Mechanical characterization of a high elongation and high toughness epoxy adhesive

In this paper, a new epoxy adhesive has been mechanically characterized. The adhesive combines the properties of an epoxy adhesive and typical polyurethane (PU) adhesive, such as high elongation and high toughness. Experimental tests were performed to measure the tensile properties, shear properties, thermal properties and fracture properties. The tensile test shows high tensile strength and high elongation. The single lap joint (SLJ) test shows that the failure load is proportional to the overlap length for hard steel adherends. For the SLJs with mild steel adherends, the failure occurred due to adherend yielding. Impact tests were conducted using SLJ specimens and the results are consistent with the SLJ tested under static conditions. The Tg was obtained using a Dynamic Mechanical Analysis (DMA) type of test. The toughness in mode I was determined using the Double Cantilever Beam (DCB) test and the toughness in mode II using End Notched Flexure (ENF) test.     

Investigation of curing characteristics of carbon fiber/epoxy composites cured with low‐energy electron beam

To solve the penetration depth of carbon fiber/epoxy prepreg and irradiation dose uniformity by low‐energy E‐Beam under 125 keV, the both‐side irradiation curing of prepreg was investigated. The results show that there is little thermal effect during the low‐energy electron beam irradiation curing process, even though the irradiation dosage reached 300 kGy, only 46.2°C can be tested on the prepreg surface. Due to the low curing temperature, the degree of cure of prepreg was only 61.8% at 300 kGy level of irradiation, and the glass‐transition temperature (T_g) was only 48.6°C. The degree of cure and T_g can be increased sharply by thermal postcure. After being postcured at 160°C for 30 min, the degree of cure and the T_g of prepreg reached 98.5% and 170.4°C, respectively. Interlaminar shear strength testing result indicate that the fabrication process of the composite layer by layer curing by the low‐ energy E‐Beam is a promising cure approach. POLYM. COMPOS., 36:1731–1737, 2015. © 2014 Society of Plastics Engineers     

The influence of hydroxyl group concentration on epoxy–aluminium bond durability

The influence of hydroxyl group (OH) concentration on the durability of adhesive bonds formed between an epoxy resin and aluminium adherend has been examined. Initially, surface analysis in combination with chemical derivatisation was employed to characterise the OH and epoxy functional groups present in FM-73, a structural epoxy adhesive. Bulk FM-73 indicated a higher degree of cure than the surface of FM-73 present at the interface of an epoxy–aluminium adhesive joint. Plasma and water treatment of the aluminium adherend was employed to alter the metal oxide's surface OH concentration. Despite a several-fold difference of aluminium surface OH concentrations for the different metal pre-treatments, there was no significant variation in the adhesive joint fracture toughness in a humid environment, G _Iscc. In contrast, grit-blasting the aluminium prior to bonding increased G _Iscc almost 15-fold. Simple calculations indicate that the aluminium surfaces used in the bonding experiments would have a large excess of OH groups available to react with a standard epoxy resin and that the influence of surface roughness on adhesion durability is not insignificant.     

Cleavage behavior of bonds made with adherends capable of plastic yield

The failure behavior of adhesive joints under cleavage stresses depends upon the thickness of the adherend. With thick, rigid adherends failure occurs by rapidly propagated adhesive rupture. Thinner adherends can exhibit plastic flexural yield, the subsequent adhesive failure then being progressive and strain-limited, and occurring only in the region of bond directly adjacent to the yielding adherend. A fairly sharp discontinuity between these two types of behavior occurs over a small range of adherend thickness T. Work to rupture can differ by more than an order of magnitude, for otherwise identical joints having T above or below the transitional range (around T_c). For T > T_c the applied load P causing rupture is proportional to T^1.5 while the moment arm remains constant, as predicted by Yurenka. For T < T_c the turning moment during failure is proportional to T² and is substantially independent of the nature of the adhesive. Empirically, the radius of the yielded adherend after failure is proportional to T. The manner of interaction of various adhesive mechanical properties in defining P in the two ranges and, thereby, T_c, are related to this and other empirical correlations. The initial free moment arm in the joint, L, determines the stability of peel at initiation of adhesive rupture. Reducing L leads ultimately to instability. The change of controlling factors as L → 0 is discussed.     

