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.     

Critical and Subcritical Adhesion Measurements of a Model Epoxy Coating Exposed to Moisture Using the Shaft-Loaded Blister Test

The shaft-loaded blister test (SLBT) was used to investigate the adhesion between a model epoxy coating and a silicon oxide surface as a function of relative humidity. Critical and subcritical strain energy release rates were measured using specimens that incorporate reinforcing layers of Kapton® film. A simplified procedure that eliminates the need for video imaging to measure the blister radius and fracture energy was developed. A critical relative humidity level for adhesion loss was observed, in agreement with measurements that have been made previously in a number of polymeric systems. The SLBT was confirmed to be particularly attractive for fracture energy measurements on thin, strongly adhered coatings and films which otherwise tend to be problematic.     

The constrained blister test for the energy of interfacial adhesion

The constrained blister test (CBT) was designed to measure the energy of interfacial adhesion ( y) of polymeric films and coatings. Theoretical analysis of the CBT established a relationship between blister growth and interfacial parameters of the form A(t) A(t₀)=exp[βp²h ph-γ (t- t₀)] where A(t) is the blister area at time t, p is the applied pressure, h is the spacer height, y is the energy of interfacial adhesion, and β is a dissipative coefficient which is also related to geometric factors. The validity of the theoretical model was tested using a rubber-based pressure sensitive adhesive (PSA) tape. The PSA tape was investigated as a function of the applied pressure and the spacer height. A value of 44 J/m² was determined for the energy of interfacial adhesion. The dissipative coefficient, β, was found to vary with the applied pressure and the spacer height.     

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.     

The effect of residual stresses on adhesion measurements

The adhesion of films and coatings is often measured by determining the load required to separate them from their substrate. If there are residual stresses that are relaxed upon delamination, then an additional contribution to the energy-release rate will affect the measurements. These residual stresses may also cause a shift in the mode-mixedness of the interface crack which, in turn, can affect the interfacial toughness. To ensure an accurate interpretation of adhesion measurements, therefore, the effects of these stresses must be considered. These effects are discussed with particular reference to two commonly used test geometries: the blister test and the peel test.     

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.     

A clamped punch-loaded blister test for adhesion: a lumped parameter model and the bending-to-stretching behavior

This paper presents a clamped punch-loaded blister test and the corresponding lumped parameter model for the adhesion between thin film and rigid substrate. In the test, circular thin film is adhered to rigid substrate and an external load is applied with a clamped punch to cause the deflection of thin film. The relations among load, deflection, residual stress and strain energy release rate are thoroughly investigated. Analytical solutions in linear and nonlinear behaviors are obtained and the bending and stretching effects are associated through a lumped parameter model. The result of lumped-parameter model shows that the blister deflection is directly proportional to the applied load in the linear bending dominant region and the blister deflection is in direct proportion to the cubic root of the applied load in the nonlinear stretching dominant region. This has been proved by the result of nonlinear finite element analysis and the experimental result as well.     

Quantification of Coating Adhesion Using Laser Induced Decohesion Spectroscopy

We present a new technique, laser induced decohesion spectroscopy (LIDS), which is capable of measuring the practical work of adhesion G between a transparent polymer coating and an opaque coating or substrate. In LIDS, a laser pulse directed onto the sample creates a blister at the transparent/opaque interface. The blister's internal pressure depends on the laser pulse energy, and at a critical pressure the sample fractures, creating an annular debond similar to that obtained in the standard blister test. By measuring physical variables such as the curvature of the blister, and its radius and thickness, it is possible to deduce G, Here we measure G between an automotive clearcoat and four opaque basecoats of various pigmentations (black, white, red, metallic green) as a function of clearcoat thickness. We find that G depends on pigmentation due to the various pigment volume concentrations (PVC's) and specific pigment-binder interactions. Also, G depends on the clearcoat thickness when the thickness is comparable with the size of the plastic zone, R_p.     

