The effect of curing temperature on thermal,physical and mechanical characteristics of two types of adhesives for aerospace structures

The effects of cure temperatures on the thermal, physical and mechanical characteristics of two types of thermosetting structural epoxy film adhesives were determined in detail. The aim of this paper is to assess the effect of cure temperatures (82–121 °C) on the degree of cure of the two adhesives and the relevant void formations that need to be addressed in bonded part production and repair. Two thermal parameters were used to characterize the advancement of the reaction, such as degree of cure and glass transition temperature. The joint properties with respect to the cure temperatures were characterized by void content and bond-line thickness measurements and lap shear strength tests. Experimental results presented that all lap shear strengths were well within minimum shear strength (29 MPa) required by the specification of the film-type adhesive. However, the lap shear strength testing after aging at 82 °C and 95%R.H for 1000 h showed that the improved durability when the adhesive is cured at 121 °C did not occur for the 82 °C cure. Low curing conversion (75–77% degree of cure) combined with high voids (over 2 areal%) has a catastrophic effect on the bonding qualities at the metal-adhesive interface and due to lack of cohesion in the adhesive. The changes in the interface caused by the low temperature curing may contribute to an increased susceptibility of the bonded joint to moisture and consequent bond-line degradation.     

Tensile strength of two-part epoxy paste adhesives: Influence of mixing technique and micro-void formation

Two-part epoxy paste adhesives are frequently used to bond metals and composite materials in many structural applications. After mixing two reactive parts (by weight or volume ratio), adhesive paste is applied to the substrate surfaces and cured at elevated temperatures. Air-entrapment during mixing and/or application process often produces micro-voids in the adhesive bondlines and influences the strength of the bonded joints. In this work, void formation was investigated using two adhesive mixing techniques: (a) dual-cartridge and static-mixer with a dispenser and (b) hand-mix. Flat adhesive sheets were cured by mixing a two-part epoxy adhesive, and bulk specimens with notches were cut using CNC-machining. Using X-ray microtomography scans, the micro-voids were detected and material porosity was evaluated. Furthermore, tensile tests were performed on the specimens and two-dimensional digital image correlation (2D DIC) was employed to analyse the surface strain concentrations near the notches. The fracture surfaces were examined using optical and scanning electron microscopy. The results indicated that mixing technique influences the formation of micro-voids and thus the tensile strength of two-part epoxy paste adhesives.     

胶接接头在静态负载条件下的蠕变和松弛行为

Modern high performance adhesives are designed to offer an optimized balance of elasticity,toughness and plastic deformation capacity for the individual fields of application in e.g. the building and construction or transportation and vehicle industry. The long-term life prediction for adhesive joints based on laboratory tests requiring only days,weeks,or months is still a demanding challenge. Testing in practice is carried out with the intention of accelerating time dependent aging effects that may occur in a bonded joint during its service time. Initial strength values of bonded joints,such as shear or peel properties can often be obtained from the adhesive manufacturers or retrieved from literature. They are useful to compare different adhesives and to demonstrate the effect of parameters such as bond line thickness,overlap length or curing conditions,and,in some cases,the surface state. On the other hand only few data are available describing the mechanical long-term properties of adhesives related to creep and relaxation under static load conditions. Due to the nature of the polymer network of organic adhesives their viscoelastic-plastic deformation behavior is strongly time-and temperature dependent. The objective of this paper is to illustrate effective methods for investigating and predicting the creep and relaxation properties of adhesively bonded joints in the long-term region and for creating basic data for the design and engineering with adhesives.     

