LONG-TERM PHYSICAL AND MECHANICAL PROPERTIES OF COLD CURING STRUCTURAL EPOXY ADHESIVES
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1 LONG-TERM PHYSICAL AND MECHANICAL PROPERTIES OF COLD CURING STRUCTURAL EPOXY ADHESIVES Omar MOUSSA Title: Civil engineer, MSc. Affiliation: Composite Construction Laboratory (CCLab) École Polytechnique Fédérale de Lausanne (EPFL) Address: Station 16, Bâtiment BP, CH-1015 Lausanne, Switzerland address: Anastasios P. VASSILOPOULOS Title: Dr. Affiliation: Composite Construction Laboratory (CCLab) École Polytechnique Fédérale de Lausanne (EPFL) Address: Station 16, Bâtiment BP, CH-1015 Lausanne, Switzerland address: Julia DE CASTRO Title: Dr. Affiliation: Composite Construction Laboratory (CCLab) École Polytechnique Fédérale de Lausanne (EPFL) Address: Station 16, Bâtiment BP, CH-1015 Lausanne, Switzerland address: Thomas KELLER Title: Prof. Dr. Affiliation: Composite Construction Laboratory (CCLab) École Polytechnique Fédérale de Lausanne (EPFL) Address: Station 16, Bâtiment BP, CH-1015 Lausanne, Switzerland address*: Abstract Adhesive bonding is a material-tailored method used to connect structural components made of fiber-reinforced polymer (FRP) composites. Compared to mechanical connections, e.g. bolts, in this method stresses are gradually introduced into the polymer matrix of the adherend before being transferred through the matrix into the fibers. A characteristic of the construction industry is that joining is usually carried out on the construction site and therefore only coldcuring adhesives can be used. The physical and mechanical properties, e.g. the glass transition temperature, stiffness and strength, thus develop slowly as a function of the ambient curing temperature. In this paper, the results of a study concerning the long-term development of the physical and mechanical properties of cold-curing structural epoxy adhesives are presented. Property development is accelerated by post-curing and long-term predictions are compared to experimental results obtained from specimens up to seven years old. Keywords: Cold-curing adhesives, curing degree, DSC, epoxy resin, glass transition temperature, mechanical properties 1. Introduction Adhesive bonding is an advantageous connection technology already common in aerospace and automotive industries that also starts finding interest in the construction industry, particularly for joining composite elements. Developments were accomplished in the strengthening of structures by bonding fiber-reinforced polymer composite laminates onto existing concrete or steel components or joining structural elements fabricated from composite materials in new construction [1-2]. Researches have proved that the early age mechanical properties strongly depend on the physical state of the adhesive [3-5]. When applied during winter for instance at relatively low Page 1 of 8
2 temperature, development of thermophysical and consequently mechanical properties are much decelerated, particularly when the developed glass transition temperature, T g, approaches the curing temperature, T cure. In this case significantly long curing periods or postcuring are required in order to achieve higher level of properties [6-7]. The long-term curing behavior of a cold-curing structural adhesive is investigated in this paper. An accelerated experimental method based on post-curing of the adhesive at different temperatures is used to achieve a fully cured system. The corresponding mechanical properties and physical characteristics are observed. 2. Experimental work 2.1 Material A thixotropic bi-component epoxy adhesive Sikadur-330 supplied by Sika Schweiz AG was used. This adhesive contains a small quantity of silica-based fillers (<20% by weight, based on burn off of the adhesive). Components are mixed at room temperature at a ratio of 4:1 by weight of the respective constituents (resin and hardener). The tensile strength and modulus of elasticity of specimens cured at lab temperature and examined according to EN ISO are 38.1 MPa and 4.6 GPa respectively. The glass transition temperature exceeds according to the manufacturer s datasheets. This adhesive is fabricated for manual application to surfaces and is used to impregnate FRP fabrics employed to strengthen existing concrete or steel structures. 2.2 Experimental set-up and procedure Physical characterization A heat-flux differential scanning calorimeter (DSC-TA Q100) connected to a thermal analyzer was used to detect the heat released during the cure reaction. The DSC is equipped with a liquid nitrogen cooling system providing an inert atmosphere. DSC samples, each weighing 5-10 mg, were cured under laboratory conditions (T=23±5 C and RH=50±10%). Afterwards, post-curing at different temperatures and during different time periods was performed either outdoors, under laboratory conditions or in a climate chamber (details are given in Section 1.3). Samples were then left under laboratory conditions for 24 hours. The residual cure and the corresponding glass transition temperature were obtained by running a non-isothermal scan between -50 and 250 C at a heating rate of 5 C/min. Data acquisition was performed using the accompanying software (TA analysis) Mechanical characterization Tension specimens were fabricated in aluminium molds and examined according to ASTM D 638 as shown in Figure 1. Specimens