An experimental partitioning of the mechanical energy expended during peel testing

Peeling of polyimide coatings bonded to aluminum substrates was analyzed from a thermodynamic perspective with the intent of determining how the energy expended in separating the bonded materials is consumed. The mechanical work expended and the heat dissipated during peeling were simultaneously measured using deformation calorimetry. The surfaces exposed by peeling were analyzed by electron microscopy and electron spectroscopy. The thermodynamics of tensile drawing for polyimide were studied using deformation calorimetry and thermomechanical analysis. When polyimide coatings were peeled from aluminum substrates at a peel angle of 180°, almost all of the mechanical energy was consumed in propagating the bend through the coating being peeled. The fraction of peel energy dissipated as heat was 48 ± 1.3% and nearly all of the remainder was stored as latent internal energy in the peeled polyimide. When the bend is propagated through aluminum, which has a limited capacity to store latent internal energy, 97-100% of the mechanical energy is dissipated as heat.     

Study of a 'T'-type peel test on a metal/polymer/metal sheet sandwich

This paper describes the specific 'T'-type peel mode in the case of a metal/polymer/metal sheet sandwich and gives experimental results on the influence of plastic deformation in the metallic substrates on the peel energy. We propose an experimental method of carefully determining the peel energy of a metal-polymer interface in a sandwich structure. Based on the mechanical properties of the stainless steel substrates and the maximum curvature of the metallic sheet measured experimentally during the peel test, several expressions for the clastoplastic deformation energy of the metal substrates are given. It is noteworthy that the curvature of the metal substrate layers depends not only on the mechanical properties of the material, but also on the work necessary to overcome the interfacial or cohesive forces. It is shown that even for thin metallic substrates (0.1 mm thick stainless steel), the work absorbed by the deformation represents roughly 50% of the total measured energy. During peeling the same specimen at different rates, the propagation peel force is higher or lower than the initiation force depending on the previous curvature of the metal sheets.     

Experimental determination of the peel adhesion strength for metallic foils

This work addresses the problem of experimental measurement of peel adhesion in cases where a non-recoverable (plastic) deformation energy of the peeled foil, plus frictional losses, constitutes a significant portion of the total peel energy. In standard tests, when the true adhesion strength is desired, the plastic energy has to be calculated and deducted from the total energy. Several studies have been dedicated to the modelling and calculation of the energy dissipated through plastic deformation so that the net adhesion energy could be deduced. These calculations are cumbersome and impractical for general use. A simple experimental technique for the determination of the net adhesion strength is proposed. Experimental results with ～ 0.1 mm thick foils of stainless steel, nickel, and titanium confirm the theoretical predictions regarding the energy balance during peeling. Using the proposed methodology, there is no need to calculate or otherwise determine the deformation energy losses of the peeled foil or the frictional dissipation. The method is not limited to a particular material and can be used successfully for strain hardening plastic as well as metallic foils. Peel tests on adhesively bonded specimens of stainless steel and nickel and of a thermal spray-coated Ti alloy foil were carried out to demonstrate the applicability of the proposed method.     

An Elasto-Plastic Investigation of the Peel Test

This work outlines an elasto-plastic investigation of two common peel tests which use high and low yield strength aluminium adherends. An elastic, large-displacement, finite element program has been extended to include elasto-plastic material behaviour. This has been used to analyse both peel tests. The adhesive stresses near the crack tip have been shown to be finite while the corresponding strains remain singular. A failure criterion based on a maximum adhesive strain has been used to predict the relative strengths of the peel test. The amount of energy dissipated in the plastic deformation of the peeling adherends has been assessed by a series of tests and has been shown to be a considerable amount of the total energy supplied to the peeling system. Further, although the two aluminium alloys considered have grossly different yield strengths the energies dissipated in plastic deformation are similar. Material data for the finite element analysis and the plastic work calculations have been obtained from uniaxial tensile tests of both the adherends and the adhesive and actual peel strengths have been measured in a series of peel tests.     

An Elasto-Plastic Investigation of the Peel Test

This work outlines an elasto-plastic investigation of two common peel tests which use high and low yield strength aluminium adherends. An elastic, large-displacement, finite element program has been extended to include elasto-plastic material behaviour. This has been used to analyse both peel tests. The adhesive stresses near the crack tip have been shown to be finite while the corresponding strains remain singular. A failure criterion based on a maximum adhesive strain has been used to predict the relative strengths of the peel test. The amount of energy dissipated in the plastic deformation of the peeling adherends has been assessed by a series of tests and has been shown to be a considerable amount of the total energy supplied to the peeling system. Further, although the two aluminium alloys considered have grossly different yield strengths the energies dissipated in plastic deformation are similar. Material data for the finite element analysis and the plastic work calculations have been obtained from uniaxial tensile tests of both the adherends and the adhesive and actual peel strengths have been measured in a series of peel tests.     

