Effect of Peel Angle Upon Peel Force

Measurements of peel force P per unit width are reported for samples of three adhesive tapes, adhering to two different substrates. In all cases, the work of detachment per unit area of bonded interface was found to depend upon the angle θ of detachment, increasing as θ increases. This effect is attributed to dissipation of energy in bending the tape away from the substrate at the line of detachment, to a greater degree as θ increases. Extrapolation to θ = 0 is suggested as a simple way of minimizing contributions to the observed work of detachment that arise from bending an imperfectly-elastic adhering layer as it is peeled away from a flat rigid substrate. But at small peel angles the tape tends to stretch appreciably. Peeling at 45° is recommended to minimize both effects.     

New and Improved Tests for Adhesion

Three new methods are discussed for measuring the work G_a, required to detach unit area of an adhering material from a substrate. The first is a simple modification of the Outwater double-torsion test for long rectangular plates, bonded together. This method is suitable for evaluating aluminum-epoxy bonds, for example, or the transverse strength of fibrous composites. The second is a pull-off test for long strips adhering to a rigid surface. It seems suitable for adhesive tapes and laminates. The third is a reconsideration of the “blister” test for films and coatings, in which a circular debond at the interface is made to grow by internal pressure. The relation obtained between pull-off force F for a strip, or blow-off pressure P for a layer, takes the unusual form:

F⁴ (or P⁴) ∞ KG³_a

where K is the tensile stiffness of the detaching layer. This dependence arises from the non-linear (cubic) relation between load or pressure and deflection in these configurations. Nevertheless, the product Fθ, where θ is the angle of detachment of a strip, or Py, where y is the height of a “blister”, give direct measures of the strength of adhesion G_a, independent of the stiffness of the adhering material and of the extent of detachment.     

Peel mechanics of adhesive joints

A review is given of the mechanics of peeling rupture of an adhesive joint, consisting of a flexible adhering strip peled away from a layer of adhesive. Attention is drawn to a number of anomalous results that cannot be accounted for solely, in terms of the thermodynamic work of formation of two new surfaces. The work of detachment is found to be generally much larger than the theoretically-predicted amount. Moreover, the value obtained is greater for thicker layers of adhesive, and for detachment at a peel angle of 180° rather than at 90°. Also, it is found to increase with increasing thickness of the adhering strip, passing through a maximum value in some cases and then decreasing as the strip thickness is increased still further. All of these effects are attributed to dissipative processes, for example, plastic yielding, in one or both of the adhering layers as they are peeled apart. Some quantitative relationships are given for the additional peel forces arising from plastic yielding of the adherend or the adhesive.     

Evaluation of the Constrained Blister Test for Measuring Adhesion

The constrained blister test (CBT) was evaluated as a method for measuring adhesion using a model system, electrical tape bonded to polystyrene. Pressure is applied through a circular inlet hole in the substrate, causing the adhesive to “blister” up and peel radially away from the substrate. A glass constraint, placed some distance above the adhesive, limits deformation of the adhesive in the vertical direction and promotes radial peel. By operating at low spacer height (the distance of the constraint above the adhesive) and very low growth rates, the energy spent for deformation of the adhesive and viscoelastic dissipation is minimized. Blister radial growth was linear with time, and growth rate increased linearly with the second power of the energy input. An intrinsic, rate-independent adhesion energy was obtained by extrapolation to zero crack growth rate. The CBT was compared with two peel tests. The dependence of the growth rate on energy input was different, but the extrapolation to zero growth rate gave the same value of the intrinsic adhesion energy.     

Quantifying the Relationship Between Peel and Rheology for Pressure Sensitive Adhesives

An attempt is made in this work to model quantitatively the peel force vs. rate behavior of a pressure sensitive adhesive (PSA) tape. The approach follows suggestions of previous authors in modeling the deformation of the PSA as uniaxial extension of individual strands. A debonding failure criterion based on stored elastic energy density is used. In this work, experimental measurements of dynamic mechanical master curves are used to provide the mechanical properties of the PSA in the model. The predictions are compared with experimental peel force vs. rate master curves on tapes made from those same adhesives. The only adjustable parameter for the fitting is the quantity related to the debonding criterion. In this set of natural-rubber-based PSAs, the general shape of the peel master curve and the changes in peel behavior associated with tackifier loading and rubber molecular weight are well explained by the model. The effect of changes in substrate chemistry are not well explained.     