Plasticity in peeling

Contrary to classical theory, a high proportion of bond failures by peeling involve progressive plastic adherend flexural yield. Such yield occurs with adherend thicknesses below a critical value, T_c, which is shown calculable by combining elastic peel mechanics with plastic bending criteria. The geometry of such “peel with yield,” and thence the moment-controlled peel forces, can be accounted for only if the adhesive is also recognized as behaving essentially plastically. Subsequent plastic adherend unbending is important with highly extensible adhesives. The geometry of “legging” peel in such cases is best described by fully plastic mechanics. These are derived and shown to account for literature data on dependencies of peel force upon peel rate and adhesive thickness. “Stick-slip” peel phenomena are indicated to be controlled by recurring interacting plastic–elastic transitions, in both adhesive and adherend: adhesive strain rate is critical in such phenomena. Four regimes of peel behavior can therefore apply as adherend thickness (T) increases, with peel forces proportional respectively to T⁰, T^2/3, T^3/2 (above T_c) and finally controlled by moment limitations due to joint configurational constraints (“cleavage”).     

Strain rate dependence of adhesive joints for the automotive industry at low and high temperatures

In this study the impact and quasi-static mechanical behaviour of single lap joints (SLJ) using a new crash resistant epoxy adhesive has been characterized as a function of temperature. Single lap adhesive joints were tested using a drop weight impact machine (impact tests) and using a universal test machine. Induction heating and nitrogen gas cooling was used in order to achieve a homogeneous distribution of temperature along the overlap of + 80 °C and ?20 °C, respectively. Adherends made of mild steel, similar to the steel used in automobile construction, were chosen in order to study the yielding effect on the strength of the SLJ. Results showed that at room temperature (RT) and low temperature (LT), failure was dictated by the adherends due to the high strength of the adhesive. At high temperature (HT), a decrease was found in the maximum load and energy absorbed by the joint due to the reduced strength of the adhesive at this temperature. The results were successfully modelled using the commercially available finite element software Abaqus^®. Good correlation was found between experimental and numerical results, which allows the reduction of experimental testing.     

Properties of carbon fiber composite laminates fabricated by coresin film infusion process for different prepreg materials

A new cocured process called coresin film infusion (co‐RFI) process, which combines RFI process and prepreg/autoclave process, was introduced and four kinds of commercial carbon fiber prepreg material systems and a kind of resin film were applied to fabricate co‐RFI laminates. The compatibility between the resin film and the prepreg matrix and the application of co‐RFI process were investigated based on the resin flowability, glass transition temperature of cured resin, processing quality of laminate, and variation in resin modulus on cocured interphase region measured by nanoindentation. Furthermore, mode I (G_IC), mode II (G_IIC) delamination fracture toughness, and flexural strength and modulus were measured to evaluate the mechanical properties of cocured laminates with different prepreg materials. The experimental results show that thickness and fiber volume fraction of co‐RFI laminates with the four kinds of prepreg materials are similar to those of prepreg laminates and RFI laminate with acceptable differences. In addition, there are no obvious defects in co‐RFI laminates. Moreover, the reduced modulus of resin at cocured interface and glass transition temperature values of the mixed resin reflect good compatibility between prepreg matrix resin and RFI resin. The G_IC, G_IIC values, and flexural performances of cocured laminates lie between and even exceed those of prepreg laminates and RFI laminates, indicating no weakening effect in the cocured interface. Therefore, the co‐RFI process is believed to effectively fabricate composite with low cost and it can be applied using various prepreg systems. POLYM. COMPOS., 34:2008–2018, 2013. © 2013 Society of Plastics Engineers     

Preparation and characterization of modified telechelic natural rubber-based pressure-sensitive adhesive

Telechelic natural rubber (TNR) was prepared by the use of potassium persulfate and propanal at 70 °C and various degradation times from 0 to 30 h. These samples were then grafted by maleic anhydride (MA) in toluene solution before modification with 3-amino-1,2,4-triazole (ATA) to produce modified TNRs (AMTNRs). Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) was used to identify the chemical compositions. Carboxyl and hydroxyl groups of TNRs were clearly observed, due to chain scission, oxidation, and modified chain ends. The viscosities of TNRs were dropped greatly after 5 h and then decreased slowly as a function of degradation time. ATR-FTIR spectra of AMTNRs showed amide bonds between ATA and MA groups, and then the multiple hydrogen bonding arrays were formed. The glass transition temperatures (T_g) of AMTNRs were determined by differential scanning calorimetry. The T_g of AMTNR_0 moved to a higher temperature of –55 °C after modification by ATA, confirming the formation of multiple hydrogen bonding arrays. However, the T_g of AMTNR_5 to AMTNR_30 decreased slightly due to chain scission in the degradation process. The adhesive properties of AMTNR-based pressure-sensitive adhesive were evaluated by a Lloyd adhesion tester. The tack of AMTNRs depended on wettability whereas peel and shear strengths were responded by a combination between wettability and multiple hydrogen bonding arrays.     

