different resins from PE‐80 up to PE‐100 grades. Two different geometries, the standard and an alternative named CDNT (Circumferentially Deep Notched Tensile), were employed. Failure times were correlated with intercrystalline parameters like tie molecules and the molecular weight between entanglements. Experimental results showed good correlations using both direct SCG test (standard PENT and CDNT geometries). Finally, the strain hardening modulus was correlated with PENT failure times. The results disclosed an outstanding correlation for several polyethylene grades from blow molding up to PE‐80, PE‐100, and higher resistant to crack grades. These results permitted an easy‐classifying and ranking method as much to the old polyethylene grades as to the new generation of HDPE resins with a very high SCG resistance. POLYM. ENG. SCI., 55:1018–1023, 2015. © 2014 Society of Plastics Engineers     

Curing studies on modified epoxy and unsaturated polyester resins

Experimental studies were carried out on the curing behavior of unsaturated polyester and epoxy resins. The latter were modified with three different fillers (CaCO₃, CaSiO₃, and glass powder) and their curing behaviors studied. Polyesters exhibited faster cure rates than the epoxy resins. The gel time of the epoxy resins decreased with the addition of fillers. Data indicated that the peak exotherm of these thermosetting resins increased when filled with glass powder. The hardness of the curing mass increased with curing time. The use of gel-hardness number as a quality control parameter has been suggested.     

Mechanics of crack growth in epoxide resins

Experiments have been conducted employing tapereddouble-cantilever-beam joints with different epoxide adhesives. Depending on the adhesive employed, crack propagation occurred either (a) in a continuous stable manner with crack propagation velocities in the range 10^?4 to 5 m/s and values of the adhesive fracture energy, G_Ic, being almost independent of the crack velocity, or (b) intermittently in an unstable manner when the initial crack velocity was never less than about 20 m/s and, in some instances, rose to about 450 m/s; values of G_Ic (initiation) increased rapidly with increasing velocity. It is proposed that the amount of localized plastic deformation arising from shear yielding that occurs at the crack tip prior to crack propagation is controlling. Secondly, the longterm strength of stressed, structural adhesive joints has been investigated. The fracture of these joints over eight decades of time is uniquely described by a critical plastic zone size developed at the crack tip at failure.     

Thermomechanical and morphological properties of epoxy resins modified with functionalized hyperbranched polyester

Thermomechanical and morphological properties of blends of epoxy monomers and hydroxyl and epoxy functionalized hyperbranched polyesters have been studied. Different properties of the blends were found by changing the cure cycles (a precure step followed by a postcure at higher temperature). All the blends showed phase separation with a particulate morphology. Through the addition of the hydroxyl‐ended modifiers, rather than the epoxy‐ended, an increase of the viscosity and of the reactivity of the uncured blends was obtained. The blends containing the epoxy functionalized polymer showed some liquid–liquid transitions in the rheological traces, probably because of the phase separation phenomena. POLYM. ENG. SCI., 46:1502–1511, 2006. © 2006 Society of Plastics Engineers     

High temperature slow crack growth in polyoxymethylene

Brittle failure has been observed in polyoxymethylene during long‐term low‐level tensile loading at elevated temperatures. It is argued to be associated with slow crack growth via the breakdown of the localized planar fibrillar damage zones that form under these conditions. This phenomenon has been characterized using notched compact tension specimens tested under various static loads and at different temperatures. The specimen lifetime at a given load is found to decrease strongly with increasing temperature and to increase with molar mass at a given load and temperature. The associated crack‐tip fibrillar damage zones are shown to arise from the breakdown of more localized microfibrillar deformation zones, which in turn result from interlamellar cavitation in the early stages of tensile deformation.     

