Polyimide Adhesives and Aluminum

This study examines the effect of thioether sulfur in the polyimide backbone, polyimide T_g, and adherend surface pre-treatment on aluminum bond strengths as determined with both peel and wedge specimens. Surface pretreatment and T_g had more of an effect on peel strength than the presence of sulfur in the polyimide backbone. NaOH etching and comparatively low T_g polyimides combined to produce the highest peel strengths. Together, these factors combined the removal of surface oxide from the adherend with a flexible polyimide which could better relieve stress during testing. Little difference was observed between the peel strengths of sulfur and non-sulfur containing polyimides, and no oxidation of sulfur was observed in the peel samples. NaOH etching also caused both wedge and peel specimens to fail more within the polyimide than in the oxide layer of the adherend. Thus, the NaOH etch appeared to increase interfacial adhesion between the aluminum and the polyimide. The low T_g polyimides performed better than the high T_g polyimides in the wedge test, with the polyimide derived from 4,4'-bis(3,4-dicarboxyphenoxy) diphenyl sulfide dianhydride and 4,4'-diaminodiphenyl ether (BDSDA/ODA) performing the best. This observation could be due to a metal-sulfur interaction since oxidized sulfur was surprisingly observed on the failed surfaces of these bonds regardless of the environment or surface pretreatment. A metal component in the aluminum alloy rather the aluminum is believed to promote the sulfur oxidation.     

Effects of peel angle on peel force of adhesive tape from soft adherend

In the case of the peeling of adhesive tapes from soft adherends, the contributions of the compressive force at the adhered portion as well as the larger deformation of adherend have essential roles in determining the peeling properties. In this paper, the peel force of an adhesive tape from a soft adherend has been measured to understand the peeling mechanism, which is greatly affected by the peel angle. A commercially available pressure-sensitive adhesive was used as the tape, and a cross-linked polydimethylsiloxane (PDMS) was used as the soft adherend. The purpose of this study is to clarify the effects of the peel angle on the peel behavior of this system at room temperature under different material specifications and different experimental conditions. The factors that affect the peel force of the PDMS adherend included the degree of cross-linking in PDMS, the thickness of PDMS, peel angle, and peel velocity. Two characteristic peel patterns were observed, which depended on the material specifications and different experimental conditions. The peel mechanism was discussed in terms of the deformation of the adherend.     

Effect of Deformation-induced Residual Stress on Peel Strength of Polymer Laminated Sheet Metal

The adhesion between adhesively bonded polymer film and a metallic sheet substrate in a polymer laminated sheet metal (PLSM) subjected to large deformation, such as in a forming process, is influenced by two deformation-induced factors. These are (i) evolution of surface roughness of metallic substrate with applied strain and (ii) development of residual stress in the polymer adherend (polymer film with a thin uniform adhesive layer on one side) arising from significant differences in the deformation behavior of metal and polymeric components. A new experimental methodology was devised in this study to decouple the effects of substrate surface roughness and residual stress on interfacial peel strength (IPS) of uniaxially deformed PLSMs. This methodology was based on 180° peel testing of PLSM specimens prepared under two different lamination conditions, one involving systematic pre-straining in uniaxial tension of the metallic substrate prior to laminations and the other involving post-lamination pre-straining of the PLSM. The role of pre-strain and peel test speed, for the above laminations conditions, were critically analyzed for their effect on IPS of two differently tailored PLSM systems. The IPS results were attributed to the effect of deformation-induced residual stress and metallic surface roughness. The analysis suggests that IPS is strongly dependent upon the residual stress induced by uniaxial deformation but only marginally on substrate surface roughness depending upon the constituents (film and adhesive) of the adherend. The magnitude of pre-strain was inversely and non-linearly related to IPS for both deformed PLSMs. Peel test speed, on the other hand, showed a more complex behavior in terms of IPS for the two PLSM systems.     

On the work of adhesion and peel strength between pressure sensitive adhesives and the polymeric films used in LCD devices

Peel strength, a convenient measure of bond strength in adhesive/adherend systems, is known to be a function of various factors such as the thermodynamic work of adhesion, rate of measurement, thermal history, and temperature. Generally, it is believed that the work of adhesion is primarily involved in the first stage of adhesion through wetting phenomenon and beyond that its role diminishes in that the portion of thermodynamic contribution to actual bond strength is insignificant. In practice, however, we often observe that a suitable surface treatment increases the surface energy of the substrate, which further enhances the bond strength. One practical example is the surface treatment carried out in LCD industry to obtain sufficient bond strength between pressure sensitive adhesives and polymeric films. To further our understanding of the effect of surface treatment, we attempted to establish a possible correlation, if any, between the thermodynamic work of adhesion and peel strength. For this, we carefully measured the contact angles of water and diiodomethane against various polymeric films, and calculated the surface energy and the thermodynamic work of adhesion using the two widely used approaches: Young-Fowkes-Girifalco-Good, and Wu methods. Before establishing a correlation, some general aspects of the above two methods are discussed. The values of the work of adhesion obtained were compared with the measured peel strength. Indeed, we observed a clear correlation between the two quantities: the increase of the work of adhesion led to the increase of peel strength. As a reason for this correlation, we proposed that the increase of surface energy might be associated with the increase of various surface functional groups, which, in turn, contributed to the formation of chemical bonding with the PSA leading to the increase of peel strength.     

