EXPERIMENTAL TESTS OF FATIGUE INDUCED DELAMINATION IN GFRP LAMINATES D. Tumino, G. Catalanotti, F. Cappello, B. Zuccarello Dipartimento di Meccanica, DIMA Università degli Studi di Palermo 90128 – Palermo, Italy ABSTRACT This work deals with the experimental analysis of the delamination phenomena in composite materials under different loading conditions. Quasi-static and fatigue tests are performed on specimens made of glass-fibre reinforced plastic (GFRP). In particular, experiments have been done under single fracture modes I and II (using standard DCB and ENF test configurations) and mixed modes I+II (using the MMB test configuration) with several mode mixtures. Attention has been drawn on the relationship between the parameters that describe the fatigue behaviour and the mode mixture acting during the crack propagation. Introduction The study of the behaviour of long-fibre composite materials is, nowadays, a well established discipline in the field of structural materials. Although such materials have, day by day, a larger diffusion into industrial applications, the comprehension of the behaviour under different load conditions is still under investigation. Among the several kinds of damage which composites can be subjected to, the phenomenon of delamination is one of those that mostly draws the researcher’s attention. Considering only plane cases, the single fracture modes are two: opening (mode I) and sliding (mode II); mixed modes I+II cases can be also present. The case of crack propagation under quasi-static loads (when the applied load increases monotonically very slowly) has been studied by several authors, both for single fracture modes and for mixed mode. A detailed formulation on the test coupons commonly used in experiments can be found in [1] and [2]. While single modes I and II are usually obtained with the Double Cantilever Beam (DCB) test and the End Notched Flexural (ENF) test [3], for the mixed mode I+II there are different test configurations [4] (see fig. 1). The Mixed Mode Bending (MMB) test [5]-[7] is the super-position of the DCB and the ENF tests and permits a fast change of percentage of mode I and mode II by a simple variation in the lever length c. Another test configuration has also been used for mixed mode fracture: the Single Leg Four Point Bending (SLFPB) test, developed and studied in [8], that is less versatile than the MMB test, but is easier to setup. In quasi-static condition, crack propagates under single fracture modes when the Strain Energy Release Rate (SERR), G, equals its critical value (or interlaminar fracture toughness) Gc. This critical value is a material property and can be different for mode I and for mode II. It has been noted [9] that the critical SERR depends on the mode mixture φ = GII/G (where G is the sum of GI and GII) and different criteria have been proposed to model the material behaviour at fracture as φ varies. In [9] different models are compared and applied to experimental results on a carbon/epoxy material. In general, the fatigue delamination of composites, caused by the cyclic application of loads, can be described with the Paris approach. Following this method, the condition of a stable crack growth can be obtained when the instant SERR is greater than a threshold value and lower than the fracture toughness. In a log-log diagram (da/dN versus Gmax) the stable zone is m described by a line whose equation is da/dN = B(Gmax) , where B and m are characteristics of the material and of the mode mixture. Fatigue tests on different composite materials have been performed in [10] for single modes I and II and in [11],[12], where the load ratio effect and the threshold values for the SERR have been studied. In particular, results for graphite/thermoplastic resin in [11] lead to very high values for the Paris constants, suggesting that, for this material, a threshold-based design is more realistic than a propagation-based one. Single and mixed mode cases have been studied in [13] for a graphite/epoxy composite; a non monotonic trend of the Paris parameters with the mode mixture was observed. In [14] the effect of the temperature has been also verified for the same material and it has been proven that the crack growth rate increases with the temperature. Semi-empirical monotonic models have been proposed