ing. Based on the obtained results the BG annealing was selected in order to achieve a higher tensile strength at moderate elongation. The average relative deviation between the predicted and the experimental data for the tensile strength for linear regression and genetic programming is 3.55 % and 3.08 %, respectively. The average relative deviation bet- ween the predicted and the experimental data for elon- gation for linear regression and genetic programming is 3.56 % and 2.65 %, respectively. In the future the proposed concept will be used for analyzing the properties of selected steel grades. 6 REFERENCES 1 S. Bruschi, T. Altan, D. Banabic, P.F.Bariani, A. Brosius, J. Cao, A. Ghiotti, M. Khraisheh, M. Merklein, A. E. Tekkaya, Testing and modelling of material behaviour and formability in sheet metal forming, CIRP Annals – Manufacturing Technology, 63 (2014) 2, 727–749, doi:10.1016/j.cirp.2014.05.005 2 Q. Zhang, M. Mahfouf, A nature-inspired multi-objective optimi- sation strategy based on a new reduced space searching algorithm for the design of alloy steels, Engineering Applications of Artificial Intelligence, 23 (2010) 5, 660–675, doi:10.1016/j.engappai.2010. 01.017 3 M. Kova~i~, B. [arler, Application of the Genetic Programming for Increasing the Soft Annealing Productivity in Steel Industry, Materials and Manufacturing Processes, 24 (2009) 3, 369–374, doi:10.1080/10426910802679634 4 M. Kova~i~, Modeling of Total Decarburization of Spring Steel with Genetic Programming, Materials and Manufacturing Processes, 30 (2014) 4, 434–443, doi:10.1080/10426914.2014.961477 5 M. Kova~i~, D. Novak, Prediction of the chemical non-homogeneity of 30MnVS6 billets with genetic programming, Materiali in tehnologije, 50 (2016) 1, 69–74, doi:10.17222/mit.2014.280 6 M. Kova~i~, R. Jager, Modeling of occurrence of surface defects of C45 steel with genetic programming, Materiali in tehnologije, 49 (2015) 6, 857–863, doi:10.17222/mit.2013.304 7 Z. Wang, P. Liu, Y. Xu, Y. Wang, Y. Zhan, Hot Stamping of High Strength Steel with Tailored Properties by Two Methods, Procedia Engineering, 81 (2014), 1725–1730, doi:10.1016/j.proeng.2014. 10.221 8 A. K. Lakshminarayanan, Enhancing the properties of friction stir welded stainless steel joints via multi-criteria optimization, Archives of Civil and Mechanical Engineering, 16 (2016) 4, 605–617, doi:10.1016/j.acme.2016.03.012 9 X. Kong, L. Lan, Z. Hu, B. Li, T. Sui, Optimization of mechanical properties of high strength bainitic steel using thermo-mechanical control and accelerated cooling process, Journal of Materials Pro- cessing Technology, 217 (2015), 202–210, doi:10.1016/j.jmatprotec. 2014.11.016 10 R. S. Khabba, B. D. Manshadi, A. Abedian, R. Mahmudi, A sim- plified fuzzy logic approach for materials selection in mechanical engineering design, Materials and Design, 30 (2009) 3, 687–697, doi:10.1016/j.matdes.2008.05.026 11 D. Pandya, D. Shah, Experimentation and its Prediction of Process Parameters Effects on Elongation in Tensile Test of AISI 1008 Steel Using ANN Model, Procedia Technology, 14 (2014), 282–289, doi:10.1016/j.protcy.2014.08.037 12 I. Mohanty, D. Bhattacharjee, S. Datta, Designing cold rolled IF steel sheets with optimized tensile properties using ANN and GA, Computational Materials Science, 50 (2011) 8, 2331–2337, doi:10.1016/j.commatsci.2011.03.007 13 Y. Y. Yang, M. Mahfouf, D. A. Linkens, Q. Zhang, Tensile Strength Prediction for Hot Rolled Steels by Bayesian Neural Network Model, IFAC Proceedings Volumes, Vol. 42 (2009) 23, 255–260, doi:10.3182/20091014-3-CL-4011.00046 14 J. Chen, M. Mahfouf, G. Sidahmed, A new holistic systems approach to the design of heat treated alloy steels using a biologically inspired multi-objective optimisation algorithm, Engineering Applications of Artificial Intelligence, 37 (2015), 103–114, doi:10.1016/j.engappai. 2014.08.014 15 J. Han, H. Li, Z. Zhu, L. Jiang, H. Xu, L. Ma, Effects of processing optimisation on microstructure, texture, grain boundary and mechanical properties of Fe-17Cr ferritic stainless steel thick plates, Materials Science and Engineering: A, 616 (2014), 20–28, doi:10.1016/j.msea.2014.07.107 16 S. Chen, X. Jin, L. Rong, Improving the strength and ductility of reduced activation ferritic/martensitic steel by cold-swaging and post-annealing, Materials Science and Engineering: A, 631 (2015), 139–143, doi:10.1016/j.msea.2015.02.044 17 L. Chen, J, Huang, Y. Zhao, H. Di, F. Zhu, Processing, Microstruc- tures and Mechanical Properties of Ultra-high Strength Steel Sheet, Procedia Engineering, 81 (2014), 84–89, doi:10.1016/j.proeng. 