Structure and strength of a polyethylene pipe grade containing glass spheres and low-molar-mass linear polyethylene

The resistance to slow crack growth and to internal over-pressure of pipes based on a commercial polyethylene gas pipe grade (BPE; 0.6 mol% butyl branches and M?_W = 197,000 g/Mol) blended with both an injection molding grade linear polyethylene (LPE;M?_W = 42,000 g/mol) and 0.5 ± 0.1 mm glass spheres was studied. The blends and the pure polymer components were characterized by density measurements, differential scanning calorimetry, small-angle X-ray scattering, and transmission electron microscopy. The fracture properties of extruded pipes were measured using hydrostatic pressure testing and notched uniaxial testing on samples cut from the pipe wall. The polymer components were macroscopically uniformly blended and differential scanning calorimetry indicated the occurrence of partial co-crystallization between the branched and linear components. Transmission electron microscopy showed molar mass segregation on a 100 nm level. Notched uniaxial testing showed that the slow crack growth resistance of pure BPE was considerably higher than that of the LPE/BPE blend with 30% LPE. Fractography indicated that the fracture-initiating particles were larger in pipes failing after shorter period of time in the hydrostatic pressure testing. The lifetimes of hydrostatic pressure tested pipes based on the BPE grade containing glass spheres were similar to those of pipes based on the LPE/BPE blend with 30% LPE.     

Detection of divergences in polyethylene resins fabrication by means of the modified stepwise isothermal segregation technique

The selective crystallization behavior of a series of commercial medium- and high-density polyethylene resins has been studied by means of an original modified procedure of the stepwise isothermal segregation technique using differential scanning calorimetry. The technique consists of a sequenced multiple-stage stepwise thermal treatment of the materials allowing separation of the macromolecules with respect to their length-to-branching content and distribution. It is assumed that such a separation process gives an image of the proportion of specific crystallizable species, which are in turn responsible for slow crack growth resistance of the resins under study. A drift molecular parameter is calculated from a combination of the crystallization data at 119°C and 114°C. This molecular parameter is capable of revealing some divergences regarding the fabrication of a commercial polyethylene resin within a decade. Such divergences are well correlated with premature brittle failures under hydrostatic pressure testing of a series of correctly extruded pipes. Furthermore the drift molecular parameter allows a ranking of different medium- to high-density polyethylene resins—the lower this parameter the better the slow crack growth resistance of the materials. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 2103–2112, 1999     

Evaluation of the chemical resistance of high‐density polyethylene geomembranes

The chemical resistance of high‐density polyethylene geomembranes (GMs) with smooth and textured surfaces in notched and unnotched forms at different pH values and in the range of 20–80°C was examined with stress crack resistance testing. Surface microcracks in GMs were observed in scanning electron microscopy images. Smooth and textured GMs did not show significant differences in their mechanical behaviors. The yield strength decreased with the temperature, pH, and exposure time. The yield strain increased with the temperature, but there were no good correlations with pH values. The break strength also decreased with the temperature and showed no significant correlation with pH variations. The break strain did not show a good correlation with the temperature and pH variations. The stress crack resistance was independent of pH variations but significantly depended on the temperature. It was negatively correlated with the exposure time. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Interpretation of results of full notch creep test and comparison with notched pipe test

Abstract

An investigation of two tests commonly used to determine resistance to slow crack growth in PE pipes and materials is detailed, in order to gain a greater understanding of the mechanisms involved and to resolve differences in results observed. The full notch creep test (FNCT) is carried out on small notched bars machined from sheet or pipe loaded to create high constraint at the notch tip. The notched pipe test (NPT) is a pressure test on pipe containing external machined notches. In this test, it has been observed that the use of more flexible materials allows deformation in the crack tip region and contributes to slow crack growth resistance via crack tip blunting. Good pipe performance can be achieved by selecting materials with high inherent slow crack growth resistance or by combining inherent resistance with blunting mechanisms promoted by a lower density material. It is concluded that the FNCT test, while useful for an indication of inherent slow crack growth resistance, cannot be used to predict pipe performance for a range of materials, and therefore is unsuitable as a reference test for a pipe product specification. The NPT test remains the benchmark test for pipe performance and is referenced by many specifications.     