The effect of the morphology on the hygroelastic behaviour of polyester and epoxy resins

The effect of the morphology on the hygroelastic behaviour of polyester and epoxy resins is studied. The morphology is expressed by two factors, namely, the free volume of the polymer and a two-phase formation. The first factor is varied in styrene-crosslinked polyester using different styrene/alkyd proportions, and by using different immersion temperatures. The second is investigated in polyesters by replacing styrene with bromostyrene inducing a two-phase structure, and in epoxies by changing the hardener/epoxy ratio. It is shown that the hygroelastic response is affected markedly by the morphology. In general, both the moisture content and its rate of absorption are higher when the polymer network is more open and when more free volume is available. In some cases, however, the hygroelastic parameters are dominated by a two-phase structure where present.     

Fracture and mechanical properties of epoxy resins and rubber-modified epoxy resins

Fracture and mechanical property data on a wide range of epoxy resin systems are presented. The extent to which toughening can be induced by heterophase rubber inclusions depends more on the curing agent used than on the resin component. The greatest improvements in toughness were obtained by rubber modification of epoxy resins cured with an anhydride. A preformed ABS polymer can be used to toughen many epoxy resin systems. With one major exception (where a large improvement was found) only small changes in tensile properties occur when small amounts of rubber are present.     

Statistical analysis of slow crack growth experiments

A common approach for the determination of slow crack growth (SCG) parameters are the static and dynamic loading method. Since materials with small Weibull module show a large variability in strength, a correct statistical analysis of the data is indispensable. In this work we propose the use of the Maximum Likelihood Method and a Baysian Analysis, which, in contrast to the standard procedures, take into account that failure strengths are Weibull distributed. The analysis provides estimates for the SCG parameters, the Weibull module, and the corresponding confidence intervals and overcomes the necessity of manual differentiation between inert and fatigue strength data. We compare the methods to a Least Squares approach, which can be considered the standard procedure. The results for dynamic loading data from the glass sealing of MEMS devices show that the assumptions inherent to the standard approach lead to significantly different estimates.     

Polyether and polyester polyol based glycidyl-terminated polyurethane modified epoxy resins: Mechanical properties and morphology

A glycidyl-terminated polyurethane prepolymer was synthesized and used to enhance the properties of epoxy resins. Some properties of glycidyl-terminated PU/epoxy with polyether based (PPG) and polyester based (PBA) glycidyl-terminated PU were investigated in this research. The polyether based glycidyl-terminated PU(PPG) modified epoxy resin proved to be superior to conventional epoxy resins in improved impact strength and fracture energy, but not tensile strength, tensile modulus, flexural strength and flexural modulus. On the other hand, the polyester based glycidyl-terminated PU(PBA) modified epoxy resin had increased mechanical properties while showing slight variation of impact strength and fracture energy. Different mechanisms for this behaviour are advanced in this paper.     

The anisotropy of slow crack growth in polyethylene pipes

Slow crack growth was measured in the perpendicular and parallel directions relative to the extrusion direction of the pipe. For five pipes from different manufacturers, the anisotropy factor, the lifetime to fracture in the perpendicular direction divided by lifetime in the parallel direction, varied from 1.2 to 4.7 for complete fracture and 1.4 to 4.0 for crack initiation. The degree of molecular orientation was determined by measuring the shrinkage that occured when a pipe specimen was heated near its melting point. The amount of shrinkage correlated with the anisotropy factor for slow crack growth. The shape change after shrinkage was related to the flow pattern of the resin during extrusion and the cooling rate after extrusion.     

管材树脂耐慢速裂纹增长性能快速评价方法

介绍了评价管材料耐慢速裂纹增长性能的3种实验方法:管材切口实验、全切口蠕变实验和宾夕法尼亚州切口实验的研究进展情况,并对3种方法进行深入分析和对比,可为管材料的研究和性能评价提供参考.     

