Structural health monitoring of an adhesive disbond through electromechanical impedance spectroscopy

The aerospace industry continues to increase the use of adhesives for structural bonding due to the increased joint efficiency (reduced weight), even distribution of the load path and decrease in stress concentrations. However, the limited techniques for verifying the strength of adhesive bonds has reduced its use on primary structures and requires an intensive inspection schedule. This paper discusses a potential structural health monitoring (SHM) technique for the detection of disbonds through the in situ inspection of adhesive joints. This is achieved through the use of piezoelectric wafer active sensors (PWAS), thin unobtrusive sensors which are permanently bonded to the aircraft structure. The detection method utilized in this study is the electromechanical impedance spectroscopy, a local vibration method. This method detects disbonds from the change in the mechanical impedance of the structure surrounding the disbond. This paper will discuss how predictive modeling can provide valuable insight into the inspection method, and provide better results than purely empirical methods will provide. A method for identifying the appropriate frequency range and sensor locations is presented, and the method was verified experimentally using a large aluminum test article, and included both pristine and disbond coupons.     

人造板胶粘剂现场固化监测系统

介绍了人造板胶粘剂现场固化监测的系统组成,尤其对同面叉指电极电容传感器涉及的边缘电场、电极电容形态参数的计算方法以及测量终端连线方法等进行了分析.利用该介电测量方法可以准确了解人造板胶粘剂在实际热压时的固化开始温度和时间,对改进现有胶粘剂配方、优化热压工艺曲线具有明确的指导作用.     

Methodology for optimization of the curing cycle of paste adhesives

This contribution, carried out in the frame of the European Joint Technology Initiative ‘Clean Sky’, presents the results of a research program investigating the influence of fast curing on the quality of epoxy based paste adhesives. Today, the curing of paste adhesives is typically carried out following the supplier's recommendations. In order to reduce cycle time, save costs and energy resources, paste adhesives could be cured at higher temperature. To ensure a bonded joint quality with maximum mechanical performance, the limitation of this temperature increase is studied. This study shows the effects of the use of high temperatures in the curing process, which can lead to a degradation of the adhesive system due to the increase of void content, decreasing the mechanical performance in the paste adhesive as well as in the bonded joint. The goal of this research is to find fast and robust processing of paste adhesives and to develop a methodology to determine the maximum curing temperature possible. Different properties of the adhesive are investigated, including different thermal analysis techniques, optical and mechanical testing of the pure adhesive. Additionally, state of the art qualification of paste adhesives, single lap shear testing, is considered. In this study, a novel method to control the quality of the cured paste adhesives is defined based on the analysis of the pure cured paste adhesive, not influenced by the adherent quality, by measuring the void content and its effects on the bonded joint.     

Diagnosis criterion for damage monitoring of adhesive joints by a piezoelectric method

Adhesive joints have been widely used for fastening thin adherends because they can distribute the load over a larger area than mechanical joints, require no holes, add very little weight to the structure and have superior fatigue resistance. Since the reliability of an adhesive joint is dependent on many parameters, such as the shape of joint, type of applied load and environment, an accurate prediction of the fatigue life of adhesive joints is seldom possible, which necessitates an in situ damage monitoring of the joints during their operation. Recently, a piezoelectric method using the piezoelectric characteristics of epoxy adhesives has been successfully developed for adhesive joints because it can continuously monitor the damage of adhesively bonded structures without producing any defects induced by inserting a sensor. Therefore, in this study, the damage of adhesive joints was monitored by the piezoelectric method during torsional fatigue tests in order to develop the diagnosis criterion for damage monitoring of adhesive joints by the piezoelectric method. The diagnosis criterion was developed by analyzing damage monitoring signals under various test conditions and adopting normalized parameters.     

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.     

Lowering curing temperature in adhesive bonding of aluminum AA6061-T4

ABSTRACT

To minimize the part distortion and investment in the E-coat oven in adhesive bonding of metals for automotive applications, lowering the curing temperature of adhesive without apparent loss of the joint strength is desirable. The key to lower the curing temperature of adhesive bonding of lightweight materials is to accelerate the curing process of structural adhesives. In this study, curing agent (i.e., aliphatic polyamine) and curing accelerator (i.e., acetylacetone salt) were added into commercial Henkel 5089 adhesive and the effect of these curing additives on the curing temperature of Henkel 5089 in adhesive bonding of aluminum AA6061-T4 was studied. The test results showed that the addition of a curing agent and accelerator in Henkel 5089 lowered the curing temperature from 177°C to 130°C without sacrificing the strength of the adhesive-bonded aluminum AA6061-T4.     

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.     

