See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/254114061 The Effects of Loading History and Manufacturing Methods on the Mechanical Behavior of High-Density Polyethylene Article in Journal of Elastomers and Plastics · September 2011 DOI: 10.1177/0095244311404181 CITATIONS READS 13 373 2 authors, including: Bulent Aydemir The Scientific & Technological Research Council of Turkey 108 PUBLICATIONS 378 CITATIONS SEE PROFILE Some of the authors of this publication are also working on these related projects: Force and Force Measurements View project Design and development of road lighting fixtures with LED for M1 and M2 lighting class roads View project All content following this page was uploaded by Necmi Düşünceli on 12 May 2016. The user has requested enhancement of the downloaded file. The Effects of Loading History and Manufacturing Methods on the Mechanical Behavior of High-Density Polyethylene NECMI DUSUNCELI* Department of Mechanical Engineering, Aksaray University, Aksaray 68100, Turkey BULENT AYDEMIR The Scientific and Technological Research Council of Turkey (TUBITAK), National Metrology Institute, Kocaeli 41470, Turkey ABSTRACT: This article describes a series of experiments conducted to determine the effects of loading history and manufacturing techniques on mechanical behavior of high- density polyethylene (HDPE). The main reason for undertaking the research was to investigate multiple creep, multiple relaxation, and cyclic loading on uniaxial tension. The samples used for tensile tests were obtained from extruded pipe and compression-molded sheets. The stress–strain responses of both samples under uniaxial tensile were found to be independent of the loading history. It was observed that the compression-molded specimens exhibit greater deformation ratio than the extruded specimen. Understanding the deformation behavior under different loading can offer the designer of highdensity polyethylene products reliable data relevant to practical applications. KEY WORDS: high-density polyethylene, loading history, mechanical properties, creep, relaxation, manufacturing techniques. *Author to whom correspondence should be addressed. E-mail: dusunceli@gmail.com JOURNAL OF ELASTOMERS AND PLASTICS Vol. 43–September 2011 0095-2443/11/05 0451–18 $10.00/0 DOI: 10.1177/0095244311404181 ß The Author(s), 2011. Reprints and permissions: http://www.sagepub.co.uk/journalsPermissions.nav 451 452 N. DUSUNCELI AND B. AYDEMIR INTRODUCTION been replacing metallic materials in many engineering applications such as load-bearing components and applications involving the use of high-explosive materials and expected to perform as reliably as the components that they replace. Polymers present a very complex nonlinear behavior depending on external factors and structural parameters and are classified by taking into account three basic characteristics that greatly influence the processing and end-use properties. These characteristics are density, molecular weight, and molecular weight distribution. High-performance thermoplastics such as high- density polyethylene (HDPE) are semi-crystalline polymeric materials having a microstructure that has both crystalline and amorphous regions. HDPE has a ratio of up to 90% crystallinity; however, low-density polyethylene has a ratio of up to 40% crystallinity. Thus, it can be seen that the greater the crystalline regions, the higher the density of polymeric materials and this affects a number of physical and mechanical properties of HDPE. Generally, increasing degree of crystallinity results in greater yield strength and stiffness. The mechanical behavior of HDPE is viscoelastic, and because of its semi-crystalline composition, it is very complex, being directly related to time and temperature. The crystalline region that accounts for the elastic response to forces is stiff; the amorphous region accounting for the viscous fluid-like response is soft. If polymeric materials are subjected to a constant load, initially they undergo a rapid deformation and then the deformation continues at a slower rate until eventually the material ruptures. This deformation is named viscoelastic creep and this may occur even at room temperature and under modest stress level below the yield point of polymeric materials. Relaxation can be defined as a change in the stress level with time when the strain is held constant. Relaxation is one of the most basic techniques to determine viscoelastic behavior. Initially, stress relaxation occurs rapidly, then gradually decreases, and after some time, the stress level reaches equilibrium [1–4]. Structural components to be subjected to severe loading conditions must be reliable. Hence, performance analysis needs to be carried out prior to production. The first step in this process is inelastic analysis, which provides information about stresses and strains during manufacturing and lifetime. For the inelastic analysis and lifetime predictions of engineering components, both experimental results and constitutive models are needed to estimate the deformation behavior of these P OLYMERIC MATERIALS HAVE Effects on the Mechanical Behavior of HDPE 453 materials as accurately as possible. In order to develop an experimentalbased constitutive model, the mechanical response of polymer needs to be investigated under different loading conditions, such as uniaxial and multiaxial, monotonic and cyclic, and single and multiple loadings. HDPE