CHARACTERIZING ADHESION OF PSA TAPES USING THE SHAFT LOADED BLISTER TEST

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1 .. CHARACTERIZING ADHESION OF PSA TAPES USING THE SHAFT LOADED BLISTER TEST Emmett O'Brien Graduate Student Dept. of Chemical Engineering Virginia Tech Blacksburg, VA Shu Guo Graduate Student Dept. of Engineering Science and Mechanics Virginia Tech Blacksburg, VA Thomas C. Ward Adhesive and Sealant Council Endowed Professor Dept. of Chemistry Virginia Tech Blacksburg, VA David A. Dillard Director for Cemer for Adhesive and Sealant Science Dept. of Engineering Science and Mechanics Virginia Tech Blacksburg, VA ABSTRACT The shaft loaded blister test (SLBT) was investigated for measuring the strain energy release rate (G ) of a pressure sensitive adhesive (PSA) tape bonded to a rigid substrate. G values were calculated from three different equations: (1) the load based, (2) hybrid, and (3) displacement based. Samples consisting of stacked films: 1, 2, and 4 plies thick, were tested to determine if the backing' s tensile rigidity (Eh) had any affect on the measured G. The results suggest that the number of plies had no effect on the measured G provided that backing still behaved as a stretching membrane. Using the linear elastic model, an experimental compliance calibration was carried out, and the effective tensile rigidity, (Eh)~fr, was determined. Using the effective tensile rigidity resulted in better agreement between the Go values. G values obtained from the pull-off test were of the same order of magnitude as the SLBT. G values obtained from the 90 peel test were an order of magnitude greater than the SLBT test due to plastic deformation. It was demonstrated that the SLBT could be used in-situ to measure the strain energy release rate of PSA tapes exposed to liquid environments. Furthermore, if the PSA film behaves like a stretching membrane, Go can be calculated using the hybrid equation and only two variables: load and displacement, and the crack length is not required, which eliminates much of the experimental difficulty. 225

2 INTRODUCTION A measure of the fracture toughness of an adhesive bond is the strain energy release rate (G~) or the rate of release of energy per unit surface area created during crack growth. The strain energy release rate reflects the energy required to break interfacial bonds and the energy dissipated at the viscoelastic zone ahead of the crack tip. The expressions used to calculate G~ are typically derived using linear elastic fracture mechanics (LEFM), that is, by assuming that the adherend and adhesive are loaded within the elastic range, except locally at the crack tip, where plastic deformation occurs. In practice, adhesive systems behave viscoelastically or elastic-plastically, thus yielding often occurs. The extent of yielding depends on how much the stress (~) in the sample exceeds the yield stress (~y). For thin films, the effects of plastic deformation and yielding may be significant given the small load-bearing capacity, which is a result of small thickness, and the relatively strong adhesion. 'i We review the shaft loaded blister test proposed by K.T. Wan 10_), shown schematically in Figure 1. Experimentally similar to the pressurized blister test, a PSA tape is bonded to a substrate that has a hole in its center. The sample is mounted in a universal testing machine (UTM) and a force is then applied through the hole into the underside of the film by controlled displacement of a shaft. The resulting debond occurs axisymmetrically and a blister is formed. From three variables: the radius of debonding (a), the central shaft displacemem (w0), and load (P), Gc may be determined. P T h... I T w ~o Figure 1 Schematic of the shaft loaded blister test " 2a " SHAFT LOADED BLISTER TEST THEORY The model proposed by Wan assumes that the film undergoes pure elastic stretching, no bending occurs, and the load is approximated as a point load. For a small angle of deflection, (0), between the substrate and film the following relation is predicted: 226

3 3 rcehw = 0.5 8Pa 2 Eq. 1 Where E is the Young's tensile modulus and h is the thickness of the backing. Collectively, (Eh) is commonly referred to as the film tensile rigidity or compliance. During stable crack growth the slopes of P vs. a, P vs. w0, and w0 vs. a are linear. From the respective slope, Go can be calculated from either of the following three equations: G~- 4rc Eh Eq. 2 Load equation G~ #2-Eh, Eq. 3 Hybrid equation 4-16 Eq. 4 Displacement equation Examination of three aforementioned equations reveals that Go calculated from equation 2 depend strongly on the measured load (P), Go calculated from equation 4 depend strongly on the measured displacement (w0). Equation 3 is a hybrid of equations 2 and 4. As a consequence equations 2, 3, and 4 are referred to as the load, hybrid, and displacement equations respectively. ALTERNATIVE TEST GEOMETRIES For the 90 peel (2) test the strain energy release rate can be calculated from equation 5. P Gc-~ b Eq. 5 where b is the tape width. For the pull-off test (3) the strain energy release rate can be calculated from equation 6. 3PO G~ 8 b Eq