in [15] and [16] to correlate the Paris parameters B and m to the mode mixture φ, on the basis of experimental results on different materials. In [16] several mode mixtures have been analysed for glass/epoxy composites; the model fits quite well with the peculiar behaviour of the tested composite, but could not work for other materials (as in the case of the present work). In [17] three mode mixture have been studied (φ = 0, 0.5 and 1) for carbon/epoxy material; although the non-monotonic model proposed to relate φ with the Paris parameters can be considered of general validity, it is based on very few experimental data. In this work experiments of fatigue crack propagation on unidirectional GFRP have been performed under single and mixed fracture modes. Preliminary quasi-static tests have been done to calculate the fracture toughness of the material. For the analysed material, the accordance between the monotonic and non monotonic criteria with the experimental results, has been verified. l max v,P l min l l a l a c v,P v,P v,P SLFPB Figure 1. Test configurations for single and mixed fracture modes Material tested The material used is a glass/epoxy composite manufactured by the hand lay-up technique. It consists of 12 laminae of dry unidirectional fabric stacked together with an epoxy resin. In the half-thickness of the laminate a short strip of anti-adhesive (Mylar®) which standard thickness is about 10 μm, has been inserted, with the aim to create a pre-crack in the specimens. The cure of the resin has been obtained with a first period (12 hours) at room temperature followed by a second period (12 hours) in the oven at 60°C. During the entire period of curing a slight pressure was applied to the laminate. After the curing process, the fibre weight fraction Wf has been calculated by measuring the weight of the composite and knowing the weight of 3 3 the fibres. It results Wf = 40%. Then, knowing the density of glass fibres (ρf = 2.5 g/cm ) and matrix (ρm = 1.07 g/cm ) the 3 density of the composite can be calculated (ρc = 1.43 g/cm ) and the fibre volume fraction via the relation [18]: Vf = ρc W = 26% ρf f (1) The reason for the low value of Vf can be found in the manufacturing process, where no vacuum techniques have been adopted, and in the particular morphology of the dry patches of fibres, that consists of well-separated bundles (see also figure 2.a). The gap between bundles is filled with the resin during lamination resulting in a matrix excess into the composite. Preparation of the specimens Specimens have been cut from the plate following the standard ASTM D3039 for tensile test, the ASTM D790 for flexural test and the standard ASTM D4255 for the rail shear test. Each specimen has been instrumented with resistance gauges to measure the longitudinal and the transversal strain. Tests have been carried out with an electro-mechanical testing machine with a 20 kN capacity load cell, under displacement control. Results of the tests are summarised in table 1. TABLE 1. Material properties. Material E-glass/Epoxy EL [GPa] 21 ET [GPa] 6 νLT 0.28 GLT [GPa] 1.6 Specimens for delamination tests have been machined from the composite plate following the indications of the standard ASTM D5528. Width and thickness of the specimens are the same for all the tests performed in this work. In particular, a width Bw = 20 mm and a total thickness 2h = 4.7 mm (where h is the thickness of one arm of the specimen after the crack propagation) have been measured. Each specimen has been painted in its lateral face with a matt white colour and marks have been drawn at regular intervals (1 mm). Except the ENF test, for both DCB and MMB tests (where a mode I component is present) hinges have been glued to the precracked ends of the specimens using a cyanoacrylate fast-curing glue (see fig. 2.b). Because of the high values of loads applied to the hinges, premature debonding between hinge and specimen was observed during the linear part of the loading curve. This issue has been solved with a more accurate preparation of the surfaces glued together: surfaces were initially roughed with sand paper and then cleaned with degreasing agents. (a) (b) Figure 2. Close-up on the fibres (a) and the DCB specimen (b). Quasi-static tests Quasi-static delamination tests have been performed with an