were cured under laboratory conditions for two weeks. Post-curing of specimens was then carried out under different conditions (temperature and time as presented in Section 1.3) and then left for 24 hours under laboratory conditions. Tensile experiments were performed using an MTS Landmark 25-kN servo-hydraulic load unit calibrated to 20% of its load capacity. Longitudinal strains were measured using an MTS clip-on extensometer mounted across the specimen as shown in Figure 1b. The extensometer has a gage length of 25±0.05mm and minimum accuracy of ±0.5% of the measured strain. Experiments were performed in displacement control at a loading rate of 5mm/min according to the followed standard. Five specimens were examined for each condition and a minimum of three specimens results were considered in analysis after discarding defected specimens with flaws or voids and specimens exhibiting a tab failure. Page 2 of 8
3 W = 13 mm R = 76 mm WO = 19 mm G L = 57 mm T = 4 mm D = 115 mm D = 115 mm LO = 165 mm Figure 1: a) Specimens dimensions according to ASTM-D638 b) Experimental set-up 2.3 Experimental program In order to investigate the long-term change in T g, DSC samples were prepared from adhesive material cured under laboratory conditions during different time periods, t, of between 1 and 7 years as shown in Table 1. Similar samples were prepared from material exposed to outdoor curing (in Lausanne) between , in order to compare the results with those from samples cured under relatively controlled conditions in the laboratory. A minimum of two samples was examined for each condition. Table 1: Experimental program for DSC samples cured during several years Curing Condition Laboratory Outdoors t (yr) Physical Moreover, several sets of tensile specimens and DSC samples were examined according to the conditions shown in Table 2. The long-term development was simulated by post-curing at elevated temperatures, T pc. Table 2: Experimental program for post-curing of DSC samples and tensile specimens T pc ( C) Reference ~ 23 C t pc (hr) Physical Mechanical The tensile specimens and DSC samples from one set, denominated the reference set, were examined immediately after curing (no post-curing involved). The obtained strength and stiffness values and the corresponding glass transition temperature, T gl, were used as reference values during the analysis in order to observe the changes in properties after subjecting the material to various post-curing conditions. Three experimental groups representing post-curing at different temperatures are presented as follows: Group 1 consists of five sets of tensile specimens and DSC samples post-cured at during different time periods, t pc, between four and 168 hours. Page 3 of 8
4 Group 2 consists of three sets of tensile specimens and DSC samples post-cured at between 24 and 168 hours. Group 3 consists of two sets of tensile specimens only cured under laboratory conditions (~ 23 C) during 3 months and two years. Results from this group are used to verify the applicability of the experimental method (accelerated curing procedure). 3. Experimental results and discussion 3.1 Physical investigation The change in T g over a long-term period of up to seven years is presented in Figure 2. A quasi-linear increase of approximately 13% in T g took place between the period of one to seven years. This can be attributed to the increase in cure level (due to cross-linking) and/or the physical aging of the adhesive. Samples cured outdoors showed an additional supplementary increase in T g values due to their exposure to variable environmental conditions (which increases their aging) including wider temperature ranges (> 30 C during summers) compared to samples cured in the laboratory. It was not possible to precisely measure the curing degree, α, corresponding to these high T g values due to the difficulty in precisely monitoring the small residual cure that took place during the later stages of the curing process. However, according to experimental results, it can be concluded that a curing degree exceeding 98 % was achieved by all samples Lab temperature Outdoor 60 T g ( C) y = 0.76 x Time, t (years) Figure 2: Measured T g vs. time for samples cured for up to seven years The development of curing degree and T g vs. post-curing time is presented in Figures 3 and 4 during the post-curing of samples at 40 and (results from all experimental sets are shown). The curing degree increased from an average of 96.5% for samples cured for two weeks under laboratory conditions to above 98% and 99% for samples post-cured at 40 and respectively. Compared to T gl, an increase in T g of around 63% and 41% was observed when samples were post-cured for one week at 60 and respectively. Page 4 of 8
5 Curing degree, α (-) Post-curing time, t pc (hr) Figure 3: Curing degree vs. time for samples post-cured under different conditions T g ( C) fitting Post-curing time, t pc (hr) Figure 4: T g vs. post-curing time for samples post-cured at different temperatures The equivalent time, t eq, required to achieve a certain T g value when the adhesive is cured under laboratory conditions was determined by a logarithmic fitting of the experimental results expressing the change in T g over the long term (Figure 2). Figure 5 shows the equivalent curing time required at ambient temperature to attain similar T g values as those obtained by post-curing at 60 and. 3.2 Mechanical investigation The development of tensile strength and stiffness for specimens post-cured at 60 and is shown in Figures 6a and b respectively. By knowing the corresponding T g, the equivalent time required to achieve a certain property level under laboratory conditions was derived from Figure 5. An increase of 48% and 15% was attained for tensile strength and stiffness respectively by post-curing at for one week (168 hours), a condition which is equivalent to curing at ambient temperature during approximately 17 years. Page 5 of 8