The use of stimulated boundary gas release for determination of the adhesion of thin films by the blister test

The processes of stimulated gas release and gas blister growth were investigated at the interface of 100 nm thick silver films on glass substrates after irradiation by hydrogen ions of 1 MeV energy to fluences of 1 x 10¹³-1 x 10¹⁵ ion cm^-2. An interference microscope was used to examine the gas blisters and to measure the blister parameters. The relationship of these processes to the adhesion of a thin film system was established. A method to determine the adhesion and to compute the adhesion characteristics in the film-substrate system is described. The calculated energy of the detachment ranges between 0.06 and 28 J m^-2. Based on the results of this study, a series of practical approaches are proposed to measure the adhesion of thin films to substrates with the method of stimulated gas release.     

Effect of interlayer deformation on blister test

The effect of interlayer deformation on blister test for measuring adhesive strength was analyzed by modeling the interlayer as a Winkler foundation. Critical load for the initiation of debonding along the interface between the interlayer and an elastic thin film was obtained as a function of the adhesive strength, interlayer deformation, elastic modulus of Winkler foundation, and blister size. The critical pressure increases with increasing the elastic modulus of Winkler foundation. The propagation of debonding was discussed, and the arrest of debonding was observed for the condition of constant deflection. The results provide a rational for characterizing the effect of interlayer deformation on the measurement of adhesive strength from a blister test.     

Gas permeation and temperature effects in laser-induced delamination

Laser-induced delamination (LID) is a technique aimed at measuring the work of adhesion of thin polymer coatings on metal substrates. A laser pulse is used to create a blister that initiates delamination of the film under pressure. The stress fields in the blister wall and the work of adhesion of the interface are determined using a linear elastic model.In this paper we discuss validity of the LID results addressing permeation of gas through the blister wall and the initial high temperature of the substrate. A procedure to account for the effect of gas permeation in the calculations of the work of adhesion is proposed. Permeation of gas is also considered under compressive and tensile in-plane stresses. Modeling of the permeation process demonstrates a good agreement with the experiment.At early stage of the blister formation the metal substrate and the blister gas experience high temperatures. The time scales of the cooling processes are estimated. Possible effects of the high temperatures on the permeation of gas and on the process of delamination are discussed.     

Fundamentals of Adhesion Failure for a Model Adhesive (PMMA/Glass) Joint in Humid Environments

The origins for the abrupt adhesion loss at a critical relative humidity (RH) for polymeric adhesives bonded to inorganic surfaces were explored using a poly(methyl methacrylate) (PMMA) film on silicon oxide as a model system. The interfacial and bulk water concentrations within the polymer film were quantified as a function of D₂O partial pressure using neutron reflectivity. The adhesive fracture energies of these PMMA/SiO₂ interfaces at the same conditions were determined using a shaft-loaded blister test. Discontinuities in the adhesive fracture energy, bulk moisture solubility, and the width of the interfacial moisture excess near the interface were observed at the critical RH. A mechanism based on the coupling of bulk swelling-induced stresses with the decreased cohesive strength due to moisture accumulation at the interface is proposed and is consistent with all experimental observations.     

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.     

Effect of Adhesion, Film Thickness, and Substrate Hardness on the Scratch Behavior of Poly(carbonate) Films

The effect of adhesion, film thickness, and substrate hardness on the scratch behavior of poly(carbonate) (PC) films was investigated. Films of various thickness were prepared by spin-coating solutions of PC in chloroform onto glass, ferroplate, Al 1100, Al 6022, and Al 6111 substrates. Adhesion between the films and the substrates was controlled by pretreatment of the substrates and the thickness of the films was controlled by the concentration of the PC solutions. Adhesion of the films to the glass substrates was measured by a blister test. Scratch tests were performed using a custom-built, progressive-load scratch tester with interchangeable diamond indenters; the resulting scratches were observed by optical microscopy, atomic force microscopy (AFM), and environmental scanning electron microscopy (ESEM). The critical normal load (i.e., the smallest applied normal load for which delamination of the film from the substrate was observed) was used as a criterion to determine the scratch resistance of the films. It was found that better film/substrate adhesion resulted in a higher critical load for delamination. As film thickness increased, the critical load and, thus, scratch resistance also increased. Substrate hardness had a strong influence on the scratch behavior of the PC films. For a low-hardness substrate (i.e., Al 1100), the work from scratching was mainly consumed by deforming the substrate. In the case of substrates with intermediate hardness (i.e., Al 6022, Al 6111, and ferroplate), the substrates were more resistant to the stresses that were generated in the films; hence, the deformation of the substrates was less severe. A high-hardness substrate (i.e., glass) resisted the applied load and resulted in higher stress concentrations in the films and at the interface. Consequently, a rougher surface inside the scratch track was observed.     