Toughness measurement on ball specimens. Part I: Theoretical analysis

A new toughness test for ball-shaped specimens is presented. In analogy to the “Surface Crack in Flexure”-method the fracture toughness is determined by making a semi-elliptical surface crack with a Knoop indenter into the surface of the specimen. In our case the specimen is a notched ball with an indent opposite to the notch. The recently developed “Notched Ball Test” produces a well defined and almost uniaxial stress field.The stress intensity factor of the crack in the notched ball is determined with FE methods in a parametric study in the practical range of the notch geometries, crack shapes and other parameters. The results correlate well with established calculations based on the Newman-Raju model.The new test is regarded as a component test for bearing balls and offers new possibilities for material selection and characterisation. An experimental evaluation on several ceramic materials will be presented in a consecutive paper.     

Experience with a full notch creep test in determining the stress crack performance of polyethylenes

A laboratory method to measure the stress crack resistance of polyethylenes was developed and has since been applied in our laboratory for more than twelve years. The experience gathered since our first paper is herewith reported. The creep rupture test of circumferentially notched specimens cut from plaques or pipes has proven to be a rapid and reliable method to evaluate the stress crack performance. Surfactant-assisted stress cracking was employed to accelerate testing. The stress crack resistance of several polyethylene samples was studied with respect to its dependence on stress, temperature, and environment. The creep rupture behavior at different temperatures could be superposed by horizontal shifting when the stresses were normalized in proportion to the respective bulk yield stresses. The notch tip radius turned out not to be very crucial, and variation of the nominal concentration of the surfactants, nonylphenolpolyglycolethers, scarcely affected slow crack growth. Acceleration of testing by surfactants equalized property differences to a noticeable extent but did not influence the ranking of the materials. The activation energy of crack growth was in the expected range. Defects introduced into the line by butt joint welding were precisely modeled by the full notch creep test.     

Biaxial Fracture Studies of a Glass-Ceramic

Uniaxial and equibiaxial tensile strengths are reported for glass-ceramic specimens exhibiting strength isotropy. Uniaxial strengths were determined in both 3- and 4-point bend tests. Stressing rate was a controlled variable and the tests were conducted in both dry N₂ and water environments, to provide data for different conditions of slow crack growth. There was little or no difference between strengths in the 3- and 4-point bend tests, indicating the absence of a size effect. In comparable tests, the strength under equibiaxial tension was greater than under uniaxial tension. The biaxial strengthening became less pronounced with increased slow crack growth during testing. A maximum observed biaxial-to-uniaxial strength ratio of 1.21 resulted from ball-on-ring and uniaxial bend tests in dry N₂. These results are attributed to differences in flaw severity between biaxial and uniaxial stressing. The decreasing strength ratios can be explained by a change in configuration of critical flaws due to slow crack growth. Numerical calculations, using a simplified two-dimensional model of the strength-controlling flaw, supported this hypothesis. The calculations also indicate that the slow crack growth exponent is smaller for the biaxial tension mode of stressing than for the uniaxial mode.     

Accelerated test for evaluating slow crack growth of polyethylene copolymers in igepal and air

The time for brittle failure by slow crack growth for 22 polyethylene copolymers was measured in Igepal and air. The notched tensile tests were conducted in Igepal and air at 50°C and 4.2 MPa and in air at 80°C and 2.4 MPa. For failure times less than 10³ min, the difference between the Igepal and air environments was not measurable. As the failure time increased beyond 10³ min, the ratio of failure in air compared to that in Igepal increased so that for the very highest failure times of 5 × 10⁵ to 108 min in air, the failure time in Igepal was reduced by 25—50 times. The correlation between the Igepal and air tests was generally good with respect to all types of polyethylene. However, a separation of the polyethylenes with respect to their comonomer, butene, hexene, or octene improved the correlation. The resistance to slow crack growth of all the current commercial polyethylene copolymers can be assessed by a notched tensile test in Igepal in about a week or less.     

Strain hardening modulus as a measure of environmental stress crack resistance of high density polyethylene

In this paper it is shown that the resistance to slow crack propagation in polyethylene can be predicted from a simple tensile measurement performed at 80 °C. It is shown that for different types of polyethylene homopolymers and copolymers the slope of a tensile curve above its natural draw ratio (i.e. strain hardening) correlates well with the measured stress crack resistance. The data presented in this paper confirm that the slow crack resistance in polyethylene is determined by the failure of the fibrils within the craze, which is shown to be determined by the strain hardening of a tensile curve. A material with a strong strain hardening will reduce the strain rate and consequently the time to failure will be strongly increased. Considering the fact that the slow crack resistance of polyethylene is usually assessed by tedious and time consuming testing methods performed on the notched samples in contact with specific fluids, the findings reported in this publication offer a possibility to assess the information on slow crack propagation in much simpler and faster way.     