新型可见光固化口腔正畸粘合剂研制

介绍了一种新型可见光固化正畸粘合剂的组成、性能及正畸粘接的工艺。此粘合剂由一种单组分液体底胶和单组分糊剂组成。与化学固化粘合剂相比,其操作使用方便,固化时间短。这种新型粘合剂的粘接强度完全满足了正畸粘合剂的要求。     

Statistical aspects of the mechanical behaviour a paste adhesive

We present experimental results describing the mechanical behaviour of an epoxy-based structural paste adhesive with aluminium powder filler under proportional loading. The main aim of the present study is to relate the dispersion on joint strength (variability) to void and particle sizes and distributions, also taking into account effects of the curing cycle. Tensile tests with dogbone specimens were done at different strain rates. The statistical nature of results is related to the heterogeneous material microstructure, containing voids as well as mineral particles for reinforcement. A Weibull-type statistical analysis is suggested for use when the stress distribution is heterogeneous. Mechanical dynamical analyses were done with evaluation of polymerisation steps. Multiple dynamical testing was done with temperature scanning on samples having undergone various cure cycles.     

Investigating tensile behaviour of toughened epoxy paste adhesives using circumferentially notched cylindrical bulk specimens

Toughened epoxy adhesives are frequently used to bond metals and polymer-matrix composite materials in many structural applications. The mechanical properties of adhesives are often characterised by testing either bulk adhesive specimens or bonded joints (i.e. in-situ form). In this paper, cylindrical bulk specimens with circumferential notches were manufactured and tested to investigate the tensile behaviour of an epoxy paste adhesive toughened with hollow glass microspheres. Bulk specimens were manufactured from the paste adhesive using injection moulding. Tensile tests were conducted for strain-rate and stress triaxiality effects by varying displacement rates and notch radii, respectively. Fracture surfaces were examined using optical and scanning electron microscopy to identify failure mechanisms. The results obtained from the toughened paste adhesive indicate that strain-rate and stress triaxiality influence its tensile fracture behaviour.     

Assessment and prediction of long-term mechanical properties of adhesives with high plasticity

Long-term life prediction for adhesives based on laboratory tests requiring only days, weeks, or months, is still a demanding challenge. Testing is carried out with the intention of simulating and often accelerating time-dependent aging effects that may occur in a joint during its lifetime. Initial strength values of bonded joints, such as shear or peel properties, can often be obtained from the adhesive manufacturers or retrieved from the literature. They are useful to compare different adhesives and to demonstrate the effect of parameters such as bondline thickness, overlap length or curing conditions and, in some cases, also the surface state. On the other hand, only few data are available relative to the long-term mechanical properties of adhesives with high plasticity. Due to the specific network structure of elastomer adhesives their viscoelastic-plastic deformation behavior is strongly time- and temperature-dependent. Therefore, the main objective of this paper is to illustrate methods for investigating the viscous properties of elastomer-based adhesives and creating basic data for the design and engineering of adhesive joints with enhanced plasticity.     

Influence of the mechanical behaviour of different adhesives on an interference-fit cylindrical joint

Hybrid adhesive joining techniques are often used in many industrial sectors to design lightweight structures. A hybrid adhesive joint results from the combination of adhesive bonding with other traditional joining methods such as welding and mechanical fastening, with the aim of combining the advantages of the different techniques and overcoming their drawbacks.This study focuses on the interference fitted/adhesive bonded joining technique. In this application, two cylindrical components are coupled together by inserting one into the other, after having placed an adhesive between them. Generally anaerobic acrylic adhesives, also known as “retaining compound” are used for this application. However the effect of the adhesive nature and of its mechanical and adhesive responses on the performance of the hybrid joint is still unclear. The aim of the present research is to improve the understanding of the behaviour of different adhesives, including rigid epoxies and flexible polyurethanes, in the presence of an interference-fit. Static strength of bonded and unbonded interference fit joints have been compared in order to investigate the role of the different adhesives.     