Adhesive Bonding of Oil-Contaminated Steel Substrates

Durability of adhesive bonds formed by curing epoxies against oil-contaminated steel substrates using amidoamine curing agents was determined during exposure to boiling water. The most durable bonds were obtained using amidoamine curing agents with relatively low amine numbers and by blending silane coupling agents such as γ-glycidoxypropyltrimethoxysilane (γ-GPS) and N-(2-aminoethyl)-3-aminopropyltrimethoxy silane (AAMS) into the adhesives. When X-ray photoelectron spectroscopy (XPS) was used to characterize the failure surfaces of the adhesive joints after exposure to boiling water, it was determined that adhesives prepared using amidoamine curing agents with low amine numbers were able to displace the oil from the steel surface but adhesives prepared with amidoamine curing agents with high amine numbers were not. Results obtained from XPS also showed that the amino groups on the substrate fracture surfaces of joints prepared using curing agents with low amine numbers were protonated whereas the amino groups in the bulk adhesive were not, indicating that there was a chemical interaction between the curing agent and the hydrated surface of the substrate. It was also shown using infrared spectroscopy that the amidoamine curing agents formed salts with calcium compounds in the oil.     

Effect of adhesive on the performance of piezoelectric elements used to monitor structural health

The effect of adhesive thickness and its modulus on the performance of adhesively bonded piezoelectric elements for the purpose of monitoring structural health has been experimentally investigated. All the piezoelectric elements were adhesively bonded to aluminum plates. Experimental results revealed that an increase in adhesive thickness alters the electromechanical impedance and the resonant frequency of the piezoelectric elements as well as the amplitude of the sensor signal. When the modulus is within a certain range, the modulus of adhesive slightly affects the impedance of PZT element and the amplitude of sensor signal at lower frequency, while at high frequency, the impedance response and sensor signal are more sensitive to the modulus of adhesive.     

Adhesive Bonding of Clean and Oil-Contaminated Electrogalvanized Steel Substrates

The performance of two-part, amidoamine-cured epoxy adhesives on clean and oil-contaminated electrogalvanized steel (EGS) was studied using screening and lap shear tests. On exposure to boiling water, the cured epoxy adhesives with amidoamines having higher amine value delaminated from the clean and oil-contaminated EGS surfaces before those cured with amidoamines having low amine value. The results of X-ray photoelectron spectroscopy (XPS) showed that the adhesives cured with amidoamines having high amine value were unable to displace the oil from the EGS substrate. However, the durability and the strength of the adhesive bonds on the oiled EGS could be improved by adding proper amounts of silane or wetting agent to the adhesive. The preferential adsorption of amino curing agents occurred on the clean EGS surface, confirmed by XPS and reflection absorption infrared spectroscopy, and this decreased the durability of the bonds in boiling water. In addition, from XPS analyses of various specimens, different amounts of cured resins were detected in the adhesive/EGS interfacial regions which affecting the durability of the adhesive bonds. In addition, the amidoamine curing agents may form complexes on the EGS surface.     

Alkali catalysed curing of starch-melamine resin systems

Summary The curing process in starch adhesives modified with melamine resin can take place by co-condensation or self-condensation. A high degree of co-condensation is required to provide a good water resistance of a cured glue joint. This can be attained by using melamine resins with a high concentration of hydroxymethylamino groups. The reduced effect of the adhesive on storage is due to a degradation of the melamine resin through the elimination of formaldehyde.     

Adhesive Bonding of Oil-Contaminated Steel Substrates

Durability of adhesive bonds formed by curing epoxies against oil-contaminated steel substrates using amidoamine curing agents was determined during exposure to boiling water. The most durable bonds were obtained using amidoamine curing agents with relatively low amine numbers and by blending silane coupling agents such as γ-glycidoxypropyltrimethoxysilane (γ-GPS) and N-(2-aminoethyl)-3-aminopropyltrimethoxy silane (AAMS) into the adhesives. When X-ray photoelectron spectroscopy (XPS) was used to characterize the failure surfaces of the adhesive joints after exposure to boiling water, it was determined that adhesives prepared using amidoamine curing agents with low amine numbers were able to displace the oil from the steel surface but adhesives prepared with amidoamine curing agents with high amine numbers were not. Results obtained from XPS also showed that the amino groups on the substrate fracture surfaces of joints prepared using curing agents with low amine numbers were protonated whereas the amino groups in the bulk adhesive were not, indicating that there was a chemical interaction between the curing agent and the hydrated surface of the substrate. It was also shown using infrared spectroscopy that the amidoamine curing agents formed salts with calcium compounds in the oil.     

Techniques for screening adhesives for structural applications

—Due to its chemistry, no structural adhesive system (epoxies, acrylics, etc.) is likely to offer an ideal combination of toughness, strength, moisture resistance, and ambient-temperature curing. Therefore, for effective use of adhesives in primary structures, an engineer must be able to identify adhesives that represent an optimum compromise among the different properties. In this paper, we present techniques for screening high-strength, ambient-temperature-curing adhesives for (1) moisture resistance under sustained loading and (2) fracture resistance in a way that is directly related to joint performance.     