Peel and shear strength of pressure‐sensitive adhesives prepared from epoxidized natural rubber

Peel and shear strength of two grades of epoxidized natural rubber (ENR 25 and ENR 50)‐based pressure‐sensitive adhesive was studied. Coumarone‐indene resin was used as the tackifier, whereas toluene was chosen as the solvent throughout the experiment. The tackifier loading was varied from 0 to 80 parts per hundred parts of rubber (phr). A SHEEN hand coater was used to coat the adhesive on substrate to give a coating thickness of 30, 60, 90, and 120 μm. Peel strength and shear strength of the adhesive were determined by using a Lloyd adhesion tester and Texture analyzer, respectively. Results show that maximum peel strength occurs at 40 phr of coumarone‐indene resin for both ENRs studied an observation, which is attributed to the maximum wettability of the substrate. However, the shear strength shows a gradual decrease with increasing tackifier loading because of the decrease in cohesive strength of adhesive. ENR 25 consistently indicates higher peel strength and shear strength than ENR 50. Generally, peel and shear strength increases with coating thickness. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007.     

Theory and Analysis of Peel Adhesion: Adhesive Thickness Effects

The existing assumptions concerning boundary stress concentrations in peel adhesion are extended to treat the effects of adhesive thickness. In adhesive bonds involving the all-angle peeling of a flexible elastic adherend from a rigid substrate the varying of adhesive thickness is shown theoretically to predict a proportional increase of peel force (P) with adhesive interlayer thickness (a) when the product (βCa) of the cleavage stress concentration β, cavitation scale factor C, and adhesive thickness a is less than unity. When the product (βCa) becomes greater than unity the new theory predicts that cleavage stresses concentrate within a fractional layer of the total adhesive thickness f(a) and the peel force P tends to achieve a constant value P_max. This new theory is verified by experimental studies and the experimental analysis suggests new optimizations in the design and measurement of the peel adhesive bond.     

Evaluation of pressure-sensitive tape adhesion and backing directionality by excimer laser methods

The effects of 248 nm KrF excimer laser irradiation on a pressure-sensitive adhesive tape bonded to a glass substrate were investigated as a possible method to evaluate the quality of adhesion, as well as the directionality induced during manufacture. The model pressure-sensitive tape consisted of biaxially-oriented polypropylene (PP) tape coated with a hot-melt rubber resin. Analysis of the front-shot experiments, which were performed by irradiation through the PP backing, allowed correlation between the excimer laser irradiation-induced detachment and the peel adhesion strength. For this purpose, peel tests were performed before and after laser shots. The directionality induced during manufacture resulted in a more ablated area in the strength direction than in the transverse direction when the bonded tapes were irradiated with an elliptically-shaped laser beam above the ablation threshold. A correlation was found between the detachment bubbles created by irradiation below the ablation threshold and their respective peel adhesion values, which allows us to evaluate the quality of adhesion for pressure-sensitive tapes. Thus, a method to evaluate the quality of adhesion using an excimer laser is proposed based on the findings of this work.     

Calorimetric Measurements of The Heat Generated by The Peel Adhesion Test

The peel test is a simple mechanical test commonly used to measure the adhesion of flexible films bonded to rigid substrates. When the film is deformed elastically during peeling, the peel force is a direct measure of the strength of the interface. However, when plastic deformation takes place, the work of detachment is much larger than the thermodynamic work of forming the fracture surfaces. Simultaneous mechanical and calorimetric measurements of the work of detachment and the heat generated during the peeling of polymeric films from metal substrates and metal films from polymeric substrates have been made. An energy balance for peeling has been proposed. Most of the work of peeling was consumed by plastic deformation. The peeled polymer dissipated approximately one half of the work of peeling as heat and most of the remainder was stored in the peeled material. The peeled metal dissipated most of the work of peeling as heat.     