Fracture toughness of adhesive joints. I. Relationship between strain energy release rates in three different fracture modes and adhesive strengths

The three strain energy release rates, G_IC, G_IIC, and G_IIIC, of adhesive joints can be attributed to their ability to resist crack propagation of solids in the adhesive layer. The dependencies of G_IC, G_IIC, and G_IIIC on crack lengths for various adhesive joints were determined using the double-cantilever beam specimen by a compliance method. The two types of adhesive strengths, i.e., adhesive tensile strength and adhesive shear strength, corresponding to G_IC and G_IIC, respectively, were carried out at room temperature and 65% RH with a crosshead speed of 10 mm/min. The G_IC, G_IIC, and G_IIIC were dependent upon crack length and had constant values irrespective of geometric parameters of the specimen over the crack length of five times adherend thickness, 0.65 (= crack length over half a length of span) and eight times adherend thickness, respectively. In the region of the crack length, we determined the following increasing order of fracture toughness: G_IC < G_IIIC < G_IIC. A positive correlation was found between adhesive tensile strength and G_IC. A significant relation between adhesive shear strength and G_IIC was not found in this work. Further studies are needed to clarify the relation between adhesive shear strength and G_IIC with general adhesives. © 1994 John Wiley & Sons, Inc.     

Stress-free temperature in a mixed-adhesive joint

Adhesive joints used in supersonic aircraft fuselage need to withstand low (?55°C), as well as high (200°C) temperatures. However, there are no adhesives suitable for the whole temperature range. A solution would be a joint with a combination of a low-temperature adhesive and a high-temperature adhesive, called a mixed-adhesive joint. In a bonded joint, the thermal stresses are generated essentially by the different thermal expansion properties of the adhesive and the adherends and, to a lesser extent, by the shrinkage of the adhesive produced by curing. The case of a mixed-adhesive joint is more complicated because there are two adhesives with different glass transition temperatures (T _g). To determine the stress-free temperature in a mixed adhesive joint, sandwich specimens of aluminium–adhesive–CFRP (carbon-fibre-reinforced plastic) were fabricated and the thermal strains were measured with strain gauges. In a mixed adhesive joint, two stress-free temperatures were found: the stress-free temperature of the high temperature adhesive, which is its cure temperature, and the stress-free temperature of the low temperature adhesive, which is its T _g.     

TBA studies of prepreg curing behavior

The torsional braid analysis (TBA) equipment has been used as an automated torsion pendulum to characterize prepreg materials in the form of single ply strips (2-1/2 × 1/8 in.). Compared to the use of coated glass braids, the main difference was a marked weakening of the gelation mechanical damping peak in isothermal runs. However, prepreg materials consisting of epoxy resins on glass, carbon or aramid fibers were successfully run isothermally to provide gelation and vitrification times as a function of temperature, or in constant heating rate scans to reveal the T < T_g and the T_g relaxations of the uncured resins, and at higher temperatures phenomena associated with gelation, vitrification and devitrification.     

Influence of rheological properties of adhesive polymer on strain energy release rate of mode II and adhesive shear strength

It is well known that adhesive strength shows temperature and rate dependencies reflecting viscoelastic properties of an adhesive used. Specifically, a mechanical relaxation mechanism around the glass transition temperature (T_g) has a strong effect on the adhesive strength, which involves deformation of the adhesive layer. In addition, it is very interesting to know how viscoelastic properties of the adhesive affect the value of strain energy release rate since deformation and failure of the adhesive occur at the measurement of strain energy release rate for adhesive joints. In this study, adhesive tensile strength and strain energy release rate (G_IIC) in plain-shearing mode were measured under a constant experimental condition using adhesives consisting of two types of epoxy resins; the influence of viscoelastic properties on these two values was investigated, and we discuss the relationship between the adhesive shear strength and G_IIC. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 66: 525–536, 1997     

Fatigue and failure behavior of silver-filled electronically-conductive adhesive joints subjected to elevated temperatures