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.     

Polyetherimide Adhesive

High-temperature adhesives which can be adhered at adhesive temperatures lower than those of conventional polyimide adhesives were investigated. Polyetherimide (PEI), developed by General Electric Co., is one such promising low curing temperature adhesive because it melts at temperatures lower than those used for conventional polyimides. Lap shear adhesive strength was investigated in a 75 μm-thick PEI film using steel test pieces. 350 kgf/cm² was achieved after curing for 1 hour at 270°C and 150 kgf/cm² was achieved at the test temperature of 200°C. PEI adhesive dissolved by N, N-dimethylformamide exhibited a high adhesive strength of 240 kgf/cm² after curing for 2 hours at 200°C. In addition, it was found that PEI could be used at much lower adhesive pressures than those of conventional polyimide adhesives.     

硅笼改性耐热厌氧胶的制备及其固化动力学

为提高厌氧胶的热性能,用二步法合成了邻甲酚醛环氧丙烯酸酯(o-CFEAR),并以该树脂为单体,不饱和笼型倍半硅氧烷(POSS)为耐高温改性剂,选择合适的氧化还原体系及其它助剂,制成耐高温厌氧胶,测定了相关性能,研究了该胶的固化动力学。结果表明,此厌氧胶剪切强度最高达15.3 MPa,在200℃、96 h时剪切强度保持率为87%左右,耐高温性能良好;固化过程的反应级数为1.084 9,表观活化能为86.86 kJ/mol。     

Experimental and theoretical study of a fast curing adhesive

In semiconductor industry the application of fast curing adhesives with curing times below 20 s is necessary for cost-effective production of electronic packages at high throughput. For the curing process control as well as for the selection of appropriate adhesives, adequate analytical tools, which enable the measurement of fast curing reactions under package assembly conditions are essential. In this study, the curing behaviour of a commercially available adhesive, chemically based on an epoxy compound was examined by means of dielectric analysis (DEA) and differential scanning calorimetry (DSC). For the DEA method we developed an experimental set-up with similar temporal and thermal conditions as for the observed curing behaviour during the package production process. Formal kinetic analysis was performed of the isothermal DEA and the non-isothermal DSC data and kinetic models and parameters were derived and compared. This study revealed, that both measuring methods, the DEA and the DSC gain important information for characterising this curing system, although different kinetic models were found for the two methods. With the DEA method it was possible to determine an optimal curing temperature for the adhesive at process near experimental conditions.     

翼身融合体小型无人机胶接技术研究

本文介绍了翼身融合体无人机的胶接技术。详述了翼身融合体无人机的结构特点及其主要零、组件的材料构成。重点介绍了胶接用胶黏剂的选择依据、翼身融合体无人机的胶接工艺条件及几种适用的胶黏剂基本性能。同时简述了无人机的装配胶接工艺过程,包括产品零件预装配、表面处理的影响因素及不同材料所采用不同的处理工艺、胶黏剂的涂覆及装配与固化等工艺过程。经过几十架次的试验飞行证明此胶接技术胶接可靠,能满足飞行要求。     

Electrochemical Sensors for Nondestructive Evaluation of Adhesive Bonds

An in-situ corrosion sensor based on electrochemical impedance spectroscopy (EIS) has been used to detect moisture ingress into aluminum-aluminum and aluminum-composite adhesive bonds. Both wedge tests and tensile button tests (aluminum-aluminum bonds only) were performed. Upon moisture absorption, the impedance spectra change shape with the low-frequency region becoming resistive. The low-frequency impedance decreases by several orders of magnitude, depending on the adhesive and the experimental conditions. For bonds with stable interfaces, such as phosphoric acid anodized (PAA) aluminum, the absorbed moisture causes an initial weakening of the adhesive resulting in reduced strength or small crack propagation. A substantial incubation time prior to substrate hydration and bond degradation allows warning of potential joint deterioration and enables condition-based maintenance. For bonds with smooth interfaces with little or no physical bonding (mechanical interlocking), crack propagation can proceed interfacially with minimal moisture absorption. A comparison of the incubation times for Forest Products Laboratory (FPL, or sulfuric acid-sodium dichromate) etched surfaces, both bonded to epoxy adhesives and freely exposed to water or humidity at different temperatures, shows that hydration occurs with the same activation energy and, hence, the same mechanism, independent of whether or not the surface is covered with adhesive. However, the pre-exponential factor in the rate constant is dependent on the concentration of free moisture at the interface so that the hydration rate varies by several orders of magnitude.     

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.