Effect of Adhesion,Film Thickness,and Substrate Hardness on the Scratch Behavior of Poly(carbonate) Films

The effect of adhesion, film thickness, and substrate hardness on the scratch behavior of poly(carbonate) (PC) films was investigated. Films of various thickness were prepared by spin-coating solutions of PC in chloroform onto glass, ferroplate, Al 1100, Al 6022, and Al 6111 substrates. Adhesion between the films and the substrates was controlled by pretreatment of the substrates and the thickness of the films was controlled by the concentration of the PC solutions. Adhesion of the films to the glass substrates was measured by a blister test. Scratch tests were performed using a custom-built, progressive-load scratch tester with interchangeable diamond indenters; the resulting scratches were observed by optical microscopy, atomic force microscopy (AFM), and environmental scanning electron microscopy (ESEM). The critical normal load (i.e., the smallest applied normal load for which delamination of the film from the substrate was observed) was used as a criterion to determine the scratch resistance of the films. It was found that better film/substrate adhesion resulted in a higher critical load for delamination. As film thickness increased, the critical load and, thus, scratch resistance also increased. Substrate hardness had a strong influence on the scratch behavior of the PC films. For a low-hardness substrate (i.e., Al 1100), the work from scratching was mainly consumed by deforming the substrate. In the case of substrates with intermediate hardness (i.e., Al 6022, Al 6111, and ferroplate), the substrates were more resistant to the stresses that were generated in the films; hence, the deformation of the substrates was less severe. A high-hardness substrate (i.e., glass) resisted the applied load and resulted in higher stress concentrations in the films and at the interface. Consequently, a rougher surface inside the scratch track was observed.     

Fundamentals of Adhesion Failure for a Model Adhesive (PMMA/Glass) Joint in Humid Environments

The origins for the abrupt adhesion loss at a critical relative humidity (RH) for polymeric adhesives bonded to inorganic surfaces were explored using a poly(methyl methacrylate) (PMMA) film on silicon oxide as a model system. The interfacial and bulk water concentrations within the polymer film were quantified as a function of D₂O partial pressure using neutron reflectivity. The adhesive fracture energies of these PMMA/SiO₂ interfaces at the same conditions were determined using a shaft-loaded blister test. Discontinuities in the adhesive fracture energy, bulk moisture solubility, and the width of the interfacial moisture excess near the interface were observed at the critical RH. A mechanism based on the coupling of bulk swelling-induced stresses with the decreased cohesive strength due to moisture accumulation at the interface is proposed and is consistent with all experimental observations.     

Local Bending Moment as a Measure of Adhesion: The Blister Test

We propose to characterize joints between materials by the maximum bending moment, M_max, borne just prior to delamination. We suggest to evaluate M_max in the blister test geometry through direct measurement of the blister curvature in the vicinity of the separation line and employ a scanning capacitance microscope for the blister profiling. The methodology and apparatus were tested on measurements of adhesion of two commercial polymer films to Plexiglas and Teflon.     

Dissipative Processes in Interfacial Failure

An investigation of the failure behavior of pressure sensitive adhesive tape was performed utilizing the constrained blister test. The constrained blister test was designed to measure the energy of interfacial adhesion of thin polymeric coatings. A constant energy of interfacial adhesion of 1.8J/m² was determined for a rubber based pressure sensitive adhesive on a copper substrate. An active zone was visualized through the transparent backing. The deformation within the active zone was found to consist of cavitation and deformation of ligaments. Fracture of the ligaments causes the detachment front to advance. It was proposed that the rate of energy dissipation, D, reflects the resistance of the bond to time dependent deformation, and therefore dictates the lifetime for this particular specimen geometry. A direct relationship was established between lifetime and the inverse of the rate of energy dissipation in the active zone, D.     

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.