LABORATORY “8” Tensile Testing of GFR Nylon 6,6, Nylon 6,6, GFR PP, PP, PS, and LDPE Mohammed Alzayer Chris Clay Xinhang Shen Mat E 453 Lab Section 2 November 4th, 2014 1 ABSTRACT Eight polymer samples were analyzed under tensile testing. Glass Fiber Reinforced Nylon 6, 6 (GFR(N6,6)), Glass Fiber Reinforced Polypropylene (GFR(PP)), and Polystyrene(PS) were brittle. The polypropylene (PP), low-density polyethylene (LDPE) and Nylon 6,6 without glass reinforcement were more ductile. PP and LDPE were tested under different strain rates, with no strain rate sensitivity being observed. Young’s Modulus for each sample was calculated and analyzed by plotting both the engineering and the true stress-strain curves. 1. INTRODUCTION 1.1 Tensile Testing Tensile testing is a technique in which the mechanical properties of materials can be determined. A tensile tester subjects a sample to an axial load and Figure 1 Schematic of the ASTM D 638 [1] (right), an actual unit (left). measures the amount of deformation in mm and load in N that the sample is experiencing during the test (Figure 1). This information can be used to plot a stress versus strain plot for the tested sample. This plot can be useful in determining properties such as yield strength, ultimate tensile strength, 0.2 offset yield strength, Young’s modulus, and strain at fracture. Tensile testing 2 has the setback of destroying the sample. In other words, tensile testing is a destructive method. 1.2 Stress vs Strain Curves The stress is related to the load measured by the instrument by the following equation: 𝐹 𝜎=𝐴, (1) where σ: stress in Pa, F: load in N, A: cross sectional area of sample in m2. From Equation 1, the stress is measured by the unit 𝑁/𝑚2 which is often referred to as Pascal (Pa). The strain is given by the equation below: 𝜀= 𝐿−𝐿0 𝐿0 Figure 2. Dog-bone shaped samples used for tensile testing. , (2) where ε: strain in m/m, L: instantaneous length of the sample in m, L0 : initial length of the sample, aka gauge length, in m. The polymeric specimens used in tensile testing are often given in a dog bone shape (Figure 2). The specimens are aligned parallel to the instrument and are pulled to elongate until they break. In order to determine the stress these samples experience, the 3 cross sectional area must be calculated first. For a dog-bone shaped sample, this area is given by the product of its width and thickness in any part of the straight portion of the specimen before it curves. The length of the straight part in the middle of the specimen is known as the gauge length (Figure 2), which is 𝐿0 in Equation 2. The quantity 𝐿 − 𝐿0 is the displacement of the sample relative to its original length and is measured by the instrument. Hence, 𝐿0 must be measured before the test in order to calculate the strain. When using Equations 1 and 2, the resulted stress versus strain curve is labeled as an “engineering” curve. The engineering stressstrain curve does not account for a phenomenon known as ‘necking.’ Necking happens when the material reaches its ultimate tensile strength, which is the peak of the stress versus strain curve. After this point, the cross-sectional area of the sample decreases dramatically, causing the sample to Figure 3 Necking of samples neck. Equations 1 and 2 yield an engineering stress-strain curve because they assume a constant cross-sectional area throughout the entire test including the part when the sample necks. 4 Two other equations were derived in order to account for necking. These equations are as follows: 𝐿 𝜎𝑇 = 𝜎 𝐿 , (3) 0 where 𝜎𝑇 : true stress in Pa, 𝜎: instantaneous stress in Pa, L: instantaneous length of the sample in m, L0 : initial length of the sample, aka gauge length, in m. And the true strain can be calculated as follows: 𝐿 𝜀𝑇 = 𝑙𝑛 (𝐿 ) , (4) 0 where 𝜀𝑇 : true strain in m/m, L: instantaneous length of the sample in m, L0 : initial length of the sample, aka gauge length, in m. A typical stress-strain curve consists of four regions: elastic region, yielding region, strain hardening region, and necking region (Figure 4). The initial linear portion of the curve represents the elastic regime. The slope of this line gives an important quantity that is called Young’s modulus. According to Callister, Young’s modulus, also known as the modulus of elasticity, is “the ratio of stress to strain when deformation is totally elastic; also a measure of the stiffness of a material.” Accordingly, the Young’s modulus