Comparison of Peel Tests for Metal-Polymer Laminates for Aerospace Applications

Standard peel tests for aerospace laminates based on metal-polymer systems, namely floating-roller and climbing-drum peel methods, have been accommodated in a unified theory of peeling. This theory also accommodates more basic peel tests such as T-peel and fixed-arm peel and also newer methods such as mandrel peel. These five methods have been applied to two aerospace laminate systems to critically examine their use in the determination of adhesive strength. The theory has been used to unify the outputs from the tests in terms of adhesive fracture toughness. In this way, the comparative merits of the methods can be commented on.

The validity of the standard methods has been put in doubt because of the absence of a correction for plastic bending energy and also because of the poor conformance of the peel arm to the roller system used in these methods. The unified theory and some measurements of peel-arm curvature help but not completely overcome some of these difficulties.

A further complication that arises in peel is a change in the plane of fracture. This reflects a transition from cohesive fracture in the adhesive to an adhesive fracture at the interfaces among adhesive, primer, and substrate. It is likely that such plane-of-fracture phenomena are intrinsic to evaluation of the laminate and that contemplation of cohesive fracture toughness for the adhesive cannot accommodate such events.     

Peel strength improvement of foam core sandwich beams by epoxy resin impregnation on the foam surface

The interfacial adhesion characteristics between foam cores and faces affect much the structural integrity of foam core sandwich structures. The peel strength between the face plate and the foam core is one of the appropriate parameters for the interfacial characteristics of sandwich structures and its peel energy is also measured for the interfacial characterization. The peel strength is the first peak force per unit width of bondline required to produce progressive separation, and the peel energy is the amount of energy per unit bonding area associated with a crack opening. In this study, to improve the peel strength between the foam core and the face plate of foam core sandwich beams, the surfaces of foam core sandwich beams were resin-impregnated. Then the peel strength as well as peel energy of resin impregnated polyurethane foam core sandwich beams were measured by the cleavage peel test and compared with those of the same sandwich beams without surface resin impregnation on the foam surface.     

Protocols for the Measurement of Adhesive Fracture Toughness by Peel Tests

This article reports on the work of the European Structural Integrity Society Technical Committee 4 (ESIS TC4) and its activities in the development of test protocols for peel fracture. Thirteen laboratories have been working on peel test methods in ESIS TC4 since 1997 and their activities are ongoing.

The aim of the work is to develop robust and credible test methods for the determination of adhesive fracture toughness by peel tests. Several geometric configurations have been used, namely, multi-angle fixed arm peel, T-peel, and roller assisted peel in the form of a mandrel test.

The starting point of their work is an established analysis of a peel method that is often developed from a global energy approach. The adopted analysis is combined with an experimental approach in order to resolve ambiguities in the determination of adhesive fracture toughness (G_A). The test methods involve the measurement of peel strength in order to calculate the total input energy for peel (G) and the calculation of the plastic bending energy (G_P) during peel. The latter is often obtained from a measurement of the tensile behaviour of the peel arm. Adhesive fracture toughness is then G - G_P.

Four ESIS TC4 projects are described. The first relates to fixed arm peel whilst the second and third involve both fixed arm and T-peel. The fourth project combines mandrel peel and fixed arm peel. Each project uses different types of polymeric adhesives in the form of quite different laminate systems. The selection of the laminate system enables all characteristics of laminate property to be embraced, for example, thin and thick adhesive layers, polymeric, and metallic peel arms and a range of flexibility in the laminates.

The development of the enabling science required to establish the test protocols is described and software for conducting all calculations is referenced.     

The Mechanical Behaviour of Polyimide/Copper Laminates Part 2: Peel Energy Measurements

The mechanical peel behaviour of laminates consisting of polyimide films adhered to copper foil using a modified acrylic adhesive has been studied over a wide range of test rates and temperatures. The laminates were prepared from polyimide films which had been subjected to either a “high-thermal history” or a “low-thermal history” treatment during the production of the film. The measured peel energies of the laminates could be superimposed to give a master curve of peel energy versus the reduced rate of peel test, Ra_T, where R is the rate of peel test and a_T is the time-temperature shift factor. The appropriate shift factors were a function of the test temperature and were mainly deduced from tensile tests conducted on the bulk adhesive. The “high-thermal history” laminates gave higher peel energies and the locus of failure of the laminates was mainly by cohesive fracture through the adhesive layer. At low values of log₁₀ Ra_T, i.e. Low rates of peel and high test temperatures, the “low-thermal history” laminates also failed in the adhesive layer and possessed similar peel energies to those measured for the “high-thermal history” laminates. However, at high log₁₀ Ra_T values, the peel energies measured for the “low-thermal history” laminates were lower and showed a wider scatter. These arose from a different locus of failure occurring in these “low-thermal history” laminates when tested under these conditions. Namely, it was found that most of these laminates failed in a weak boundary layer in the outer regions of the “low-thermal history” polyimide film.     