Stringiness morphology for crosslinked polyacrylic pressure-sensitive adhesives measured by peel testing with constant rate

To clarify the formation mechanism of front frame-type morphology, the stringiness of crosslinked random copolymers of poly(n-butyl acrylate-acrylic acid) during a 180° peel test with a constant tensile rate was examined for various crosslinker contents and rates using a quartz adherend. Cohesive failure occurred for lower crosslinker content and rate, whereas interfacial failure with sawtooth-type stringiness without a frame was observed for higher crosslinker content and rate. Front frame-type stringiness was formed at the boundary of cohesive and interfacial failures. To clarify the formation mechanism, observation was conducted from the start of peel test until the equilibrium state. The sawtooth-type stringiness with branches first formed at the tip. The adjoining branches were connected and the 2D frame was formed only on the adherend surface. The formed 2D frame developed toward the 3D walls and the front frame-type was then completed. This is caused by the surface tension that acts to restrain the increase in the surface area. However, the surface area of the front frame-type morphology was larger than the no frame-type. The larger absorption of peeling stress by the formation of this morphology is expected to contribute to peel strength improvement.     

The interrelationships between electronically conductive adhesive formulations,substrate and filler surface properties,and joint performance. Part I: the effects of adhesive thickness

Electronically conductive adhesives (ECAs) have received a great deal of attention for interconnection applications in recent years. Even though ECAs have excellent potential for being efficient and less costly alternative to solder joining in electronic components, they still possess a number of problems with respect to durability and design to meet specific needs. One of the issues that requires understanding is regarding the optimum adhesive thickness (AT) to be used. This study addresses this issue in relation to the formulations of the conductive adhesives and their interactions with adherend surfaces. For this purpose, two different adherends varying in surface characteristics were utilized along with three different conductive adhesive formulations with varying particle loadings, and shapes and sizes of conductive nickel fillers. Joints were also prepared with two different AT values, to gain insight into the influence of AT on the joint strength, deformation and joint conductivity. As the AT was increased, only a small reduction in failure load and ultimate displacement values were observed with unetched adherends. With etched adherends, however, a small increase in joint stretchability was evident with higher adhesive thickness tested at a lower crosshead speed. When the AT was increased, we also noted a corresponding increase in the initial joint resistance.     

On the effect of pulsed laser ablation on shear strength and mode I fracture toughness of Al/epoxy adhesive joints

The present work describes an experimental study about the shear strength and the mode I fracture toughness of adhesive joints with substrates pre-treated by pulsed laser ablation. An ytterbium-doped pulsed fiber laser was employed to perform laser irradiation on AA6082-T4 alloy. Morphological and chemical modifications were evaluated by means of surface profilometry, scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Thick adherend shear tests were carried out in order to assess the shear strength while the mode I fracture toughness was determined using the double cantilever beam. For comparison, control samples were prepared using classical surface degreasing. The results indicated that laser ablation has a favorable effect on the mechanical behavior of epoxy bonded joints; however, while a + 20% increase was recorded for shear strength, a remarkable threefold enhancement of fracture toughness was observed with respect to control samples. XPS analyses of treated substrates and SEM observations of the fracture surfaces indicated that laser pre-treatment promoted chemical and morphological modifications able to sustain energy dissipation through mechanical interlocking. As a result cohesive failure within the adhesive bond-line was enabled under predominant peel loading.     

Effect of adhesive thickness on the stringiness of crosslinked polyacrylic pressure‐sensitive adhesives

The effect of adhesive thickness on stringiness behavior during 90° peel testing was investigated for crosslinked poly(n‐butyl acrylate‐acrylic acid) (A) and poly(2‐ethylhexyl acrylate‐acrylic acid) (B) with a constant crosslinker content. The adhesive thickness was varied over the range from 15 to 60 μm. All adhesive thicknesses exhibited sawtooth‐type peeling with a front frame for B, but only the 30‐μm thickness generated a front frame‐type for A. The peel rate decreased from 15 to 45 μm and plateaued above 45 μm under a constant load test. These results indicate that the adhesion strength increases with adhesive thickness, but reaches a constant value at high thicknesses. The stringiness was also analysed for B and the sawtooth interval observed to increase with increasing thickness. This means the sawtooth number decreased. As a result, the concentrated stress per sawtooth induces easier peeling and so this factor tend to increase the peel rate. Conversely, the stringiness width increased with increasing thickness. The stress load over the stringiness region decreased with an increase in thickness, meaning that a decrease in the concentrated stress decreases the peel rate. The actual peel rate is influenced by the contributions of these two factors. The strain rates during constant peel rate tests decreased slightly with increasing thickness, due to a reduction in the apparent modulus. The molecular mobilities near the adherend and the backing surfaces were evidently restrained by these surfaces, and the relative rates of motion of such restrained molecules decrease with increased thickness. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42210.     