Impact Modification and Fracture Mechanisms of Core–Shell Particle Reinforced Thermoplastic Protein

Mechanical properties and fracture mechanisms of Novatein thermoplastic protein and blends with core–shell particles (CSPs) have been examined. Novatein is brittle with low impact strength and energy‐to‐break. Epoxy‐modified CSPs increase notched and unnotched impact strength, tensile strain‐at‐break, and energy‐to‐break, while tensile strength and modulus decrease as CSP content increases. T_g increases slightly with increasing CSP content attributed to physical crosslinking. Changes to mechanical properties are related to the critical matrix ligament thickness and rate of loading. Novatein control samples display brittle fracture characterized by large‐scale crazing. At high CSP content a large plastic zone and a slow crack propagation zone in unnotched and tensile samples are observed suggesting increased energy absorption. Notched impact samples reach critical craze stresses easily regardless of CSP content reducing impact strength. It is concluded that the impact strength of thermoplastic protein can be modified in a similar manner to traditional thermoplastics.

     

Festigkeitsuntersuchungen and rißbehafteten Polyolefinen

The importance of fracture mechanics parameters are discussed in comparison with conventional failure criteria. As an example for conventional failure criteria the yield stress and elongation at fracture of unnotched and notched samples of polyethylene, polypropylene, and polybutene-1 are investigated as a function of strain rate and temperature. As suitable parameter describing the crack resistance of a material the fracture toughness values K_Ic and K_IQ are chosen and studied for polyethylene and polybutene-1 as a function of strain rate.     

Relationship between the material properties and fatigue crack‐growth characteristics of natural rubber filled with different carbon blacks

An investigation of the influence of different types of carbon black on fatigue crack‐growth behavior was undertaken. Fatigue tests were carried out on edge‐notched specimens under cyclic tension loading. A power‐law dependency between the crack‐growth rate and tearing energy was obtained. Natural rubber (NR) filled with N330 (the mean diameter is 30 nm) carbon black possessed the lowest values of exponent b and constant B (the two crack growth parameters determined from cyclic crack growth testing), which denoted the strongest resistance to crack growth at a given tearing energy. Strain‐induced crystallization was investigated by the modified Mooney–Rivlin equation and showed the earliest appearance and strongest ability of the crystallization of the NR/N330 composite at the largest amount of bound rubber. The study on the viscoelastic properties by dynamic mechanical analysis confirmed that the NR/N330 composite had the largest viscoelastic contribution, which was attributed to the viscoelastic dissipation in the viscoelastic region in front of the crack tip. All of these results confirm the best crack‐propagation resistance of NR filled with N330. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Preparation and characterization of perlite-filled high-density polyethylenes. III. Impact properties

Impact properties of perlite-filled high-density polyethylene (HDPE) composites were studied with the Charpy method by using both notched and unnotched samples. γ-Aminopropyltriethoxy silane (γ-APS, A-1100) was used as a silane coupling agent to improve the interfacial adhesion. The influences of the molecular parameters of HDPEs, molecular weight, degree of branching, degree of crystallinity, and also the effect of γ-APS on the impact properties are represented in this work. © 1995 John Wiley & Sons, Inc.     

Notched Fracture Behavior of an Oxide/Oxide Ceramic-Matrix Composite

The fracture behavior of an oxide/oxide ceramic-matrix composite, alumina/alumina-silica (Nextel610/AS), was investigated at 23° and 950°C using a single edge notched specimen geometry with clamped ends. Crack growth and damage progression were monitored during the tests using optical microscopy, ultrasonic C-scans, and crack mouth opening displacement. The net section strength of Nextel610/AS was less than the unnotched ultimate tensile strength. The failure mode was nonbrittle with considerable nonlinear deformation prior to and after the peak load at 23° and 950°C. The effect of temperature on the notched strength was significant. Net section failure stress decreased 50% when temperature was increased from 23° to 950°C. Observations of damage progression indicated that the reduction in notch strength with temperature was associated with self-similar crack growth at 950°C. Ultrasonic C-scans were found to be an effective method of monitoring damage progression. Ultrasonic attenuation ahead of the notch tip was correlated with surface matrix cracks and exposed fiber lengths on the fracture surface.     