Bonding of Natural Rubber to Steel: Surface Roughness and Interlayer Structure

This paper is concerned with two aspects of the adhesion produced by the vulcanisation bonding of a simple natural rubber (N.R.) compound to mild steel. Adhesion was measured using a 45° peel test.

When the N.R. was bonded, using a proprietary bonding agent (Chemlok 205/220), to 'smooth' steel (acid etched) or to 'rough' steel (phosphated) high values of peel energy (≥ 4.5 kJm^-2), and good environmental resistance to water were obtained, with failure cohesive largely within the rubber. The highest values of peel energy (≈ 7.5 kJm^-2) were associated with a phosphated surface which consisted of plate-like crystals which directed the stresses away from the substrate in a way which produced a failure surface within the rubber which showed extensive tearing and cracking.

The nature of the layer formed in the interfacial region by interaction between bonding system and rubber was investigated using a chlorinated rubber as a 'model compound' representing the adhesive and uncompounded N.R. to represent the rubber. When a blend of the two was heated in air at 150°C, evidence was found of a solid state chemical reaction in which carbonyl groups were incorporated into the blend which became visually homogeneous. Further evidence points to the relevance of this change to adhesion in rubber-to-metal bonding.     

On the importance of some surface and interface characteristics in the formation of the properties of adhesive joints

The importance of some relative surface characteristics which determines the strength of adhesive joints: specific surface of substrate , relative contact area β and specific contact area β in the adhesion interaction process were emphasised. Existing and potential methods of experimental evaluation of these characteristics were shortly analysed. The durability of the adhesive joints in water media significantly increases with growth of specific surface ^* of chemically treated substrate evaluated from the SEM micrographs. Specific surface calculated from the experimental data of hexane adsorption measurements for iron particles (particulate model of steel substrate) is more then ten times greater than respective ^* values. The relative contact area β of the Al₂O₃ particles (in wide range of ) with PE melt was in a roundabout way evaluated by experimental determination of the affect of on kinetic of peel strength formation of adhesive joints: Al₂O₃ filled PE-steel. The speculation was based on the ability of Al₂O₃ to adsorb low-molecular products of contact oxidation of PE which takes place in the process of formation of adhesive joints and determines their strength. The ability of sorption in its turn is proportional to efficient value of β. The availability of the Al₂O₃ surface was evaluated.     

Effects of Surface Modifications on the Peel Strength of Copper Based Polymer/Metal Interfaces with Characteristic Morphologies

This paper summarizes a study on the effect of changes in surface chemistry on the peel strength of copper/polymer interfaces. Two different surface topographics were created and evaluated, one produced by cleaning and etching in sodium persulfate, the other by etching then mechanically roughening using 180 grit sandpaper. Both surfaces were then oxidized in an alkaline/oxidizing treatment to form cupric oxide. Ion implantation and benzotriazole priming modified the surface chemistry of the cupric oxide samples. After lamination to form an epoxy/copper interface, peel strength measurements were taken. The results showed that ion implantation degraded the peel strength while priming with benzotriazole improved the peel strength compared with the unmodified cupric oxide. In a separate comparison study, peel strength measurements were taken on interfaces formed from copper oxides with the same oxide structure but with widely different gross morphologies, “As laminated” adhesive strength was virtually the same. The bonded interfaces were aged at elevated temperature and the peel strength obeyed first order degradation kinetics. Two terms can be determined from the degradation studies, the first is the long term peel strength, A(∞), and the other is Ω, the degradation rate with units of time^-1. A value of A(∞) was 3.0 lbs/in for etched copper interfaces while A(∞) was 0.5 lbs/in for the sanded interfaces.     