is a widely used raw material in the manufacture of pipes. Even though there are large numbers of experimental and analytical investigations on HDPE, few have examined the effects of manufacturing techniques on the small and finite deformation behaviors of HDPE. Since HDPE is a semi-crystalline polymeric material, the degree of crystallinity, molecular morphologies, and molecular structure extensively affect its mechanical behavior. Different manufacturing methods result in different molecular morphologies and molecular structure in the final product. Various experimental studies have investigated singly or combined aspects of deformation such as loading–unloading, relaxation, creep, multiple creep behavior of HDPE. However, this study has only been carried on one manufactured sample such as compression-molded or injection-molded sample. Understanding the deformation behavior under different loadings can offer the designer of HDPE products reliable data relevant to practical applications. The study of the loading history is important in engineering design because the mechanical properties and deformation mechanism may be heavily dependent on the applied loading types. Khan and Zhang [5] performed a series of tests on polytetrafluorethylene (PTFE) samples that included monotonic loading and multiple creep, multiple relaxation tests. This investigation revealed that the mechanical behavior of PTFE is independent of loading history. Zhang and Moore [6] investigated the multiple creep, relaxation, and cyclic compression behavior of HDPE including the testing of specimens after loading and partial unloading. Khan [7] performed a series of loading– unloading tests and multiple relaxation and creep tests on thermoplastics samples. He aimed to compare the effect of loading history on relaxation and creep tests at different loading and unloading stress– strain levels. Avanzini [8] carried out a fully reversed symmetric tensile and compression loading test on ultra-high molecular weight polyethylene (UHMWPE) samples and reported that strain softening and stress–strain hysteresis were observed after cyclic loading. Meyer and Pruitt [9] performed cyclic tensile loading tests on UHMWPE samples at large deformation levels and indicated that the mechanical behavior of UHMWPE was related to microstructural variables. Therefore, an increasing amount of strain and number of cycles increases the residual plastic strain, which reduces density. 454 N. DUSUNCELI AND B. AYDEMIR Zrida et al. [10] investigated the mechanical behavior of three grades of polypropylene (PP) at various loading conditions that include monotonic loading, cyclic loading–unloading, and multiple relaxations. This study showed that mechanical behavior of PP is highly nonlinear and hysteretic. This behavior depends on strain rate level. Zhang and Chen [11] performed multiaxial ratcheting test on solid cylindrical PTFE samples under constant axial stress with cyclically controlled shear strain at room temperature. They concluded that the ratcheting behavior of PTFE strongly depends on loading histories and increasing number of cycles decreases the ratcheting strain rate. Drozdov and Christiansen [12] conducted uniaxial tensile tests, relaxation tests, creep tests, and cyclic tests on two grades of HDPE. Their work focused on the mechanical behavior of HDPE associated with molecular weight. Increasing molecular weight affects crystalline morphology by making it more regular. This regularity causes an increasing elastic modulus and a slowing down of the viscoelastic processes. In the literature, much investigation has been conducted on the effect of strain rate, loading types, and temperature on the mechanical behavior of polymeric materials. A few studies have investigated the effect of loading history, cyclic deformation behavior, and manufacturing methods. The aim of experimental work reported in this article was to explore the mechanical behavior of HDPE associated with loading history, manufacturing methods, and cyclic loading–unloading. Multiple creep and relaxation tests were performed by loading two and three stress–strain levels. Cyclic loading–unloading tests were conducted for various strain and strain rate levels, and for each of the manufacturing methods. EXPERIMENTAL WORK The experiments are carried out with a Zwick 250 tensile machine at the National Metrology Institute in The Scientific and Technological Research Council of Turkey (TUBITAK). The load-cell capacity of the tensile machine can be adjusted for loads of 10, 20, 50, and 100 kN. A load-cell with capacity of 10 kN is used in tensile tests. First, the extruded samples for the tensile tests were obtained from PE100 (HDPE) pipe with a diameter 160 and wall thickness 5 mm. The extruded samples were created according to the ISO 6259-1 and ISO Effects on the Mechanical Behavior of HDPE 455 6259-3 standards for the determination of the properties of tensile deformation in polymeric pipes [13,14]. The compression-molded samples were punched out from compression-molded 2-mm thick HDPE sheets. The density of this material is 0.954 g m 3 and the trade name TotalXS10B. The samples were crated according to the ISO 527 Standard [15,16]. Figure 1 shows the dimensions of the extruded and compression- molded samples. To investigate the behavior of HDPE samples, the following experiments were performed. 1. Uniaxial loading and unloading at different strain rates, 1.E 4 s 1. 