2014.09.131 18 S. Klemen, M. Kova~i~, P. Kitak, J. Pihler, Electric-arc-furnace pro- ductivity optimization, Materiali in tehnologije, 48 (2014) 1, 3–7 19 M. Kova~i~, B. [arler, Genetic Algorithm-Based Batch Filling Sche- duling in the Steel Industry, Materials and manufacturing processes, 26 (2011) 3, 464–474, doi:10.1080/10426914.2010.525576 20 J. F. Wang, W. L. Kang, J. L. Zhao, K. Y. Chu, A simulation approach to the process planning problem using a modified particle swarm optimization, Advances in Production Engineering & Management, 11 (2016) 2, 77–92, doi:10.14743/apem2016.2.211 21 S. Ramadan, A bi-objective inspection policy optimization model for finite-life repairable systems using a genetic algorithm, Advances in Production Engineering & Management, 11 (2016) 1, 38–48, doi:10.14743/apem2016.1.208 22 M. Hrelja, S. Klan~nik, T. Irgoli~, M. Pauli~, Z. Jurkovi~, J. Bali~, M. Brezo~nik, Particle swarm optimization approach for modelling a turning process, Advances in Production Engineering & Mana- gement, 9 (2014) 1, 21–30, doi:10.14743/apem2014.1.173 23 M. Hrelja, S. Klan~nik, J. Bali~, M. Brezo~nik, Modelling of a Turn- ing Process Using the Gravitational Search Algorithm, International Journal of Simulation Modelling, 13 (2014) 1, 30–41, doi:10.2507/ IJSIMM13(1)3.248 M. KOVA^I^ et al.: INCREASING THE TENSILE STRENGTH AND ELONGATION OF 16MnCrS5 STEEL ... 888 Materiali in tehnologije / Materials and technology 51 (2017) 6, 883–888 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 889–895 DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN OBSTOJNOST FRP/LESNIH SKLOPOV, LEPLJENIH Z EPOKSI SMOLO Jan Vanìrek, Milan [mak, Ivo Kusák, Petr Misák Brno University of Technology, Faculty of Civil Engineering, Veveøí 95, 602 00 Brno, Czech Republic vanerek.j@fce.vutbr.cz Prejem rokopisa – received: 2016-11-18; sprejem za objavo – accepted for publication: 2017-04-20 doi:10.17222/mit.2016.321 The paper describes the properties of FRP/wood bonds, made of different wood species commonly used in the timber industry within Central Europe (oak, spruce, pine and larch). An FRP fabric (glass-fiber-reinforced polymer – GFRP, carbon-fiber-reinforced polymer – CFRP) was applied as the reinforcement. The durability of all the reinforced FRP/wood assemblies was verified with short-term exposure tests following the tensile-shear-strength and wood-failure criteria for the shear area of a single-lap joint. To precisely define the effect of the mechanical interlocking mechanism of the bond, analyses of porosity and surface roughness, and SEM were performed. Keywords: durability, epoxy, FRP, wood adherend ^lanek opisuje lastnosti FRP/lesnih sklopov, narejenih iz razli~nih vrst lesa, ki se obi~ajno uporablja v lesni industriji v Srednji Evropi (hrast, jelka, bor, macesen). FRP-materiali (polimeri, oja~ani s steklenimi vlakni – angl. GFRP, polimeri, oja~ani z ogljikovimi vlakni, angl. CFRP) so bili uporabljeni za oja~anje. Obstojnost vseh FRP/lesnih sklopov so preverjali s kratkotrajnimi stri`nimi preizkusi. Kriterij je bil povr{ina stri`nega preloma na enojni prekrivni ploskvi med FRP in lesom. Da bi lahko natan~no definirali mehansko trdnost spoja, so izvedli analize poroznosti, povr{inske hrapavosti in SEM-analize. Klju~ne besede: trajnost, epoksi, FRP, lepljivost lesa 1 INTRODUCTION The main purpose of the FRP usage with timber in the construction industry is generally to improve the stiffness/strength of reinforced items without any influence on their service life or any environmental impact. From the perspective of the timber-rein- forcement process, the optimum dimensional stability during moisture changes in wood should be one of the most important criteria for such joints. Different studies were made for the FRP/wood bond durability using different types of adhesives. The optimum results of adhesion were achieved using formaldehyde-based adhesives;1–3 different, contrary results were found using epoxy resins.4,5 The results1 for the epoxy resins showed an inability to reach the requirement for a cohesive failure of 80 % (in wood) after an exposure to cyclic hygrothermal conditions. Moreover, positive results were found using priming treatments (hydroxymetyl resorcinol – HMR; resorcin-fenol – RF; hexamethylolmelamin metyl ether – MME) before the gluing process.2 The durability of FRP/wood joints using epoxy has not been completely established. Therefore, the final aim of this experiment was to establish the durability aspect of such joints. The focus was on the observation of the wood adhering parameters having a significant impact on the mecha- nical interlocking process to understand the impact of mechanical interlocking on the joint durability. 