electro-mechanical testing machine with a 2 kN capacity load cell, under displacement control. The displacement, v, of the cross-head and the load, P, measured by the load cell have been recorded. The crack length, a, has been evaluated by optical observation of digital photos of the lateral face of the specimen taken with a high resolution Nikon camera equipped with a macro lens. Average dimensions of the specimens used for the tests are summarised in table 2. TABLE 2. Specimen dimensions [mm]. Test DCB MMB (φ = 0.25) MMB (φ = 0.5) MMB (φ = 0.75) ENF Mid-span length l 75 75 75 55 Pre-crack a0 40 38 46 52 30 Lever length c 125 66 45 - Data reduction Figure 3 shows the typical load-displacement curves for DCB, ENF and MMB tests performed under monotonic loads. For the DCB test it is easy to distinguish the linear region from the softening region of the diagram. The first one corresponds to a strain energy increasing process where the crack doesn’t grow, the second one corresponds to the strain energy release process where the crack propagates and load decreases. For the ENF test, different parts can be pointed out: in the first linear one the load increases and the crack doesn’t grow, then, near the maximum point, the crack starts to propagate slowly; after the maximum point, the crack propagates very fast and the load decreases; in the last part the crack passes the mid-span length and the load increases again. Similar considerations to those relative to the ENF test can be done for the MMB tests, although curves in figure 3.c show results from test stopped soon after the maximum point has been reached. Simplified and more efficient data reduction theories [2]-[6] can be found in literature to obtain the Strain Energy Release Rate from the recorded data. Taking into account spurious phenomena like rotations of the arms in correspondence of the crack tip, or shear deformations, the data reduction theory suggested in [13] is adopted. In this theory the components in mode I and in mode II of the total strain energy released can be found (for DCB, ENF and MMB) via the relationships: PI2 (a + Δ ) BW E L I H 2 GI = (2) and GII = 3PII2 a 2 64 BW E L I H ⎛ EL h 2 ⎞ ⎜1 + ⎟ ⎜ 9 KG a 2 ⎟ LT ⎝ ⎠ where IH is the moment of inertia of half-thickness of the specimen, Δ is a correction factor of the crack length a given by: (3) ⎡⎛ E Δ = h ⎢⎜⎜ L ⎢⎣⎝ 6 ET 1/ 4 ⎞ ⎟⎟ ⎠ + EL ⎤ ⎥ GLT ⎥ ⎦ 1 2π (4) K = 5/6 is the shear factor. For the single mode tests, loads can be simply taken from the value, P, measured by the load cell; for the DCB test eq. (2) is used and PI is the load applied at the hinges, whereas for the ENF test eq. (3) is used and PII is the load applied by the pin in the mid-span length of the specimen. For the MMB test, loads in eq. (2) and (3) can be evaluated via the following formulas: 3c − l P 4l c+l P PII = l PI = 90 (6) 800 (a) 80 250 (b) 700 (c) φ = 0.75 200 70 600 60 500 40 150 P [N] 50 P [N] P [N] (5) 400 φ = 0.5 100 300 30 200 20 0 φ = 0.25 50 100 10 0 5 10 15 20 25 30 35 40 0 45 0 2 v [mm] 4 6 8 10 12 14 0 0 5 10 v [mm] 15 20 25 30 v [mm] Figure 3. Load-displacement plots for DCB (a), ENF (b) and MMB (c) tests. In figure 3 the circles indicates the loads used to the evaluation of the SERR that have been selected in accordance with the ASTM D5528. Table 3 summarises the critical values of the total SERR for the different value of the mode mixture φ. These critical values are quite different with respect to those reported in [16] but are in good agreement with data reported in [10] for a similar material. TABLE 3. Critical values of SERR [N/mm]. Mode mixture φ 0 0.25 0.5 0.75 1 Test DCB MMB MMB MMB ENF GIcφ 1.25 1.14 0.97 0.60 0 GIIcφ 0 0.38 0.97 1.81 3.6 Gc 1.25 1.52 1.94 2.41 3.6 For the DCB and ENF tests, the resistance curves, i.e. the SERR as a function of the actual crack length, are plotted in figure 4. In details, figure 4.a shows the resistance curve calculated for the DCB test; the critical value of the SERR in table 3 is located, in figure 4.a, at the beginning of the curve, when the crack starts to grow. The curve has a monotonic trend and doesn’t show an horizontal asymptote. This behaviour is due to fibre-bridging phenomena in front of the crack tip that are evident after few millimetres of crack propagation. The fracture toughness is calculated at the