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.     

Some observations on heat transfer to agitated liquids

Heat transfer coefficients for agitated liquids in a flat-bottomed vessel equipped with a heating coil have been measured over wide ranges of Prandtl and Reynolds numbers in order to examine the effect of coil surface, impeller design and coil geometry. The study of impellers included a comparison of flat-bladed and pitched-bladed agitators. Helical and baffle coil geometries were tested using smooth, knurled and finned tube surfaces. For all systems studied the Reynolds number exponent was observed to be dependent on viscosity. The data for finned tubes indicated higher transfer rates due to increased surface area and wall-turbulence.     

Peel Analysis Using the Finite Element Method

Large displacement finite element analysis and subsequent experimental work has been used to investigate the adhesive peel test; at this stage, only elastic behaviour has been considered.

Both non-cracked and cracked configurations have been analysed, representing initial and continuous failure of the peel test. Analysis of the former indicated that initial failure was caused by the adhesive principal stresses driving a crack towards the interface with the flexible adherend. Investigation of the cracked configuration has shown that the amount of mode II loading at the crack tip is significant and is essentially independent of peel angle, load and adhesive or adherend modulus, only decreasing as the adhesive becomes incompressible. Failure (propagation) has been shown to occur at a critical applied bending moment for a particular adherend and adhesive, independent of peel angle. Further, the strength (load)'measured by the peel test is not proportional to the actual strength of the adhesive, a small increase in the adhesive strength causing a much larger increase in the applied peel load.     

Peel mechanics for an elastic-plastic adherend

The force required to propagate a 180° bend in an elastic-plastic strip has been calculated from elementary bending theory. Measured forces for Mylar strips of various thicknesses, bent to various degrees, were in good agreement with these calculated values. The corresponding additional stripping force in a peeling experiment will depend upon the thickness of the elastic-plastic adherend, becoming zero both for infinitesimally thin adherends and for those exceeding a critical thickness t_c and passing through a maximum value at intermediate thicknesses. Published data are in good agreement with these conclusions. For a strongly adhering strip, higher peel strengths are found for a peel angle of 180°, compared to 90°, and the effect is greater than can be accounted for solely by plastic yielding of the adherend. It is attributed in part to greater energy dissipation within the adhesive layer.     

Peel Analysis Using the Finite Element Method

Large displacement finite element analysis and subsequent experimental work has been used to investigate the adhesive peel test; at this stage, only elastic behaviour has been considered.

Both non-cracked and cracked configurations have been analysed, representing initial and continuous failure of the peel test. Analysis of the former indicated that initial failure was caused by the adhesive principal stresses driving a crack towards the interface with the flexible adherend. Investigation of the cracked configuration has shown that the amount of mode II loading at the crack tip is significant and is essentially independent of peel angle, load and adhesive or adherend modulus, only decreasing as the adhesive becomes incompressible. Failure (propagation) has been shown to occur at a critical applied bending moment for a particular adherend and adhesive, independent of peel angle. Further, the strength (load)'measured by the peel test is not proportional to the actual strength of the adhesive, a small increase in the adhesive strength causing a much larger increase in the applied peel load.     

Analytical Peel Load Prediction as a Function of Adhesive Stress Concentration

Peel data for two epoxy adhesives and a recent model of the adhesive stresses in the peel geometry are used to investigate the effectiveness of two constitutive models and several adhesive failure criteria. The failure criteria are based on either the critical strain energy-release rate or the critical von Mises strain at the peel root, both taken as functions of the “loading zone length” (LZL), defined as a measure of the degree of stress concentration at the root of the peeling adherend. The peel model uses LZL as an independent parameter that captures the effects of the peel angle, adherend thickness, and the mechanical properties of the adhesive and adherend. Both the energy- and strain-based failure criteria can be used to predict the steady-state peel load with an average absolute error of less than 10% over the range of conditions that were examined.     