2 EXPERIMENTAL PART 2.1 Materials Carbon, glass or aramid are common reinforcement- fiber materials used for external polymer-composite systems known as fiber-reinforced polymers (FRPs). Reinforcing of wood with FRP lamellas/fabrics could be applied without any restriction regarding the wood species. To evaluate the influence of wood species, the experiment used glass-fiber-reinforced polymer (GFRP) and carbon-fiber-reinforced polymer (CFRP) fabrics applied to different wood adherents. Oak (Quercus robur), spruce (Picea abies), pine (Pinus sylvestris) and larch (Larix decidua) with a uniform thickness of 25 mm were chosen. The fabrics with carbon fibers (Tyfo SCH-41, FYFE Co.) with a width of 1.0 mm and the GFRP with glass fibre (Tyfo-SEH-51A, FYFE Co.) with a width of 1.3 mm were used. As the adhesive, the epoxy resin TYFO S (diglycidyl ether of bisphenol-A, DGEBA) with an amine hardener was used. Pre-treat- ment including penetration of the wood surface to ensure stabilization of wood cells (200 g/m2) was applied. Similarly, the FRP fabrics were saturated with epoxy resin (400 g/m2) on both sides. After 30 min of such Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 889 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS UDK 67.017:674-419.3:678.686 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 51(6)889(2017) pre-treatments, the FRP strips were applied to the wood surface. After 24 h of the epoxy curing process, the final layer of the epoxy matrix in the amount of 200 g/m2 was also applied without any pressure. All the applications were carried out at a laboratory ambient temperature of 20 °C. To ensure the post-curing process, the assemblies were exposed to a constant temperature of 60 °C for 72 h. After the post-curing process, the test samples of 20 mm × 8 mm × 150 mm with 3-mm-thick notches in the wood were adhered to the fabrics and the CFRP or GFRP layers were made, defining the shear area. 2.2 Tensile-shear-strength testing The FRP/wood specimens were subjected to accele- rated tests, exposing them to all the climatic treatments and different hygrothermal conditions (classes A2–A5, specified in ^SN EN 302-1, Table 1). Tensile-shear tests were performed on the test specimens, for each condition class, and a total of 12 test samples were used. The tests were performed on a Testometric M350-20CT machine (Testometric Company Ltd., UK), digitally recording the test progress at a crosshead speed of 1 mm/min. As an additional evaluation of the bond durability, the wood failures within the shear area (rounded to the nearest value in multiples of 10 %) were visually assessed. Table 1: Types of exposure treatments prior to the tensile-shear testing Treatment Climatic treatment Specification A1 Standard climate 7 d 20 °C/65 % A2 Immersion in coldwater 7 d 20 °C/65 % 4 d in water (15±5 °C) Tested in a wet state A3 Immersion in coldwater 7 d 20 °C/65 % 4 d immersion in water (15±5 °C), conditioning at 20 °C/65 % Tested in a dry state A4 Immersion inboiling water 7 d 20 °C/65 % 6 h in boiling water 2 h immersion in water (15±5 °C), Tested in a wet state A5 Immersion inboiling water 7 d 20 °C/65 % 6 h in boiling water 2 h immersion in water (15±5 °C) 7 d conditioning at 20 °C/65 % Tested in a dry state 2.3 Microstructural analysis To assess the effect of mechanical interlocking as a possible aspect of a bond, the microstructures of all the tested wood adherents were analyzed. The sizes of the main structural elements of the transverse wood microtome samples were assessed. Electron scanning microscopy provided an accurate evaluation of a failed bond based on the loss of adhesion. 