4 where 0 is the angle in radians between the substrate and peel arm. A schematic of the pull-off test is shown below in Figure 2. P Figure 2 Schematic of the pull-offtest KAPTON PSA TAPE Kapton polyimide film tape was used as a model PSA tape. The total thickness of the tape is 2.5 mil; the Kapton membrane thickness is 1 mil and the PSA thickness is 1.5 mils. The PSA is a silicon based thermosetting adhesive. The tensile modulus of the Kapton film was determined using ASTM D : Test Methods for Tensile Properties of Thin Plastic Sheeting. From the initial slope of the stress-strain curve Young's modulus was determined to be 3 GPa. EXPERIMENTAL SET-UP The Kapton tape was bonded to the substrate using hand pressure. Mounted on the shaft tip is a ball bearing 0.7 cm in diameter. An aluminum disk 3" in diameter with a 0.8 cm hole bored in its center served as the substrate for the blister test. The film was mounted face down in a stand, and using a mirror and a transparent ruler, the debond radius was recorded in a video camera. The load (P) vs. displacement (w0) was recorded by an Instron UTM at a shaft displacemem rate of 0.1 mm/sec. Prior to each blister test, samples were scrubbed with cotton saturated with acetone followed by an acetone rinse and air dry. The experimental set-up is shown in Figure 3. Samples tested consisted of stacked Kapton tape 1, 2, and 4 plies thick. The number of stacked films is designated as n. The only criteria each sample must meet is that the debond must occur axisymmetrically. 228

5 Stand J Shaft Film Transparent Ruler Video Camera Mirror Figure 3 Schematic of the experimental set-up of the shaft loaded blister test RESULTS AND DISCUSSION The load (P) vs. shaft displacement (w0) curves obtained directly from the UTM are shown in Figure 4 for n = 1, 2, and 4. There are three regions of interest: 1) the pre-debonding region at the beginning of the test where the blister begins to form, 2) the stable crack growth region where once a critical load (P*) is reached, the slope of P vs. w0 is linear, and 3) where edge effects occur and the load begins to drop. From the slope of the stable crack growth region, G~ may be determined using the hybrid equation (Eq. 3) n=4 A 2o z v "0 0..J lo ' / ~4r" 0 ",~~..-~ o,,, Wo (mm) Figure 4 Load (P) vs. cemral shaft displacement (w0) for n = 1, 2 and 4,

6 The crack length (a) vs. shaft displacement (wo) curves are shown in Figure 5 for n = 1, 2, and 4. The relationship is linear, which is characteristic of stable crack growth. From the slope of a vs. w0, G~ may be determined using the displacement equation (Eq. 4). During stable crack growth the slope of the load (P) vs. crack length (a) is also linear, but is not shown. From the slope of load (P) vs. crack length (a), G~ may be determined using the load equation (Eq. 2). 15 I n=l 12 n=.~., ~ -i A 9-- ~ n= 4 m I Wo (mm) Figure 5 Debonding radius (a) vs. central shaft displacemem (w0) for n = 1, 2 and 4 The calculated strain energy release rate, G, determined from the load, hybrid, and displacement equations are shown below in Table 1 for n = 1, 2, and 4. For the load equation the calculated G values are in excellent agreement for n- 1, 2 and 4. The hybrid equation shows excellent agreement between n = 1 and 2 but not 4. The displacement equation exhibits a similar trend however G values are significantly larger than those calculated by the load or hybrid equation. Table 1 Calculated strain energy release rates (G ) for n = 1, 2, and 4 using load, hybrid, and displacement equations n=l n=2 n=4 load (P/a) avg. std. dev hybrid (P/wo) avg. std. dev displacement (wo/a) avg. std. dev The discrepancies that exist for the hybrid and displacement equations are attributable to the plastic deformation at the contact zone between the shall tip and PSA tape. The theoretical model is based on an elastic, conical blister profile (Figure 1), however the actual blister profile resembles that shown in Figure 6. As a result, the measured w0 is larger than the elastic w0 (see Fig. 6), from which the G~ equations were derived from, and as a consequence the G~ determined 230

7 from the displacement equation is significantly greater than the G from the load or hybrid equation. Area of plastic deformation ~... IT Figure 6 Schematic of the actual blister profile [, i"i,i,,,,:... ",~i, ~ Wplastic WElastic Using scaling laws, the load, hybrid and displacement equations predict that the slopes of (P / a), (P / w0) and (a / w0) should scale with or should be linear with h 1/4, h 1/2, and h 1/4 or n 1/4, n 1/2, and n ~/4 respectively. Plots of the respective graphs using average slopes obtained from the group of samples are shown below in Figure 7. The graphs show that for n = 4 the scaling law fails, a result attributable to the film behaving more like a bending plate and less like a stretching film OC /,/1/4 tl( ) "E 15oo =_., e= i nl/ o0,, / I ' E z I ~ 31111O - I I o- I I 1/2 I n l I i ~--... o n Figure 7 Plots of predicted scaling laws based on load, hybrid, and displacement equations 231