Adhesion of Polyethylene to Metals: The Role of Surface Topography

Previous work established the importance of the fibrous substrate topography in obtaining good adhesion of polyethylene to matt black oxide films formed on copper in alkaline solution. In this paper the effect of the very rough surface topography is shown to be general. Anodising treatments for copper and zinc and a high temperature oxidation for steel are described which give a very rough surface consisting (respectively) of fibrous, dendritic and blade-like growths. The peel strength of polyethylene to these substrates is high even under circumstances, for example when the polymer is stabilised with anti-oxidant, where adhesion to a chemically similar smooth surface is low. The high peel strength is associated with large amounts of energy being dissipated during peeling in plastic deformation of the polymer near the interface. It is suggested that this is caused by the development of high shear stress concentration at the fibre ends causing yielding in a large volume of polymer.     

Determination of Quasiequilibrium Work of Adhesion of Elastic Coatings

Present methods for the determination of adhesion bonding of elastic polymeric materials entail certain experimental difficulties. In particular, the necessity of strict centering of the test specimen, and the difficulty associated with application of a homogeneously distributed stress over the whole cross-sectional area (homogeneous detachment or shear), or the excessive expenditure of work resulting from polymer deformation (peel).^1,2

We are suggesting a method to determine the quasi-equilibrium work of adhesion during the peeling process for elastic polymeric coatings, the value of which, as was demonstrated experimentally, does not depend on the coating thickness, deformation or rate of peeling.     

Application of the Island Blister Test for Thin Film Adhesion Measurement

The island blister test has recently been proposed as an adhesion test which allows the peel of thin, well-adhered films without exceeding the tensile strength of the film. The island blister test site is a modification of the standard blister test site, consisting of a suspended membrane of film with an “island” of substrate at the film center. The membrane support and island are secured to a rigid plate and the film is pressurized, peeling the film inward off the island. A model for this inward or “annular” peel indicates that even for systems of good adhesion, peel can be initiated at low enough pressures to prevent film failure by making the center island sufficiently small relative to the size of the film.

We have fabricated island blister test sites using micromachining techniques and have used them to measure the debond energy of polymer films on various substrates. The peel data obtained from these island sites match well to the behavior predicted by a simple fracture mechanics analysis. This paper reports the fabrication of the island test sites, the experimental verification of the test, and the results of application of the test to polyimide films on metallic and polymeric substrates.     

Application of the Island Blister Test for Thin Film Adhesion Measurement

The island blister test has recently been proposed as an adhesion test which allows the peel of thin, well-adhered films without exceeding the tensile strength of the film. The island blister test site is a modification of the standard blister test site, consisting of a suspended membrane of film with an “island” of substrate at the film center. The membrane support and island are secured to a rigid plate and the film is pressurized, peeling the film inward off the island. A model for this inward or “annular” peel indicates that even for systems of good adhesion, peel can be initiated at low enough pressures to prevent film failure by making the center island sufficiently small relative to the size of the film.

We have fabricated island blister test sites using micromachining techniques and have used them to measure the debond energy of polymer films on various substrates. The peel data obtained from these island sites match well to the behavior predicted by a simple fracture mechanics analysis. This paper reports the fabrication of the island test sites, the experimental verification of the test, and the results of application of the test to polyimide films on metallic and polymeric substrates.     

Interfacial and Bulk Contributions to Peeling Energy

Thin polyurethane films, having low adhesion to dried protein, were developed as candidate materials for non-adhesive surgical dressings. In order to model wound-adhesion, gelatine was cast from solution on to the film and allowed to dry. The film was peeled from the gelatine at 180° peel angle, and the peel force measured as a function of the temperature of test. The dynamic mechanical properties of the films were measured over the range -90°C to 110°C and values of tan δ were determined at the temperatures employed for peeling. Thus, a correlation was obtained between peeling energy and tan δ for each of eight films.

The generalised theory of fracture mechanics states that the adhesive failure energy is given by the product of an interfacial energy term and a “loss function” involving the hysteresis ratio of the material. If the strains are small the hysteresis ratio is proportional to tan δ. The experimental results show excellent agreement with the theory, but the interfacial term turns out to be much greater than the true interfacial energy (or thermo-dynamic work of adhesion). The reason for this result is discussed.     

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.     

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.     

On using a penalty-based cohesive-zone finite element approach,Part II: Inelastic peeling of an epoxy-bonded aluminum strip

Previous work has demonstrated the use of a penalty methodology for enhancing the use of cohesive-zone elements to simulate double cantilever beam (DCB) and flexible-arm peeling problems, both involving elastic arm deformation. This approach is extended to the general case of inelastic peel arm deformations. Refinements to the original penalty selection methodology are included to account for the influence of plasticity in the peel arms. Accuracy of the method is demonstrated by comparing simulation results to experimental data of epoxy-bonded aluminum arms being peeled at different angles from a rigid substrate. This work addresses significant complexities in the analysis that arise due to the inelastic deformation of the aluminum peel arms.     