differs from material to another. By this definition, Young’s modulus is given by the following equation: 5 𝜎 𝐸 = 𝜀, (5) where 𝐸: Young’s modulus in Pa, σ: stress in Pa, ε: strain in m/m. In the yielding region, the material exhibits a plastic behavior which is a permanent deformation. Strain hardening commonly occurs in metals. In this region there is an increase in the stress experienced by the sample meaning the material becomes harder. The material finally starts to neck before it fractures. Figure 4 Vairous regions and points on the stress-strain curve [2] 6 1.3 Modes of Fracture Polymers will exhibit different types of fracture depending on how free the polymer chains are to move past each other when a stress is applied. A polymer is said to be hard if it shows a high slope in the region of elastic deformation, indicating that it requires a higher stress to cause the polymer chains to stretch elastically. Similarly, if a polymer shows a low slope in the region of elastic deformation. It should be noted that “hard” and “soft” are relative terms, as almost all polymers would be considered soft when compared to metals or ceramics. If the polymer chains are completely fixed in place, the polymer will break immediately after the elastic stretching has completed. This is called brittle fracture, as no plastic deformation is observed. Brittle fracture typically results in shiny surfaces where the fracture occurs as the lack of plastic deformation results in relatively smooth surfaces that light can specularly reflect off of. Chains are typically more immobile in cross-linked polymers and when bulkier side groups are present to prevent slippage. If the polymer chains are less fixed in place, the chains can start to slip past each other after elastic deformation has concluded. This results in ductile fracture, which is evident because of rough, uneven surfaces which light reflects diffusely off of, meaning that the fracture will not appear shiny. 7 If a polymer deforms plastically, its toughness will increase as more energy will be required to cause chain slippage before it fractures. In a stress-strain curve, the area under the curve is equal to the toughness. Another common fracture mode is known as crazing. Crazing causes fracture in regions of high hydrostatic tension or in regions of localized yielding in thermoplastic polymers. Crazing occurs in polymers due to the combination of weak forces such as Van der Waals and the stronger covalent bonds. If a local stress is sufficient, it can overcome the Van der Waals force, allowing a narrow gap to form. The covalent bonds which hold the chains together prevent further widening of the gap. Oftentimes, a craze cannot be felt on the surface of a material. A craze is different from a crack in that it can continue to support a load. Typical stress strain curves for the different fracture modes are shown in Figure 5. Figure 5 Plots of stress-strain curves of typical polymeric materials [2] 8 2. EXPERIMENTAL PROCEDURES 2.1 Materials Table 1 shows the repeating units of each material tested in this lab: Table 1: Repeating units of samples tested in lab. In total, 8 specimens were tested: 1. Glass Fiber Reinforced Nylon 6,6 at 5 mm/min. 2. Nylon 6,6 at 5 mm/min. 3. Glass Fiber Reinforced Polypropylene at 5 mm/min. 4. Polypropylene at 5 mm/min 5. Polypropylene at 50 mm/min. 6. Polystyrene at 5 mm/min. 7. Low-density polyethylene at 5 mm/min. 8. Low-density polyethylene at 50 mm/min. 9 2.2 Specimen Measurement The polymer specimens were cut into dog-bone shapes. 1) The thickness and width of polymer samples were measured using a micrometer. 2) Sample defects were made note of. 2.3 Software Setup 1) The tensile test instrument and the video extensometer were turned on. 2) On the main page, “Test” was selected to start a new sample. 3) The load cell was calibrated. All loads were removed from the load cell and calibrated. 4) The load was zeroed once the clamps were installed. 5) The up and down arrows were pressed on the controller until the clamps were just touching. 6) The up and down arrows were used until the clamps were about 100 mm apart. 7) The polymer sample was placed vertically between the grips of both the tensile test instrument. 8) The extension and the load were zeroed. 9) Geometrical dimensions of the sample were entered. 10) The “Start” button was clicked. Observed the experiment at a safe distance at an angle and note of the failure mode was taken when the specimen failed. 