very beginning of the curve, when fibre-bridging phenomena are not present yet. Resistance curve for the ENF test is shown in figure 4.b; it can be seen how, in the first phase, the SERR increases with the crack length; at this stage the load increases with the displacement in figure 3.b. The maximum value of load corresponds to a crack length of 40 mm, then the test becomes unstable and the crack suddenly reaches the mid-span length of the specimen. The energy released can be considered constant with the crack length for a > l, as shown in figure 4.b. 3 4.5 (a) 2.8 (b) 4 2.6 3.5 2.2 GII [N/mm] GI [N/mm] 2.4 2 1.8 1.6 3 2.5 2 1.4 1.5 1.2 1 40 42 44 46 48 50 52 54 56 58 1 60 30 35 40 a [mm] 45 50 55 60 65 70 a [mm] Figure 4. Resistance curve for DCB (a) and ENF test (b) The optimal resistance criterion that describes this material can be found by plotting the points in table 3 on a plain (G φ IIC ) ( ) φ / G IIC , GIC / GIC . Following the generalised power criterion proposed in [9], the equation that describes the resistance of a material under mixed mode is: φ ⎛ GIC ⎜ ⎜G ⎝ IC α ⎛ Gφ ⎞ ⎟ + ⎜ IIC ⎜G ⎟ ⎝ IIC ⎠ β ⎞ ⎟ =1 ⎟ ⎠ (7) In figure 5 the experimental points are drawn together with the equation (7) obtained by the best-fitting procedure implemented in Matlab® environment. It is seen that, although the curve fitting gives α = 1.21 and β = 0.84, the approximation obtained by using α = β = 1 (linear resistance behaviour) can be also used in practice (the difference between the two lines is negligible). mode mix = 0.25 mode mix = 0.5 mode mix = 0.75 power int. linear int. 1 GφI /GIc 0.8 0.6 0.4 0.2 0 0 0.2 0.4 0.6 0.8 1 GφII/GIIc Figure 5. Fracture domain Fatigue tests Fatigue tests have been performed by using a MTS servo-hydraulic testing machine, equipped with a in-house made 1 kN load cell. Both displacement and load control have been used to carry out the experiments. Similarly to quasi-static tests, the crack length is measured via optical observation of high resolution digital photos. Typical loading frequency was 2 Hz, but in some cases it was properly lowered because of resonance phenomena of the hydraulic circuit. Due to this problem, the mixed mode experiments have been carried out by the SLFPB test that requires small displacement of the actuator. After some modifications to the hydraulic circuit of the machine, experiments with the MMB test have also been done and two further mode mixtures (φ = 0.25 and φ = 0.75) have been analysed. All the output files given by the MTS software have been postprocessed in Matlab® environment. A constant load ratio R = Pmin/Pmax = 0.1 was adopted. DCB and ENF fatigue tests have been carried out under load control. In order to obtain a wide interval of variation for the SERR, specimens were analysed with different initial crack lengths and/or under different load levels. For both the DCB and the ENF test under load control, the crack rate is rising with cycles up to sudden failure in proximity of the critical value of the static toughness Gc. The components of the total energy released estimated from the SLFPB data are given by the following relationships: GI = b11nλ− 3 4 Φ 2 (8) GII = b11nλ (9) −1 4 Θ 2 where: 3 nh3 Φ = λ3 8 M 9 4nh3 , Θ = λ1 8 M (10) and n= ρ +1 2 , ρ= 2b12 + b66 2 b11b22 , λ = b11 b22 (11) being M the moment (per unit width) at the crack tip and bij the terms of the generalised Hooke law. By substituting of eqs. (10) and (11) into eqs. (8) and (9) a mode mixture φ = 0.43 is obtained. To plot the fatigue plots (da/dN vs. Gmax) the crack length with cycles, a(N), and the maximum load with cycles, Pmax(N), have been recorded; the crack length is obtained from the digital photos and the load is given by the testing machine software. The experimental data of the crack length are fitted with power or exponential curves and the derivative da/dN has been calculated analytically from the fitting curve. The instant value of Gmax is evaluated from the load, Pmax(N), and the current crack length, a(N), via equations (2) and (3). In figure 6 and 7 the crack growth rate is plotted versus the maximum value of the total SERR for the tests performed. Power laws have been adopted to interpolate the data. In some cases (see for example the curve φ = 0.25), when Gmax approaches to the static toughness Gc the resulting