Susceptor-assisted induction curing behaviour of a two component epoxy paste adhesive for aerospace applications

The curing behaviour and the mechanical behaviour of susceptor-assisted induction-cured adhesively bonded joints has been investigated. Induction Heating (IH) was established by mixing Iron particles into a two component epoxy paste adhesive. The effect of different process parameters, such as particle content, coupling distance and coil current, on the IH curing process was evaluated by experimental tests and simulation of the induction heating process in COMSOL multiphysics. The process simulation showed that hysteresis losses has a major contribution for the heat generation of IH using Iron particles. Differential scanning calorimetry (DSC) analysis was used to assess the effect of susceptor particles on the cure behaviour of the adhesive. The results showed that the Iron particles do not interfere with the curing process of the epoxy adhesive in scope.The mechanical performance was evaluated through Single Lap-Shear (SLS) testing at different volume-percentages of Iron particles in combination with glass fibre reinforced plastic (GFRP) adherends. Induction-cured SLS samples were compared with conventional oven-cured SLS samples. In the oven cured samples, the addition of Iron particles resulted in a decrease in the lap-shear strength of 15% to 20%, even for a volume-percentage as low as 0.5%. An additional increase in particle content up to 7.5 v% did not show any additional reduction in the lap-shear strength. Furthermore, results show that when curing the adhesive layer from the inside, as in the susceptor-assisted induction heating, the lap-shear strength is 6% higher than in oven-cured samples (curing the adhesive layer from the outside).     

Strength prediction of adhesively bonded joints under cyclic thermal loading using a cohesive zone model

Structural adhesives are being widely adopted in aerospace and automobile industries. However, in many cases, hostile environments cause non-ignorable degradation in joints mechanical performance. In this work, a combined experimental–numerical approach was developed to characterise the effect of cyclic-temperature environment on adhesively bonded joints. The environmental degradation factor, Deg, was introduced into a cohesive zone model to evaluate the degradation process in the adhesive layer caused by the cyclic-temperature environment and the stress states in adhesive layer before and after temperature exposure treatment were investigated. Carefully designed experimental tests were carried out to validate the simulation results and help the numerical procedure to predict joint mechanical behaviour after environmental exposure. A response surface method was utilised to provide a better visualisation on the relationship between selected factors and response. Finally, the scanning electron microscopy was carried out to investigate the micro fracture mechanisms of adhesively bonded joints.     

Bonding Optimization on Composite Surfaces using Atmospheric Plasma Treatment

The effect of atmospheric plasma treatment (APT) on the bonding performance of a cyanate ester and an epoxy carbon fiber reinforced composite fabricated with a polyester peel ply was evaluated. A room temperature (RT) cured epoxy, an elevated temperature cured epoxy, and a cyanate ester resin, were used as the bonding adhesives. Only small increases in the carboxyl species concentration were observed for both composite systems as a function of increasing plasma treatment. Lap shear (LS) tests of the bonded composites showed that the APT resulted in a 30% strength improvement for the RT cured epoxy bonded specimens while the cyanate ester composite exhibited negligible increases due to the formation of a highly oxidized, weakly bonded ash. Contact angle measurements indicated that the temperature exposure associated with the curing of the elevated temperature adhesives also reduced the efficacy of APT. Modifications of the bonding surface of these composites by the incorporation of a plasma responsive (PR) layer resulted in significant LS improvements. After incorporating the PR layer, the improvement in adhesive strength was over 225% that of an untreated specimen and approximately 190% that of the equivalently treated unmodified system. Bond strengths correlated with corresponding increases in carboxyl concentrations after APT.     

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.     

Benchmark tests on adhesive strengths in butt, single and double lap joints and double-cantilever beams

The RC99 committee of the Japan Society for Mechanical Engineers conducted the benchmark tests on strengths of adhesive joints using different testing methods. The effects of joint configuration, loading mode, adherend yield strength and so on, on the strength and data scatter were investigated using two typical epoxy adhesives. The strengths obtained by various tests were compared with each other. The relationships among strengths of butt, single lap and double lap joints and fracture toughness were given. Thirteen member institutes of the committee participated in this project. The benchmark results allow us to recognize that the joint strengths are strongly affected by the curing process. The key to obtaining the appropriate joint strength, is precise temperature control inside the adhesive layer for curing. Toughened adhesives do not always give higher joint strengths than untoughened adhesives. The yield strength of adherends much affects the observed lap joint strength of adhesives.     