Oxidation effects on toughness and slow crack growth in polycrystalline graphites

The fracture toughness (K_Ic) and slow crack growth behavior of four fine-grained polycrystalline graphites, oxidized to 5, 10 and 20% weight losses, were measured in air at room temperature. Exponential decreases in the elastic moduli as well as decreases in the fracture surface energy contributed to lowering K_Ic. Oxidation generally shifted the stress intensity-crack velocity (K_I-V_I) diagram to lower stress intensity values, and decreased the slope, or N-value. Scanning electron microscope fractography revealed that a combination of filler particle and binder phase degradation with increasing oxidation was responsible for the decreased toughness and changes in the (K_I-V_I) characteristics. Oxidation conditions were shown to significantly affect the magnitude of decreases in the physical, elastic and mechanical properties of these graphites.     

Measurement of thermal conductivity of epoxy resins during cure

This work reports the development of a methodology for the measurement of thermal conductivity of thermosetting polymers during their cure. The study addresses the reliability and robustness of the method through FEA modeling and testing using a noncuring material with known thermal conductivity. The thermal conductivity and its evolution during the cure has been measured for three widely used aerospace epoxy resins, namely, RTM6, 890RTM, and the XU3508/XB3473 system as function of cure temperature. A constitutive model expressing the dependence of thermal conductivity on the degree of cure and temperature has been established. The device developed here can measure thermal conductivity of epoxy resin with accuracy up to 3%. © 2018 The Authors. Journal of Applied Polymer Science published by Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47015.     

A sensitive mechanical test for slow crack growth in polyethylene

Slow crack growth (SCG) in a wide variety of polyethylenes has been investigated by a constant tensile load test (the PENT test) for a single edge notched specimen. The PENT test is very sensitive to the changes in molecular structure and morphology of polyethylene. The resistance to SCG depends on the density of the tie molecules and the strength of the crystals.     

Analysis of volumetric changes of unsaturated polyester resins during curing

Two models were proposed to predict the volume changes that occur during the cure of unsaturated polyester resin/styrene systems. These models are able to account for both thermal expansions/contractions and polymerization shrinkage during processing. One model, which is based on coversion, was developed by combining experimental results from differential scanning calorimetry and dilatometry. The second model is based on radical concentration, and was developed using results from electron spin resonance spectroscopy and dilatometry. Predictions obtained from both models were compared with experimental results and reasonable agreement was obtained.     

Nodular structure in epoxy resins

Nodular morphology is observed on free surfaces, fracture surfaces, and etched surfaces of epoxy resins of widely different cure and chemistry. The influence of high- and low-energy substrates on nodule size is illustrated. Fine structure or “dimples” exist on several individual nodules, and various states of agglomeration of nodules are depicted. The possible relations between nodular morphology and adhesion phenomena are discussed.     

An alternative approach to the evaluation of the slow crack growth resistance of polyethylene resins used for water pipe extrusion

High-density polyethylene (HDPE) pipes have been largely employed in water and gas distribution systems. In spite of offering significative advantages over other materials, HDPE pipes suffer from premature failures due to creep fracture. The current industrial criterium for design and sizing of HDPE pipes is discussed. The concept of ‘regression curve,’ i.e. of a time-to-failure criterium based in long-term-hydrostatic strength (LTHS) tests, is criticised and concluded to be unsatisfactory for this purpose. An alternative approach is suggested, which is based on shorter-term tests. This is illustrated by testing five HDPE resins designed for pipe extrusion and comparing with their standard ‘regression curves’. The obtained results are consistent with the ‘regression curve’-based analysis, justifying the use of the alternative approach in the industry.     

Assessment of residual stresses during cure and cooling of epoxy resins

A new stress monitoring technique, a stress-tracking device, is described here. It has been used to study some important properties of epoxy resin. Residual stresses, including a curing shrinkage stress and a cooling shrinkage stress, were measured automatically and continuously during curing and cooling. Simultaneously, information such as an apparent gelation time and glass transition temperature were obtained directly during the experiment. These epoxy resin properties were related to the extent of cure. Varying cure temperature produced changes of cure behavior, which resulted in different residual stresses.