curve becomes too steep; these points have been excluded from the interpolation procedure. Average Paris parameters for the tests are summarised in table 4 and plotted in figure 8. It is easy to notice that the two parameters change with the mode mixture in a different manner. The intercept B increases monotonically with φ while the slope m has low values in correspondence of the single fracture modes and a maximum value in proximity of φ = 0.5. -2 -1 10 10 (b) δa/δN [mm/cycle] δa/δN [mm/cycle] (a) spec 1 spec 2 spec 3 -3 10 -4 10 0.25 spec 1 spec 2 spec 3 -2 10 -3 0.5 Gmax [N/mm] 0.75 1 1.25 10 0.1 1 Gmax [N/mm] Figure 6. Crack growth rate versus Gmax for DCB tests (a), and ENF tests (b). 2 3 -2 -2 10 10 (b) spec 1 spec 2 spec 3 δa/δN [mm/cycle] δa/δN [mm/cycle] (a) -3 10 -3 10 mode mix 0.25 mode mix 0.75 -4 10 -4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2 10 1.3 1.4 1.5 0.5 0.6 0.7 Gmax [N/mm] 0.8 0.9 1 1.1 1.2 1.3 1.4 1.5 Gmax [N/mm] Figure 7. Crack growth rate versus Gmax for SLFPB tests (a), and MMB tests (b). TABLE 4. Paris parameters. Mode mixture φ 0 0.25 0.43 0.75 1 Test DCB MMB SLFPB MMB ENF Test control Load Displacement Displacement Displacement Load Paris param.B 2.4E-3 9.0E-4 3.3E-3 5.7E-3 6.7E-3 Paris param.m 0.42 3.09 4.43 3.3 0.7 Parameters B and m can be related to the mode mixture by using the curve that fits the experimental data. Due to the particular distribution of the points in the diagrams, a quadratic curve can be used for both parameters. Three constants must be fixed for the curve B(φ) and for the curve m(φ). The curve are expressed as follows: B(φ ) = − k Bφ 2 + (BII − BI + k B )φ + BI (12) m(φ ) = −k mφ + (mII − mI + k m )φ + mI 2 (13) It is to be noted that BI, mI and BII, mII are the intercept and the slope of the fatigue plots for single mode I and single mode II, respectively, whereas kB and km are given by the best fitting (see figure 8.a and 8.b) procedure of data. This best fit procedure provides: kB = -5.15E-3, km = 15.45. In the same figures 8, also models given in [15] and [16] are plotted. It is seen how the model proposed by Dahlen et al. works for the variation of the intercept B but fails for the slope m. Also the model proposed by Kenane et al. works in predicting the variation of the intercept, whereas this model is not able to describe the behaviour of the slope. 6 0.014 (a) (b) Experiments 0.012 Quadratic interp. Experiments Quadratic interp. 5 Dahlen & Springer Dahlen & Springer 0.01 Kenane & Benzeggagh 4 B m 0.008 3 0.006 2 0.004 1 0.002 0 0 0 0.2 0.4 φ 0.6 0.8 1 0 0.2 0.4 φ 0.6 0.8 Figure 8. Influence of the mode mixture φ on the intercept (a) and on the slope (b) of the Paris plot. 1 Conclusions Quasi-static and fatigue delamination experiments have been performed in this work on a glass/epoxy unidirectional composite. The material has been manufactured with the hand lay-up technique. Using different experimental configurations, single and mixed fracture modes (opening, shearing and a mix of them) have been analysed under quasi-static and fatigue loading. Taking into account the experimental results obtained, the following remarks can be here summarised. o Fracture toughness values from quasi-static tests are quite high for this material, but they can be compared with other found in literature. Resistance curves show that in mode I the energy required for the crack propagation increases with the crack length; this phenomenon doesn’t appear in mode II. o Fatigue Paris parameters (intercept and slope) that characterise the stable crack propagations depend on the mode mixture; in particular the experimental results show that the intercept increases with the mode mixture whereas the slope takes a maximum near to φ = 0.5. o A simple quadratic model can be used to describe this dependency, whereas other monotonic models found in literature fail when applied to the material analysed. Future developments of the work include the analysis of cases where the mode mixture changes during the crack propagation, in order to verify the quadratic interpolation model under more realistic loading conditions. Furthermore, a study on other composite materials is going to be performed to assess the role of fibres and matrix on the material behaviour under fatigue loading. 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