2. Cyclic loading–unloading at different strain rates: 1.E 3 and 1.E 4 s 1 and various loading–unloading strain levels. 3. Multiple creep at different stress levels, 6–16, 6–13, 13–16, and 6–13–16 MPa for 1200 s at the strain rate of 1.E 4 s 1. 4. Multiple relaxation at strain levels of 2–15%, 5–15%, 10–15%, and 5–10–15% at the strain rate of 1.E 4 s 1 for 1200 s. All tests were performed at 23 18C (room temperature). RESULTS AND DISCUSSIONS Loading–Unloading Behavior The uniaxial tension loading and unloading tests were performed on extruded and compression- molded HDPE at room temperature. The samples were loaded with a constant strain rate up to 15% strain and unloaded at the same strain rate. The uniaxial stress–strain behavior of HDPE at room temperature at 1.E 4 s 1 on both extruded and compression-molded samples are shown in Figure 2. The stress–strain curves have a similar overall behavior but the stress levels are different. The stress–strain curves of both the extruded and compression-molded samples demonstrated elastic–viscoelastic–viscoplastic mechanical behavior. The results of the uniaxial loading–unloading experiments performed at 15% strain levels showed that the maximum stress and yield stress of the extruded specimen were much higher than the compression-molded samples. The maximum stress levels of the extruded samples were 5 MPa higher than the compression-molded samples. The reason for this diversity is the degree of crystallinity and difference in the manufacturing technique that involves the reorientation of the polymer chains. 456 N. DUSUNCELI AND B. AYDEMIR FIGURE 1. The dimensions of the samples (all dimensions are in mm). FIGURE 2. Comparison of loading–unloading behaviors of extruded and compression-molded HDPE at 1.E 4 s 1. Loading–Unloading Strain Rate Change Dependency Two tests consisting of three loading–unloading steps were conducted to investigate the strain rate history and unloading behavior. The first test was conducted at the same strain rate, 1.E 4 s 1, and it consisted of three loading–unloading steps at 5%, 10%, and 15% strain levels. Effects on the Mechanical Behavior of HDPE 457 FIGURE 3. Comparison of cyclic and single loading–unloading behaviors of extruded HDPE at 1.E 4 s 1. FIGURE 4. Comparison of cyclic loading–unloading behaviors of compression-molded HDPE at 1.E 4 and 1.E 3 s 1. These test results are given in Figures 3 and 4 for the extruded and compression-molded samples, respectively. The second test was performed three loading–unloading steps at 5% strain level at 1.E 4 s 1, followed by 10% at 1.E 3 s 1, and 15% strain level at 1.E 4 s 1 458 N. DUSUNCELI AND B. AYDEMIR FIGURE 5. Comparison of cyclic and single loading–unloading behaviors of extruded HDPE at 1.E 4 and 1.E 3 s 1. strain rate; see Figures 5 and 6 for studying the extruded and compression-molded samples, respectively. The strain rate of the last step for each test was the same; so, the stress level at the same strain rate could be directly compared for different histories. The shapes of the unloading curves are nonlinear concave curvature for each of the samples at each of the loading–unloading steps. For the unloading, only the initial stress level affected the evolution of the unloading curve. Increasing the stress level shifted the loading curve inward and increased the amount of recovery on unloading. The magnitudes of the recovered strain magnitudes are given in Table 1. The unloading behavior of both samples at all strain rates is nonlinear and the viscoelastic recovery during the unloading (until zero stress level) increases with an increase in the strain level. The extruded samples are more recovered than compression-molded samples. Figures 5 and 6 show that despite the second step loading–unloading strain rate on the second test not being the same as the other two steps; there is no difference in the last loading curve. Finally, in Figures 3 and 4, the loading–unloading stress–strain curves at 15% at 1.E 4 s 1 are compared with the cyclic loading–unloading stress–strain curve and it can be seen that cyclic loading–unloading history has no effect on the mechanical behavior of HDPE. 459 Effects on the Mechanical Behavior of HDPE FIGURE 6. Comparison of cyclic loading–unloading behaviors of compression-molded HDPE at 1.E 4 and 1.E 3 s 1. Table 1. The percentage of viscoelastic recovered strain during unloading. Number of step Single 1 2 3 1 2 3 Strain rate (s 1) 1.E 1.E 1.E 1.E 1.E 1.E 1.E 4 4 4 4 4 3 4 Strain level (%) Extruded sample (%) Compression-molded sample (%) 15 5 10 15 5 10 15 10.34 3.65 6.96 10.34 3.65 6.2 10.34 8 2.57 5.34 8 2.57 5.1 8 Creep Creep is a strain increasing with time when the stress level is kept constant. For the prediction of the durability and reliability over the lifetime of components made from polymeric materials, the creep responses of the polymers are fairly important. Creep deformation of polymeric materials can occur at relatively small stress level at room temperature. Two- and three-step multiple creep tests were conducted to investigate the effects of stress and loading history. Multiple creep tests were performed for both sample types at different stress 460 N. DUSUNCELI AND B. AYDEMIR FIGURE 7. Comparison of creep stress–strain behaviors of extruded HDPE at various stress levels. levels: 6–16, 6–13, 13–16, and 6–13–16 MPa for 1200 s at the strain rate of 1.E 4 s 1 in Figures 7 and 8. The percentages of