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     

Evaluation of crack-Growth resistance curve for a particulate ceramic–Metal composite

A technique is described to evaluate the crack growth resistance behaviour in brittle ceramic-base materials. In this method, the crack increment measurements during the stable crack propagation process are not required. The crack growth resistance curves are studied for a particulate ceramic–metal composite in the system lanthanium chromite–chromium. Experiments were performed with standard fracture mechanics single-edge notched beam specimens in a temperature range from room temperature up to 1100°C. Effect of temperature on crack growth resistance behaviour is discussed.     

Lifetime prediction for ABS pipes subjected to combined pressure and deflection loading

As part of an investigation into the performance of acrylonitrile‐butadiene‐styrene (ABS) systems for water transportation, this paper presents a method for predicting the service lifetimes of buried pipes under in‐service loading conditions. A linear fracture mechanics approach was used to analyze brittle failure initiating from adventitious flaws located at the bore surface of pipe. Failure criteria were determined using the time‐dependent, quasistatic, plane strain fracture toughness of the ABS material, combined with empirical parameters that describe slow, steady crack growth. The expected operating conditions of a buried pipe were then separated into static loading contributions from internal pressure, diametrical deflection and residual stress. Idealized stress intensity factors associated with mode‐I crack opening under each of these components were determined using a finite element analysis and superposed to describe the general case in service. The computed nett stress intensity factor was then combined with the previously determined fracture toughness and slow crack growth data in an algorithm to simulate incremental radial crack growth from the pipe bore. Predicted failure times compared well with an experimental model of expected operating conditions, which combined hydrostatic pressure and parallel‐plate deflection loading of an internally notched pipe. The prediction method was also used to identify the factors that control the lifetime of a pipe in service. The influence of material visco‐elasticity was investigated by simulating variations in fracture toughness and slow crack growth resistance. It was proposed that, in practice, these variations are governed by opposing changes in visco‐elasticity. The effect of changing diametrical deflection and residual stress distribution were also simulated, allowing recommendations on pipe manufacture and installation conditions to be made.     

Phase segregation behavior in PE/DOP blends and glass‐transition temperatures of polyethylene

Phase segregation behavior in PEs/DOP blends, interactions between PEs and DOP, and glass‐relaxation transitions of PEs were investigated. FTIR, DSC, and TGA data demonstrated that molecular interactions were present between PEs and DOP. DMA data demonstrated that pure PEs each (except HDPE) exhibited two loss maxima at about ?20 and ?120°C but the PEs/DOP blends (including the HDPE/DOP blend) yielded one new loss maximum at about ?60°C. The glass‐relaxation transitions corresponding to the three loss maxima on the DMA curves were designated α (?20°C), β (?60°C), and γ (?120°C) transitions and were attributed to the relaxation of the amorphous phases in the interlamellar, interfibrillar, and interspherulitic regions, respectively, based on DMA, WAXD, SAXS, and POM measurements. The controversial T_g values of PEs and their origin were thus clarified in this study. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 3591–3601, 2001     

Zero stress aging in notched multi-component glass fibers

Degradation of glass under zero applied load in the presence of humidity at ambient temperature is of great interest to the container and fiber glass industries. The phenomenon is well documented for fused silica used in optical fibers, but has not been studied in detail for multi-component glasses. In this work notches of varying length (500-1500 nm) were placed with a focused ion beam into two types of multi-component glass fibers, E-glass (48 μm diameter) and soda-lime-silicate (35 μm diameter). Notched specimens were exposed to dry and humid conditions for up to 32 days. Transmission electron microscopy revealed the presence of extensive reaction products within the root of the notch, even after only 1 day of aging in the nominally dry environment for the soda-lime-silicate glass. Surprisingly, the extensive reactions have no measurable effect on the fiber strength. The uniaxial tensile strength of the notched glass fibers, measured with the fracture surface mirror radius method, does not follow a classic fracture mechanics prediction, implying that the notches are not classic Griffith flaws. Fracture mechanics is applied to show that sharpness at the notch base may be important, especially when subcritical crack growth is present during the strength measurement.     

酞侧基聚芳醚砜／聚苯硫醚共混物的断裂韧性

本文通过有缺口和无缺口冲击试验、断裂韧性测试以及结合扫描电镜分析断面形貌，研究了酞侧基聚芳醚砜／聚苯硫醚共混物的断裂行为，讨论了聚苯硫醚增韧聚芳醚砜的机理。结果表明，共混物冲击强度的改善主要是由于其裂纹引发能的提高；共混物断裂韧性提高的原因是由于外加应力场在ＰＰＳ微纤附近产生应力集中，促使基体和微纤都发生塑性形变，从而吸收更多的能量所致。