A design of experiments assessment of moisture content in uncured adhesive on static strength of adhesive-bonded galvanized SAE1006 steel

As part of a cooperative research program to develop and implement crash-resistant toughened adhesives targeted for future vehicles, this paper summarizes a study of the influence of pre-exposure of uncured adhesive and steel sheets in a humid and elevated temperature environment on quasi-static strength of bonded hot dipped galvanized SAE1006 steel joints.In this study, we use a DOE (design-of-experiment) program called DEXPERT to design the experiment and to analyze the effects of exposure temperature, exposure time, curing temperature and curing time on joint strength of adhesive-bonded galvanized SAE1006 steel. Prior to adhesive curing, the adhesive and galvanized steel coupons were pre-exposed to various relative humidity levels and temperatures. The experimental results were then analyzed by DEXPERT and the relative contributions of each factor on variance in joint strength were calculated. It was found that curing temperature is the most influential factor affecting the strength of adhesive-bonded galvanized SAE1006 steel joints. The curing of a joint at 180 °C can increase the robustness of the process and provides the greatest strength regardless of the variation of other factors. The joint strength curing at 150 °C shows a strong sensitivity to the curing time, while the adhesive cannot cure at 130 °C at all under all conditions. It has also been found that the pre-exposure of adhesive and steel for an hour can slightly decrease the joint strength at high temperature and humidity. Therefore, the effect of long time exposure of the uncured adhesive and steel still needs to be further investigated.     

Strengthening of the adhesive bond using a mixture of adhesives between dissimilar adherends in a single lap joint

Abstract

Adhesive bonding is the best alternative to riveting in aircraft structures but the strength of the adhesive bonded joint is low and is limited by strength of adhesive. Strengthening of adhesive bonding is an important requirement. In this work, an attempt has been made to strengthen the adhesive bonding by mixing different quantities of brittle adhesive in the ductile adhesive and vice-versa. Two different adhesives, one brittle (AV138) and another ductile (Araldite-2015) adhesive have been considered. Initially single lap joint has been constructed between the CFRP and aluminium with individual adhesives, then the mixture of adhesives have been used in the bonded region in varied proportions. The X-ray radiography and ultrasonic testing have been performed to check the quality of bonding. Uniaxial tensile tests have been conducted on the lap joints along with Digital Image Correlations (DIC) to obtain the individual and mixed adhesive bond strength. The failure patterns have been identified using optical and scanning electron microscope. These studies indicate that strengthening of the adhesive bonding achieved by mixing of two adhesives and highest bond strength obtained when the mixture of AV138 and Araldite-2015 adhesives are used in equal proportions.     

Adhesive distribution related to mechanical performance of high density wood fibre board

In a full-scale mill experiment two groups of high density wood fibre boards were produced. While one group was bonded with a standard melamine reinforced urea-formaldehyde adhesive, a second group was bonded with a modified adhesive yielding systematically improved board properties at identical amounts of adhesive applied. By means of a novel fluorescence-microscopic method using the dye Acriflavine to colour the cured adhesive after board production, adhesive distribution within the industrial produced boards was evaluated and quantified. Very clear differences in the size distribution of the two adhesives were found, leading to the conclusion that a relationship exists between adhesive distribution and mechanical board performance.     

Process optimization of solvent based polybenzimidazole adhesive for aerospace applications

The use of adhesive bonding for high temperature applications is becoming more challenging because of low thermal and mechanical properties of commercially available adhesives. However, the development of high performance polymers can overcome the problem of using adhesive bonding at high temperature. Polybenzimidazole (PBI) is one such recently emerged high performance polymer with excellent thermal and mechanical properties. It has a tensile strength of 160 MPa and a glass transition of 425 °C. Currently, PBI is available in solution form with only 26% concentration in Dimethyl-acetamide solvent. Due to high solvent contents, the process optimization required lot of efforts to form PBI adhesive bonded joints with considerable lap shear strength. Therefore, in present work, efforts are devoted to optimize the adhesive bonding process of PBI in order to make its application possible as an adhesive for high temperature applications. Bonding process was optimized using different curing time and temperatures. Epoxy based carbon fiber composite bonded joints were successfully formed with single lap shear strength of 21 Mpa. PBI adhesive bonded joints were also formed after performing the atmospheric pressure plasma treatment of composite substrate. Plasma treatment has further improved the lap shear strength of bonded joints from 21 MPa to 30 MPa. Atmospheric pressure plasma treatment has also changed the mode of failure of composite bonded joints.     