The use of adhesives to replace mechanical connectors and other joining methods has enjoyed rapid growth in recent years. There are a number of issues of concern in the design of joints bonded using electronically-conductive adhesives (ECAs). One of these is the cyclic fatigue behavior of conductive adhesive interconnects under different environmental conditions, in which fatigue failure might occur due either to mechanical or thermal stresses varying in a cyclic manner. This paper addresses the effect of elevated temperatures on the fatigue and failure behavior of ECAs. For this purpose, joints were prepared using stainless steel adherend specimens bonded with a commercial ECA, and tested using monotonic and cyclic loadings, at two elevated temperatures, namely 50^°C and 90^°C. When the temperature was increased to 90^°C, close to the glass transition temperature of the adhesive, we observed consistently parallel fatigue curves at different load ratios (R = P _min /P _max) for joints, as in the case of 50^°C test condition, along with significant reduction in fatigue lives. Joint failure mechanisms were also analyzed using optical techniques, and joint conductivity measurements.     

Effect of Adherend Recessing on the Tensile Strength of Single Lap Joints

Bonded joints are gaining importance in many fields of manufacturing owing to a significant number of advantages to the traditional methods. The single lap joint (SLJ) is the most commonly used method. The use of material or geometric changes in SLJ reduces peel and shear peak stresses at the damage initiation sites. In this work, the effect of adherend recessing at the overlap edges on the tensile strength of SLJ, bonded with a brittle adhesive, was experimentally and numerically studied. The recess dimensions (length and depth) were optimized for different values of overlap length (L _O), thus allowing the maximization of the joint's strength by the reduction of peak stresses at the overlap edges. The effect of recessing was also investigated by a finite element (FE) analysis and cohesive zone modelling (CZM), which allowed characterizing the entire fracture process and provided joint strength predictions. For this purpose, a static FE analysis was performed in ABAQUS® considering geometric nonlinearities. In the end, the experimental and FE results revealed the accuracy of the FE analysis in predicting the strength and also provided some design principles for the strength improvement of SLJ using a relatively simple and straightforward technique.     

The effects of overlap length and adherend thickness on the strength of adhesively bonded joints subjected to bending moment

In this work, elasto-plastic stress analysis of a Single Lap Joint (SLJ) subjected to bending moment was investigated using 2D non-linear Finite Element Analysis (FEA). The SLJs, consisting of hardened steel as the adherend bonded by two adhesives, one stiff and one flexible, with very different mechanical behaviors were analyzed. In order to determine the effect of geometrical parameters on the performance of the SLJs, four different adherend thicknesses and overlap lengths for each adhesive were used. For verification of the analysis, the FEA results were compared with experimental results. It was observed that there was a significant effect of adherend thickness on the strength of the joint with both adhesives. However, the load carried by the SLJ with the flexible adhesive increased with increasing overlap length.     

Sealing glass‐ceramics with near‐linear thermal strain,part III: Stress modeling of strain and strain rate matched glass‐ceramic to metal seals

Thermal mechanical stresses of glass‐ceramic to stainless steel (GCtSS) seals are analyzed using finite element modeling over a temperature cycle from a set temperature (T_set) 500°C to ?55°C, and then back to 600°C. Two glass‐ceramics having an identical coefficient of thermal expansion (CTE) at ~16 ppm/°C but very different linearity of thermal strains, designated as near‐linear NL16 and step‐like SL16, were formed from the same parent glass using different crystallization processes. Stress modeling reveals much higher plastic strain in the stainless steel using SL16 glass‐ceramic when the GCtSS seal cools from T_set. Upon heating tensile stresses start to develop at the GC‐SS interface before the temperature reaches T_set. On the other hand, the much lower plastic deformation in stainless steel accumulated during cooling using NL16 glass‐ceramic allows for radially compressive stress at the GC‐SS interface to remain present when the seal is heated back to T_set. The qualitative stress comparison suggests that with a better match of thermal strain rate to that of stainless steel, the NL16 glass‐ceramic not only improves the hermeticity of the GCtSS seals, but would also improve the reliability of the seals exposed to high‐temperature and/or high‐pressure abnormal environments.     