6 80 70 T g ( C) y = 3.7Ln(x) fitting Equivalent time, t eq (years) Figure 5: Tg vs. equivalent time under laboratory conditions for samples post-cured under different conditions Tensile strength (MPa) a) Ambient Model Equivalent time, t eq (years) 6 5 E-modulus (GPa) b) Ambient Model Equivalent time, t eq (years) Figure 6: Mechanical property development due to post-curing for predicting long-term material behavior - a) Strength b) Stiffness Page 6 of 8
7 The increase in tensile strength was more significant than that in stiffness for two possible reasons: the strength is more dependent on changes in the polymeric structure in terms of increase in chain branching and molecular bond strength, which is also demonstrated by the increase of strain at failure after post-curing, as shown in Figure 7. In addition, the fillers comprised in the material contribute more to the stiffness than to the strength and therefore the change in stiffness due to changes in the polymeric structure is smaller than the change in strength. An increase in mechanical property values for specimens post-cured at was also observed albeit at a slower rate than those post-cured at during the same postcuring periods. Specimens cured at laboratory temperature for longer periods were found to follow the same trend thus confirming the applicability of the simulation of increase in cure level and corresponding mechanical properties by post-curing. Of all the experimental sets, the results of the specimens post-cured at for longer periods ( 24hours) showed the biggest scatter, which could be attributed to an insufficiently long cooling period (24 hours) or interference of physical aging following the increase in T g value (approaching ). An existing model for the long-term development of concrete properties was appropriately modified for the prediction of the long-term mechanical properties of adhesives, since both systems exhibit a similar curing behavior [8]. A good agreement between the modeling and experimental results was achieved, as shown in Figure 6. The results of this study are also applicable to other cold-curing structural epoxy adhesives [9]. 40 Reference -168hr 30 Stress, σ (MPa) Strain, ε (%) Figure 7: Change in stress-strain behavior due to post-curing for selected specimens 4. Conclusions The long-term changes in physical and mechanical properties were investigated by accelerating the curing reaction by post-curing at different temperatures above and below T g during different periods. The following conclusions were drawn: The experimental data available concerning the glass transition temperature, T g, for periods of up to 7 years are used to extrapolate the prediction up to 17 years by accelerating the curing reaction by post-curing at elevated temperatures (slightly above and below T g ). Based on this extrapolation procedure, tensile strength and stiffness results are also be extrapolated up to 17 years. Page 7 of 8
8 Structural adhesives exhibit significant increases in T g, strength and stiffness over the long term provided that joints are adequately sealed and protected from environmental degradation, particularly caused by humidity and UV radiation. Acknowledgements The authors thank the Federal Roads Authority (FEDRO) for funding this project, SIKA AG, Zurich, for its support, and the Laboratory of Composite and Polymer Technology (LTC EPFL) for use of DSC equipment. References [1] DUNN, D. J., Engineering and structural adhesives, Rapra review reports, Vol. 15, No. 1, 2004, pp [2] MAYS, G.C., HUTCHINSON, A.R., Adhesives in civil engineering, Cambridge university press, [3] SHAW, S.J, TOD, D.A, The effect of cure conditions on a rubber-modified epoxy adhesive, J. Adhes., Vol. 28, No. 4, 1989, pp [4] SINCLAIR, J.W., effect of cure temperature on epoxy resin properties, J. Adhes., Vol. 38, 1992, pp [5] LAPIQUE, F, REDFORD, K, Curing effects on viscosity and mechanical properties of commercial epoxy resin adhesive, Intl. J. Adhs. Adhes., Vol. 22, No. 4, 2002, pp [6] LEE, J.K, GILLAHM, J.K, Evolution of properties with increasing cure of thermosetting epoxy/aromatic amine system: Physical ageing, J. Appl. Polym. Sci., Vol. 90, No. 10, 2003, pp [7] STEWART, I, CHAMBERS, A, GORDON, T, The cohesive mechanical properties of a toughened epoxy adhesive as function of cure level, Intl. J. Adhs. Adhes., Vol. 27, No. 4, 2003, pp [8] MULLER, H, HAIST, M, Effects of time upon strength deformation, fib bulletin 51: structural concrete-text book on behaviour, design and performance, Vol. 1, pp [9] MOUSSA, O, Thermophysical and thermomechanical behavior of cold-curing structural adhesives in bridge construction, PhD Thesis No 5244, Ecole Polytechnique Fédérale de Lausanne, Page 8 of 8
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