室温固化高性能胶粘剂的研制

为了改善环氧树脂(EP)胶粘剂对某些金属和非金属材料的粘接性能,采用自制的增韧剂改性EP,制备了一种可室温固化的无溶剂双组分EP胶粘剂。考察了增韧剂用量、不同的室温固化剂及表面处理方法对金属和非金属材料的粘接性能、耐热性能和耐介质性能的影响。实验结果表明,该胶粘剂对金属和非金属都具有良好的粘接性能;用于PVC和ABS粘接时,则被粘材料被破坏;用于聚四氟乙烯(PTFE)和聚乙烯(PE)粘接时,其最高剪切强度分别为1.9 MPa和1.8 MPa。     

Impact of curing condition on pH and alkalinity/acidity of structural wood adhesives

Nine formulations were selected for evaluating the effect of different curing methods on pH and alkalinity or acidity of various structural wood adhesives. These included four phenol–formaldehyde (PF) resins with high pH, one phenol–resorcinol–formaldehyde (PRF) resin with intermediate pH, two melamine–urea–formaldehyde (MUF) resins, and two melamine–formaldehyde (MF) resins with low pH. The four curing methods used in the study were: (1) curing at 102–105°C for 1 h (based on CSA O112.6‐1977), (2) four‐hour curing at 66°C followed by 1‐hour curing at 150°C (based on ASTM D1583‐01), (3) curing at room temperature overnight (based on ASTM D 1583‐01), and (4) cured adhesive squeezed out from glue lines of bonded shear block samples. The effect of the different methods on pH and alkalinity/acidity of the cured adhesive depended strongly on the individual adhesives. For the PF, the alkalinity was different for the different formulations in the liquid form, while in the cured form, the difference in the alkalinity depended on the curing method used. The MF and the MUF were the adhesives most affected by the method used. In particular, the MUF showed much higher cured film pH values when cured by method 2 compared to the other three methods, while both the cured MF and MUF exhibited quite variable acidity values when cured with the different methods. The PRF showed reasonably uniform cured film pH but varying acidity values when cured with the different methods. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Room Temperature Curing Epoxy Adhesives for Elevated Temperature Service

Room Temperature curing compositions of epoxy resins with high temperature service capability (95-120°C) were formulated and evaluated. The compositions were based on selected high functionality atomatic epoxy polymers and multicomponent poly amine curing agent systems. Toughening was achieved by addition of a rubbery phase either by prereaction of the epoxy resin with carboxyl terminated (CTBN) or by amine terminated (ATBN) poly butadiene acrylonitrile. The latter elastomeric component served as a part of the poly amine curing agent.

Best results were achieved with an adhesive formulation comprising tetra glycidyl-4-4'-diaminodiphenylmethane (TGDDM) and triglycidyl ether of p-aminophenol with triethylenetetramine and addition of ATBN with a felt carrier.

Lap shear strengths of aluminum/aluminum specimens primed by silane coupling agent in the order of 22 MPa at 25°C and 11 MPa at 120°C with T-Peel strengths of 1.6N/mm at 25°C and 0.52 N/mm at 120°C, were obtained.

The thermal behaviour and transitions, the chemical and mechanical properties, the microstructure and morphology of the selected adhesive formulation were studied, using DSC, Gehman, FTIR, mechanical testing and SEM analysis, respectively.

Experimental results showed that the selected compositions could develop good high temperature (120°C) properties while cured at room temperature. Furthermore, their high temperature performance compares favorably or even exceeds that of commercially available room-temperature-curing adhesive compounds, and are competitive with elevated temperature cured film adhesives.