Thermal residual stresses in an adhesively-bonded functionally graded single-lap joint

This study investigates three-dimensional thermal residual stresses occurring in an adhesively-bonded functionally graded single-lap joint subjected to a uniform cooling. The adherends are composed of a through-the-thickness functionally graded region between Al₂O₃ ceramic and Ni metal layers. Their mechanical properties were calculated using a power law for the volume fraction of the metal phase and a 3D layered finite element was implemented. In a free single-lap joint the normal stress σ_xx was dominant through the overlap region of the upper and lower adherends and along the adhesive free edges, whereas the transverse shear stress σ_xy concentrations appeared only along the free edges. The peel stress σ_yy and the transverse shear stress σ_xy became dominant along the free edges of the adhesive layer. In addition, the von Mises stress decreased uniformly through the adherend thickness from compressive in the top ceramic-rich layer to tensile in the bottom metal-rich layer. In addition, the layer number had only a minor effect on the through-the-thickness stress profiles after a layer number of 50, except for the peak stress values in the ceramic layer. In a single-lap joint fixed at two edges both adherends underwent considerable normal stress σ_xx concentrations varying from compressive in the top ceramic-rich layer to tensile in the bottom metal-rich layer along the free edges of both adherend–adhesive interfaces, whereas the peel stress σ_yy and transverse shear stress σ_xy reached peak levels along the left and right free edges of the adhesive layer. The layer number and the compositional gradient exponent had only minor effects on the through-the-thickness von Mises stress profiles but considerably affected the peak stress levels. The free edges of adhesive–adherend interfaces and the corresponding adherend regions are the most critical regions, and the adherend edge conditions play more important role in the critical adherend and adhesive stresses. Therefore, the first initiation of the joint failure can be expected along the left and right free edges of the upper and lower adherend–adhesive interfaces.     

Steel-Epoxy Composite Joints Bonded with Nano-TiO2 Reinforced Structural Acrylic Adhesive

This article reports a study on the effect of TiO₂ nanoparticles on the adhesion strength of steel–glass/epoxy composite joints bonded with two-part structural acrylic adhesives. The introduction of nano-TiO₂ in the two-part acrylic adhesive led to a remarkable enhancement in the shear and tensile strength of the composite joints. The shear and tensile strengths of the adhesive joints increased with adding the filler content up to 3 wt.%, after which it decreased with adding more filler content. Also, addition of nanoparticles caused a reduction in the peel strength of the joints. Differential scanning calorimeter analysis revealed that glass transition temperature (T_g) values of the adhesives rose with increasing the nano-filler content. The equilibrium water contact angle decreased for adhesives containing nanoparticles. Scanning electron microscope micrographs revealed that addition of nanoparticles altered the fracture morphology from smooth to rough fracture surfaces.     

Non-linear stress and failure analyses of adhesively-bonded joints subjected to a bending moment

In this paper, the mechanical behavior of the Single-Lap Joints (SLJs) bonded with two different adhesives (FM 73 and SBT 9244) under a bending moment was analyzed, both experimentally and numerically. Four-point bending experiments for the joints with different overlap lengths were carried out and fracture surfaces of the SLJs were examined with a Scanning Electron Microscope (SEM). After the stress analysis in the SLJs was performed via a finite element method by considering the material non-linearities of the adhesives and adherend (AA2024-T3), the Finite Element Analysis (FEA) results were compared with experimental results. Finally, the stress analyses and experimental results show that the failure in the SLJs subjected to a bending moment probably initiates from the overlap region on the adhesive–upper adherend interface in tension and propagates towards the centre of the overlap. Also, in the joint subjected to a bending moment, it is seen that the load carried by the SLJ with SBT 9244 adhesive with increasing overlap length is more than that of the SLJ with FM 73 adhesive, although in the bulk form FM 73 adhesive is about three times stronger than SBT 9244 adhesive.     

Variable temperature cure polyetherimide epoxy-based prepreg systems

This work identifies the necessary attributes of variable temperature cure epoxybased prepreg systems as they relate to high performance prepreg systems capable for composite repair. Model polyetherimide epoxy blend resins were developed and hot-melt impregnated into woven carbon fabric and compared with a commercial prepreg system. It was found that when the PEI content was increased from 0 to 14 wt% in the base resin of the prepregs, the G_IC and G_IIC fracture toughness increased by over 70%. The fracture toughness was found to be similar when the model prepreg was cured at either 121°C or 177°C, a result of only a 9% difference in conversion and complete phase separation of the PEI at both cure temperatures. Void content in vacuum cured laminates were found to decrease as the PEI content was increased because of a large quantity of resin in the interstitial areas between the longitudinal and transverse tows. A comparison of the model and commercial prepreg system demonstrated many similarities and some significant differences. For example, the commercial prepreg had a 15% difference in conversion when cured at 121°C versus 177°C and very little PEI phase separation after both cure cycles. As a result, a significant difference in G_IIC for the commercial prepreg was observed for the two cure temperatures.