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.     

The Effect of Bubbles at the Interface on the Adhesion of Polyethylene to Metals

By use of a blowing agent bubbles of a few hundred microns diameter were introduced at the interface of copper and steel substrates coated with low density polyethylene. The presence of the bubbles leads to an improvement in peel strength. An explanation is put forward in terms of a suggested stress perturbation produced by the bubbles which leaves the interface itself relatively lowly stressed and leads to the expenditure of work in plastic deformation of the polymer away from the interface. Support for the explanation was obtained by photoelastic study of a model system and by scanning electron microscopy of the peeled surfaces.     

Cohesive zone models and the plastically deforming peel test

The peel test is a popular test method for measuring the peeling energy between flexible laminates. However, when plastic deformation occurs in the peel arm(s) the determination of the true adhesive fracture energy, G c , from the measured peel load is far from straightforward. Two different methods of approaching this problem have been reported in recently published papers, namely: (a) a simple linear-elastic stiffness approach, and (b) a critical, limiting maximum stress, σ max , approach. In the present article, these approaches will be explored and contrasted. Our aims include trying to identify the physical meaning, if any, of the parameter σ max and deciding which is the better approach for defining fracture when suitable definitive experiments are undertaken. Cohesive zone models Fracture mechanics Laminates Peel tests Plastic deformation     

Temperature and humidity effects on adhesion of polyimide film to a silicon substrate

A 90° peel tester with substrate heating capability was built to evaluate the adhesion strength of polyimide films to a silicon substrate. The effects of polyimide film thickness and peel rate on polyimide adhesion to a silicon substrate under high or low humidity, and at elevated temperatures, have been evaluated. In a high humidity environment, a low peel strength was measured. The influence of moisture on the peel strength increases with decreasing peel rate. Peeling at elevated temperature reduces the moisture effect even under high humidity conditions. Using a low peel rate in a high humidity environment, the measured peel strength showed a maximum as the polyimide film thickness increased. No striations in peeled polyimide films were observed for peeling in a high humidity environment.     

Wave Phenomena in Low Angle Peeling

The angular dependence of peeling has been investigated over a wide range of peel angles for a rubber strip peeled from glass. At low peel angles the peel front becomes “V”-shaped, wave phenomena are often observed and the peel energy can increase by an order of magnitude or more. A tentative theory, which appears to give the correct magnitude in a worked example, is advanced to account for the energy increase. The influence of factors such as electrostatic charge, deformation and rate on the observed phenomena are discussed.     

Changes in the Peeled Surfaces of Copper Thin Films Deposited on Polyimide Substrates After Heat Treatment

Peel strength between a copper (Cu) thin film and a polyimide (pyromellitic dianhydride-oxydianiline, or PMDA-ODA) substrate is reduced by heat treatment at 150°C in air. In this work, we investigated the peel strength, the morphology of the interface between Cu films and polyimide substrates using optical microscopy and electron microscopy, and chemical change of the interface using Auger electron spectroscopy (AES) and micro X-ray photoelectron spectroscopy (XPS). The analysis showed that CuO “lumps” were present on the peeled surface of PMDA-ODA after heat treatment at 150°C in air. The peeled surfaces of other polyimide substrates were also analyzed: biphenyl dianhydride-para phenylene diamine (BPDA-PDA) and biphenyl dianhydride-oxydianiline (BPDA-ODA). CuO lumps were present on the peeled surface of BPDA-ODA after the heat treatment, but not that of BPDA-PDA. Compared with the adhesion strength for the Cu thin film, the adhesion strength was high for the Cu/PMDA-ODA and Cu/BPDA-ODA laminates, but the adhesion strength was very low for the Cu/BPDA-PDA laminate. This low strength is the reason that CuO lumps were not detected on the peeled surface of the BPDA-PDA substrate. These CuO lumps were related to the adhesion degradation of the Cu/polyimide laminates after the heat treatment.     

Interfacial Friction in Filled Polymers Initiated by Adhesive Debonding

When a rubber is subjected to stress-strain cycles, a part of the energy of deformation is dissipated as heat. This effect is called hysteresis. I t has been recognized for years that hysteresis in filled rubbers is a complicated phenomenon comprising different mechanisms. The overall loss of energy in the strain cycle has been shown to be the sum of irrecoverable and recoverable (repeatable) dissipative processes.¹ The first process, known as the Mullins effect, represents a total action of several irreversible damage mechanisms, rubber-filler detachment being possibly the most important one in highly loaded elastomers.^2-5 The second process accounts for polymeric internal viscosity and some interfacial phenomena that probably could be treated as interfacial friction of damaged microstructural elements. There are also other dissipative sources of minor importance that will not be considered in this paper.