2.4 End of Task 1) The two handles were turned in the open directions to remove the sample. 2) The data file was saved. 3) Broken fragments were cleaned up. 4) The instrument was turned off and the program was closed. 10 3. RESULTS 3.1 Engineering Stress vs Strain The engineering stress-strain curves obtained from the raw data are shown in Figure 6. The Instron tensile tester actually measures the load it is applying as well as the sample's elongation. However, as the sample's cross sectional width and thickness were measured by micrometer (Appendix Table A1) and entered into the instrument software, the software can calculate the stress using Equation 1. Similarly, as the instrument automatically measured the initial gauge length, the software calculated the change in strain as elongation occurred using Equation 2. Using the outputted data files, the stress vs strain curves could be plotted using Excel (Figure 6). Stress (MPa) 100 80 60 40 20 0 0 0.5 1 1.5 Strain (mm/mm) Nylon 6,6 GFR Nylon 6,6 PP GFR PP (50 mm/min) PP (5 mm/min) PS LDPE (50 mm/min) LDPE (5 mm/min) Figure 6. Plot of engineering stress-strain behavior of eight samples 11 The Young's Modulus of the materials could be estimated by taking the slope of the linear region of elastic deformation (Figure 7). The results of the Young's Modulus calculation, as well as the final elongation distances and loads, are summarized in Table 2. y = 1512.4x + 10.349 Strss (MPa) 100 80 60 y = 2640.3x - 25.734 y = 1469.3x - 8.2448 y = 719.79x - 3.087 40 20 y = 705.01x - 3.7455 y = 65.871x + 0.5062 y = 75.06x + 0.9093 0 0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 Strain (mm/mm) Nylon 6,6 GFR Nylon 6,6 PP GFR PP (50 mm/min) PP (5 mm/min) PS LDPE (50 mm/min) LDPE (5 mm/min) Figure 6. Elastic region of engineering stress-strain behavior of eight samples 3.2 True Stress vs Strain Equations 1 and 2 used to calculate the engineering stresses and strains are not entirely accurate, as they assume the cross-sectional area of the specimen does not change during tensile loading. During the region of elastic deformation, this is a reasonable assumption to make. However, once plastic deformation, and in particular necking, begin to occur, the cross-sectional area of the specimen can change dramatically (Figure 3). This change 12 in cross-sectional area is accounted for in the equations for true stress and strain, Equations 3 and 4. Using these equations, the true stress vs true strain graphs could be generated (Figure 8). 140 120 Stress (MPa) 100 80 60 40 20 0 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 Strain (mm/mm) Nylon 6,6 GFR Nylon 6,6 PP GFR PP (50 mm/min) PP (5 mm/min) PS LDPE (50 mm/min) LDPE (5 mm/min) Figure 7 Plot of true stress-strain behavior of eight samples The Young's Modulus could be estimated in the same manner using the true stress-strain curves as was done for the engineering stress-strain curves (Figure 9, Table 2) 13 120 y = 1971.5x + 0.4721 100 80 60 y = 3232.1x - 26.029 40 y = 1841.6x - 8.8873 y = 902.05x - 3.3832 20 y = 807.07x - 3.0887 y = 87.806x + 0.3796 y = 94.294x + 0.9857 0 0 0.01 0.02 0.03 0.04 0.05 0.06 Nylon 6,6 GFR Nylon 6,6 PP GFR PP (50 mm/min) PP (5 mm/min) PS LDPE (50 mm/min) LDPE (5 mm/min) 0.07 0.08 Figure 8 Elastic region of true stress-strain behavior of eight samples Table 2. Loads, extensions, and engineering, true and literature Young’s Moduli Material Load Extension Engineering True E Literature (N) (mm) E (GPa) (GPa) E (GPa) GFR Nylon 6,6 27.9 8.66 1.51 1.97 2.70-8.56 [4] Nylon 6,6 17.3 98.2 0.720 0.900 1.60 [5] GFR PP 58.6 3.65 2.64 3.23 7.40 [6] PP (50 mm/min) 35.6 111 0.710 0.810 0.90-1.10 [5] PP (5 mm/min) 785 103 0.710 0.880 PS 27.0 1.96 1.47 1.84 1.90-2.90 [5] LDPE (50 11.5 91.6 0.0751 0.0943 0.30 [5] 409 56.5 0.0659 0.0878 mm/min) LDPE (5 mm/min) 14 4. DISCUSSION 4.1 Mechanical Properties The glass-fiber reinforced polymers showed the highest Young's Modulus because glass itself has a higher Young's modulus than any polymer. The benefit of reinforcing polymers with glass fibers instead of just using glass fibers is that the polymer coating protects the glass fibers from sudden impacts that could cause the glass to fracture. Also, if one glass fiber has a significant defect such as a crack in it and fails before the rest, the polymer coating separates it from the rest of the fibers preventing catastrophic failure. Thee glass reinforced polymers also