8 Support for the elastic stretching membrane model can be garnered from examination of equation 1; that when linearized equation predicts that a plot of w03/p vs. a 2 is linear with a slope equal to 4/(~Eh). A plot of w03/p vs. a 2 for n = 1, 2, and 4 is shown in Figure II A Z o,t E 15- O x ~ " n=~ o 5-0 ~ ~ n= a 2 x 10 s (m 3) Figure 8 Linearized plot of equation 3, (Wo3/p) VS. a 2 for n = 1, 2, and 4 The relation is linear and from the slope of the line the effective film tensile rigidity (Eh)~er can be calculated. A comparison of the film tensile rigidity (Eh)th~o~y determined from the Young's modulus and the backing thickness and the average (Eh)~fr is shown below in Table 2. Table 2 shows that the (Eh)eff determined from equation 1, agrees well with the (Eh)theory. Table 2 Film tensile rigidity determined from ASTM D " (Eh)theory and from the slope of linearized equation 3: (Eh) fr...[...(eh)th~orr N/m n = 1 77,500 n = 2 154,900 n = 4 309,800,. (Eh)~irN/m 69,500+/-6, ,800+/- 11, ,100+/- 17,200 When using the (Eh)eff to calculate the G~, rather than the (Eh)theory, the data sets were in better agreement. This is a technique similar to that used in other test geometries, such as the double cantilever beam test, where the data is used to make an experimental compliance calibration. The results are shown below in Table 3. A comparison of Table 1 and Table 3 reveals no significant difference between G values measured using (Eh)theory and (Eh)~fr. 232

9 Table 3 Calculated strain energy release rates (Go) for n = 1, 2, and 4 using load, hybrid, and displacement equations and the effective tensile rigidity: (Eh)~fr r load (P/a) hybrid (P/w0) avg. std. dev. avg. std. dev. n = n=2 n= displacement (wo/a) avg. std. dev < The results of alternative test geometries, the pull-off test and 90 peel test, are shown below in Table 4. These tests were performed at a crack propagation rate of 10 mm/minute. The G~ determined from the pull-off test was the same order of magnitude as that obtained using the SLBT hybrid equation. The Go determined from the 90 peel test was an order of magnitude greater due to plastic deformation. Table 4. Strain energy release rates (Go) calculated from alternative test geometries. hybrid SLBT Pull-off test 90* Peel test avg. std. dev. avg. std. dev. avg. std. dev, Gc (Jim 2) These results suggest that the calculated Go is of reasonable magnitude and that there is no advantage to measuring the crack length (a). If only the load and central displacement are needed then G~ can be calculated using the hybrid equation and the experiment is very simple. Furthermore, the measured Go appears to be independent of the backing material, provided the tape behaves like a stretching membrane. EFFECTS OF LIQUIDS AT THE INTERFACE The affect of liquid at the imerface on the measured strain energy release rate was investigated by placing methanol-water solutions of a varying methanol concentration (0, 40, 60, 80, and 100 wt. %) in the recess formed between the PSA tape and substrate. A schematic of the experimental set up is shown in Figure 9. The load (P) vs. displacement (w0) curves are shown in Figure 10. As the concentration of methanol increases the critical load where debonding begins (P*) and the slope of P vs. w0 decreases. This test geometry is advantageous because the ingression of the solvent occurs perpendicular to the debond and directly at the interface. Using the hybrid equation the resulting G values are listed in Table

10 Liquid in recess Ill II Ill Figure 9 Schematic of the experimental set-up used to make in-situ measure of liquid influence the strain energy release rate 20 t Increasing methanol content 15-!1 ~ ~. ~" neat 4-- water --40% -~ 60% -a-- 80% --P- 100% wo (mm) Figure 10 Load (P) vs. central shaft displacemem (w0) for various concentrations of methanol in water (0, 40, 60, 80, 100 wt. %) Table 5. Strain energy rates (G ) calculated from hybrid equation for single ply of Kapton Tape with various concentrations of methanol in water (0, 40, 60, 80, 100 wt. %) hybrid (P/w o) sam pie Gc (Jim neat 36.0 water % % O% % 6.9 2) 234

11 CONCLUSIONS The linear elastic fracture mechanics approach developed by K. T. Wan was applied to a Kapton Tape PSA. The experimental set-up for studying the effects of liquids on the fracture energy has been demonstrated. These results indicate that the shatt loaded blister test is an attractive and convenient test method for measuring the strain energy release rate of PSA tapes. REFERENCES 1. K.T. Wan and Yiu-Wing Mai, International Journal of Fracture, 74, (1995) 2. Kinloch, A. J., Lau, C. C. and Williams, J. G. International Journal of Fracture, 66, (1994) 3. Gent, A. N., Kaang, S., Journal of Applied Polymer Science, 32, (1986) 235

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