A New Approach to the Copper/Epoxy Joint Using Atmospheric Pressure Glow Discharge

A new approach for adhering copper to an epoxy resin was studied. In this new approach, the copper surface was first treated with hydrogen plasma generated by the atmospheric pressure glow (APG) discharge. Then a thin film of γ-aminopropyltriethoxysilane (γ-APS) was formed on the treated copper surface. The copper oxide formed by air on the copper surface deteriorated the adhesion by forming a weak boundary layer, part of which could separate from the surface. This oxide layer was reduced when an APG hydrogen plasma was applied for a couple of minutes at a frequency of 13.56 MHz and a power input of 200 W. The resulting peel strength at the copper/epoxy interface increased up to ca. 0.9 Kg/cm. Curing temperature of γ-APS was also an important factor in obtaining good adhesion at the copper/epoxy interface, with the highest value of peel strength occurring at a curing temperature of 120°C.     

Protocols for the Measurement of Adhesive Fracture Toughness by Peel Tests

This article reports on the work of the European Structural Integrity Society Technical Committee 4 (ESIS TC4) and its activities in the development of test protocols for peel fracture. Thirteen laboratories have been working on peel test methods in ESIS TC4 since 1997 and their activities are ongoing.

The aim of the work is to develop robust and credible test methods for the determination of adhesive fracture toughness by peel tests. Several geometric configurations have been used, namely, multi-angle fixed arm peel, T-peel, and roller assisted peel in the form of a mandrel test.

The starting point of their work is an established analysis of a peel method that is often developed from a global energy approach. The adopted analysis is combined with an experimental approach in order to resolve ambiguities in the determination of adhesive fracture toughness (G _A ). The test methods involve the measurement of peel strength in order to calculate the total input energy for peel (G) and the calculation of the plastic bending energy (G _P ) during peel. The latter is often obtained from a measurement of the tensile behaviour of the peel arm. Adhesive fracture toughness is then G – G _P .

Four ESIS TC4 projects are described. The first relates to fixed arm peel whilst the second and third involve both fixed arm and T-peel. The fourth project combines mandrel peel and fixed arm peel. Each project uses different types of polymeric adhesives in the form of quite different laminate systems. The selection of the laminate system enables all characteristics of laminate property to be embraced, for example, thin and thick adhesive layers, polymeric, and metallic peel arms and a range of flexibility in the laminates.

The development of the enabling science required to establish the test protocols is described and software for conducting all calculations is referenced.     

Polymer Viscoelasticity: Relation to Peel Strength in Structural Adhesives

The two tests of most importance in evaluating structural adhesives for metals are (1) lap shear strength and (2) peel strength. Epoxies perform well in the first due to high tensile and shear strength. They are poor in the second unless modified to reduce brittleness. We have developed a urethane modified epoxy for this purpose. By taking climbing drum peel data in which both the temperature and the peel rate are varied, the time-temperature superposition principle can be tested. This principle is most generally applicable to thermoplastic materials between T_θ and T_θ + 100 °C (T_θ = glass transition temperature), and serves as a measure of viscoelastic response in the polymer. First, good agreement was found for a thermoplastic adhesive (PE-AA film). This was done to verify that climbing drum peel data can be used in this manner. Next, data were taken for our urethane modified epoxy. Results showed adherence to the superposition principle only above the heat distortion temperature of the cured polymer. These results indicate, among other things, that our point of failure upon peeling is within the body of the adhesive rather than within a urethane-rich layer at the metal-adhesive interface.     

THE DEVELOPMENT OF A MANDREL PEEL TEST FOR THE MEASUREMENT OF ADHESIVE FRACTURE TOUGHNESS OF EPOXY-METAL LAMINATES

A mandrel peel test is established for measuring the adhesive fracture toughness of a metal/rubber-toughened epoxy laminate system. By adopting an energy balance analysis it is possible to determine directly both adhesive fracture toughness and plastic work in bending the peel arm around the mandrel. The suitability of the procedure is examined for various types of metal peel arms, which are classified in terms of their ability to deform plastically during the test. The plastic work is also predicted theoretically, and comparisons are made between the measured and calculated values. The fracture energies determined from the mandrel tests are compared with those obtained from 90° fixed-arm peel tests. For the calculations of plastic work in bending in the fixed arm test, various options are used when modelling the tensile stress-strain behaviour of the peel arm material. In addition, the adhesive layer thickness is considered in terms of its influence on the calculation of adhesive fracture toughness.