showed little plastic deformation as expected, because glass is a brittle material. The polymer with the next highest Young's modulus was polystyrene, which also showed little plastic deformation. This agrees with expectations, as the bulky phenyl group on the polymer chain (Table 1) acts to prevent chain slippage. Nylon 6,6 showed the next highest Young's modulus and also showed significant amount of plastic deformation. This indicates that chains are able to slide past each other and uncoil beyond the region of elastic deformation. The polymers with the two lowest Young's moduli were polypropylene and low-density polyethylene, with PP being slightly higher. These polymer both showed huge amounts 15 of plastic deformation, as polyethylene has no side groups, and polypropylene has only a small methyl side group. The Young's moduli calculated with the true stress and strain equations were higher than those calculated with the engineering stress and strain equations. The reason for this is the true equations took into account the decrease in cross-sectional area, making the true stress values higher than the engineering stresses. The experimental values for Young's moduli were all lower than the literature values. One possible reason for this include inaccuracies in the measured specimen thicknesses and widths, as these were only measured once with a digital micrometer. More measurements could lead to more accurate thicknesses and widths. A more probable reason for the deviation from literature values is that the Instron measures the gauge length to be longer than it actually is, due to the angling of the specimen between the actual gauge and where the specimen is being held. Both polypropylene and LDPE showed little sensitivity to strain rate, as the stress-strain curves are almost identical. However, as the 5 mm/min samples were stopped before they got to the strain that the 50 mm/min samples failed at, this testing is inconclusive. The stoppage occurred due to time constraints. If the 5 mm/min samples had been allowed to continue, they would have been expected to reach higher strain values than did their 50 mm/min counterparts. 16 4.2 Fracture Comparisons Polymers with glass fiber reinforcement and bulky side groups (e.g. polystyrene) showed brittle fracture characteristics such as a smooth shiny surface, as the chains are unable to slip past each other effectively. Polypropylene and LDPE showed almost complete ductile fracture (rough, uneven surfaces, while reinforced Nylon 6,6 showed intermediate properties (Figure 10). Polypropylene showed high amounts of crazing, easily seen by the fiber pullouts. The trend of more immobile chains having tendencies for brittle fracture agrees with expectations. Figure 9 Cross-sections of fours samples after fracture (left), all the eight samples after tensile testing (right) 17 5. CONCLUSIONS 1. Glass fiber reinforced polymers showed the highest Young's moduli and brittle fracture. 2. Polymers with less mobile chains, such as Nylon 6,6 and PS, showed higher Young's moduli and a tendency for brittle fracture. 3. Polymers with more mobile chains, such as LDPE and PP, showed lower Young's moduli and a tendency for ductile fracture. 4. No strain-rate sensitivity was observed due to time constrains of the lab. 5. Using true stress-strain equations instead of engineering stress-strain equations resulted in higher calculated stresses and therefore higher Young's moduli. 6. The experimental values for the Young's moduli were consistently lower than literature values. 6. ACKNOWLEDGMENTS The group would like to thank Dr De Leon for providing the polymer dogbone samples. 18 7. REFERENCES [1] Callister, W., David R. Materials Science and Engineering: An Introduction. Wiley Inc., 2010. [2] De Leon, Jose. “Lab 8: Tensile Testing.” Iowa State University. Web. [3] “Understanding Crazing.” Orton Firing Institute. Web. [4] “Overview of materials for Nylon 66/6, 20% Glass Fiber Reinforced” MatWeb. Web. [5] MakeItFrom.com. Web [6] “Borealis Nepol™ GB303HP Long Glass Fiber Reinforced Polypropylene” MatWeb. Web. 19 Appendix Table A1. Geometrical dimensions of eight samples before tensile testing. A standard gauge length of 78 mm was used in all calculations. Material Width (mm) Thickness (mm) GFR Nylon 6,6 10.34 4.06 Nylon 6,6 10.30 3.95 GFR PP 9.85 3.99 PP (50 mm/min) 10.71 3.97 PP (5 mm/min) 10.57 4.04 PS 10.61 3.98 LDPE (50 mm/min) 10.34 4.04 LDPE (5 mm/min) 10.08 4.04 20