creep strain were calculated for both the samples and are presented in Table 2. The amount of creep strain increases with the rising stress level and is independent of the effect of the loading history. These results indicated that the compression-molded samples had greater creep strain magnitude especially at high-stress level than the extruded samples. The strain versus time curves are given in Figures 9–11. All the viscous effects are related to the delayed response of the polymer chains. It is observed that at higher stress levels, compression-molded samples yielded greater change in strain than the extruded samples. Relaxation Relaxation is a drop in stress over time when the strain level is maintained. For polymeric materials, even at small strains, relaxation is observed. According to Krempl and Khan [17], relaxation is constant in the inelastic region of the stress–strain curve. To investigate both this case and the effect of the loading history, multiple relaxations at the strain levels of 2–15%, 5–15%, 10–15%, and 5–10–15% at the strain rate 1.E 4 s 1 were performed for 1200 s. Increasing strain level increases the stress drop. Finally, the relaxation was found to be at the same 461 Effects on the Mechanical Behavior of HDPE FIGURE 8. Comparison of creep stress–strain behaviors of compression-molded HDPE at various stress levels. Table 2. The percentage of strain increasing during creep test at different stress levels. Stress level (MPa) 6 13 16 Extruded sample (%) Compression-molded sample (%) 0.434 1.43 1.58 0.75 3.25 6.23 magnitude in the inelastic region. The stress versus strain at the strain levels of 2–15%, 5–15%, 10–15%, and 5–10–15% are shown in Figures 12 and 13 for the extruded and compression-molded samples, respectively. Following the relaxation experiments, the same sample was reloaded at different strain levels. It was observed that stress levels were almost the same after reloading, as can be seen Figures 12 and 13. Such an observation reveals that material is not history dependent: to a large extent, prior loadings do not affect the subsequent behavior. The percentages of the stress drop during relaxation test at different strain levels are given in Table 3. The results of three relaxation tests together with stress–time curves are compared in Figures 14–17 for all strain levels. It can be seen that evolving of trend of the curves is 462 N. DUSUNCELI AND B. AYDEMIR FIGURE 9. Comparison of creep behaviors of extruded and compression-molded HDPE at a stress level of 6 MPa. FIGURE 10. Comparison of creep behaviors of extruded and compression-molded HDPE at a stress level of 13 MPa. Effects on the Mechanical Behavior of HDPE 463 FIGURE 11. Comparison of creep behaviors of extruded and compression-molded HDPE at a stress level of 18 MPa. FIGURE 12. Comparison of relaxation stress–strain behaviors of extruded HDPE at various strain levels. 464 N. DUSUNCELI AND B. AYDEMIR FIGURE 13. Comparison of relaxation stress–strain behaviors of compression-molded HDPE at various strain levels. Table 3. The percentage of stress drop during relaxation test at different strain levels. Strain level (%) 2 5 10 15 Extruded sample (%) Compression-molded sample (%) 27 24.9 22.09 21.6 28 23.2 24.3 23.6 approximately equidistant for all the strain levels. One of the interesting aspects of the relaxation experiments is that stress drop is approximately the same in the both the extruded and compression- molded samples, as seen in Table 3. These results indicate that manufacturing methods have no influence on the relaxation behavior of HDPE. CONCLUSIONS Comprehensive research on the mechanical behavior of HDPE was carried out to investigate the effects of loading history and Effects on the Mechanical Behavior of HDPE 465 FIGURE 14. Comparison of relaxation behaviors of extruded and compression-molded HDPE at a strain level of 2%. FIGURE 15. Comparison of relaxation behaviors of extruded and compression-molded HDPE at a strain level of 5%. 466 N. DUSUNCELI AND B. AYDEMIR FIGURE 16. Comparison of relaxation behaviors of extruded and compression-molded HDPE at a strain level of 10%. FIGURE 17. Comparison of relaxation behaviors of extruded and compression-molded HDPE at a strain level of 15%. Effects on the Mechanical Behavior of HDPE 467 manufacturing methods on different manufactured samples. Uniaxial cyclic loading–unloading, multiple creep, and multiple relaxation tests were conducted at room temperature. The HDPE exhibited nonlinear time- dependent and loading history-independent behavior in the uniaxial tension test. The deformation behaviors of both samples have the same trend except for the stress–strain level. In the cyclic tests, the unloading behaviors of both samples at all strain rates were nonlinear and the viscoelastic recovery during unloading (until zero stress level) rises with an increase in the strain level. The extruded samples recovered more readily than the compression-molded samples on unloading. The creep behavior of HDPE was found to be independent of loading history and the amount of creep strain increases with the rising stress level. The amount of creep strain in compression-molded sample was greater than in the extruded samples at especially high-stress levels. The relaxation behavior of HDPE is independent of loading history and the stress drop magnitude decreases with increasing strain level. 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