Bonding characteristics and corrosion resistance of silane–cerium-treated aluminum adherend

A silane–cerium treatment was applied on an aluminum adherend to simultaneously improve the bonding performance and corrosion resistance of the adhesively bonded aluminum joint in cryogenic applications, such as with liquefied natural gas containment tanks. The lap shear strengths and corrosion performances of the adhesively bonded joints composed of treated aluminum adherends were measured with respect to the silane–cerium treatment and the surface pretreatment on the aluminum adherend. The bonding characteristics of the aluminum adherend were investigated by measuring the water contact angle and conducting the potentiodynamic polarization test after the aluminum adherends with different surface treatments of silane–cerium were immersed in a 0.5?M NaCl solution. In addition, the surfaces were analyzed with scanning electron microscopy, X-ray photoelectron spectroscopy, and Fourier transform infrared spectroscopy to characterize the chemical compositions of the silane–cerium-treated aluminum adherend. The experimental results show that an appropriate silane–cerium treatment on the aluminum adherend produces an effective corrosion-resistant layer and that it has a highly reliable bonding characteristic for the adhesive joint at a cryogenic temperature of ?150?°C.     

Effects of various adherend surface treatments on fatigue behavior of joints bonded with a silver-filled electronically conductive adhesive

Conductive adhesives have been used in a variety of electronic packaging applications. This paper presents an investigation into the effects of various adherend surface treatments on the fatigue and failure behaviors of adhesively-bonded joints. For this purpose, single-lap joints were fabricated using specimens with adherend surfaces modified employing various chemical and mechanical modification techniques, and tested under a spectrum of fatigue and environmental conditions. The results of our work indicate a profound influence of the adherend surface on both the fatigue behavior and also the moisture ingress mechanism into the joint. Finally, experiments were conducted to assess the effect of adherend surface condition on the moisture ingress mechanism.     

The Effect of Modification of an Epoxy Resin Adhesive with ATBN on Peel Strength

The effects of rubber content, rate of peel and temperature on peel strength of ATBN modified DGEBA based epoxy resin adhesives have been investigated. The fracture surfaces of peel test specimens and the distribution of rubber particles in cured bulk epoxy resin have been observed with SEM and TEM, respectively. The mechanical properties of bulk rubber modified epoxy resin have been also measured. The peel strengths increased with increasing rubber content, peel rate, and decreasing temperature. The peel strengths were superposed as a function of rate and temperature. Plots of the shift factors against temperature gave two straight lines, which followed an Arrhenius relationship. The region of temperature below the intersection of the two straight lines, temperature somewhat lower than T_g of epoxy adhesive, gave markedly high peel strengths and a stick-slip failure due to plastic deformation of the adhesive, and a number of micro holes produced by the rupture of rubber micro particles on the fracture surface. The region of temperature above the intersection gave lower peel strengths and an apparent interfacial failure with ductile fracture of the adhesive, and larger, shallow holes or no holes. From these results, the marked increase of peel strength was concluded to be mainly attributed to the plastic or viscoelastic deformation of epoxy matrix, the strong bond at the interface between rubber particles and epoxy matrix, and the dilation and rupture of a number of rubber particles.     

Stresses in an Adhesive Bond at an Adhesive/Adherend Interface Under Load

Triaxial stresses were determined by X-ray diffraction immediately adjacent to the adhesive/adherend interface of a single lap adhesive bond while under a tensile load. One adherend was a Be strip that was relatively transparent to the X-rays; the X-ray beam passed through this and the layer of FM-73M adhesive to diffract from the surface of the other adherend which was of 6061 aluminium alloy suitably annealed. The thicknesses of the Be and Al were made such that their stiffness in tension was matched.

Measured stresses were compared with stresses calculated using the Texgap-2D finite element code for a nominally identical joint and at a depth of 0.033 mm into the Al adherend which coincided with the average depth from which the X-ray data were obtained. The comparison showed a general agreement in trends and magnitudes except at the extremities of the bond. In particular the measured peel stress was found to be substantially larger at one extremity than the calculated peel stress. Possible causes of the discrepancies are discussed.     

Stresses in an Adhesive Bond at an Adhesive/Adherend Interface Under Load

Triaxial stresses were determined by X-ray diffraction immediately adjacent to the adhesive/adherend interface of a single lap adhesive bond while under a tensile load. One adherend was a Be strip that was relatively transparent to the X-rays; the X-ray beam passed through this and the layer of FM-73M adhesive to diffract from the surface of the other adherend which was of 6061 aluminium alloy suitably annealed. The thicknesses of the Be and Al were made such that their stiffness in tension was matched.

Measured stresses were compared with stresses calculated using the Texgap-2D finite element code for a nominally identical joint and at a depth of 0.033 mm into the Al adherend which coincided with the average depth from which the X-ray data were obtained. The comparison showed a general agreement in trends and magnitudes except at the extremities of the bond. In particular the measured peel stress was found to be substantially larger at one extremity than the calculated peel stress. Possible causes of the discrepancies are discussed.