2.4 Wood-surface-roughness analysis The surfaces of all the tested wood adherents were scanned using confocal laser microscopy in both the optical and confocal mode. The automatic microscope mode was used to determine the highest and lowest point of the relief of a scanned area. The number of optical sections depended only on the wood, assuming that the other parameters such as magnification and the illumi- nation mode (laser or optical light) remained unchanged. Alternatively, the number of optical sections depended on the illuminated thickness of the wood. Optical cuts from 40 to 60 in the optical mode and from 70 to 90 in the confocal mode were evaluated. The purpose of this analysis was to see if the different surface roughness of each wood species has an impact on the final durability of a FRP/wood bond. The parameters of mean quadratic heights (SRq, SPq) and mean arithmetic heights (SRa, SPa) were assessed in five different appointed places for each tested wood. Surface roughness parameters SRa, SPa, SRq and SPq are based on one-dimensional parameters Ra (the arithmetic mean of roughness), Pa (the arithmetic mean of height of a curve profile), Rq (the root mean square roughness), Pq (the root mean square height of a curve profile). The calculation of these one-dimensional parameters is specified in ^SN EN ISO 4287 and the conversion into surface parameters was calculated based on the data acquired from two perpendicular directions. 2.5 Porosity The pore size and pore distribution within all the tested wood specimens were evaluated with mercury porosimetry using the PASCAL 140/240, Thermo Finnigan equipment. Wood samples with a volume of approx. 0.75 cm3 were used. To avoid an overestimation of the portion of smaller pores, a gradual increase in the rate of pressure during the process was chosen. 3 RESULTS 3.1 Tensile-shear-strength testing The mean strength values obtained are shown in Figures 1a to 1d; it is clear that the sets of dry-wet cycling ageing tests show a reduction in the joint strength. The most significant strength reduction in the dry state for both FRP materials resulted from the specimens subjected to both exposure treatments, providing a significant hygrothermal-stress concentration in the bond line. To compare the test results, variance tests (ANOVA) were analyzed. The influence of the type of exposure was tested using the one-way ANOVA. Based on this analysis, the tensile strength is significantly influenced by the type of exposure. In addition, the two-way ANOVA was used when both the type of exposure and the type of reinforcement were factors. The purpose of J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 890 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 891 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 2: Cross-section of oak wood, apparent vessel elements and libriform cells, magn. 100× Figure 3: Cross-section of an early part of the annual ring of spruce wood, magn. 200× Figure 1: Mean tensile-shear strengths of the samples tested after the exposure to climatic treatment according to EN 302-1;  denotes the mean value; the box plot – rectangle shows the interquartile range (IQR) with the median depicted within the box; for each exposure, the value of wood failure is stated Table 2: Mean values of the wood-element size proportion of the used wood species Size (diameter) of wood elements (μm) Lumina Cell-wall thickness tracheids vessels libriform tracheids libriform early wood late wood early wood late wood early wood late wood Pine (Pinus sylvestris) 26.1 9.7 6.0 11.7 Larch (Larix decidua) 30.7 10.1 4.7 9.2 Spruce (Picea abies) 31.2 10.3 4.0 8.9 Oak (Quercus robur) 245.0 41.9 9.0 4.0 pre-treatments, the FRP strips were applied to the wood surface. After 24 h of the epoxy curing process, the final layer of the epoxy matrix in the amount of 200 g/m2 was also applied without any pressure. All the applications were carried out at a laboratory ambient temperature of 20 °C. To ensure the post-curing process, the assemblies were exposed to a constant temperature of 60 °C for 72 h. After the post-curing process, the test samples of 20 mm × 8 mm × 150 mm with 3-mm-thick notches in the wood were adhered to the fabrics and the CFRP or GFRP layers were made, defining the shear area. 2.2 Tensile-shear-strength testing The FRP/wood specimens were subjected to accele- rated tests, exposing them to all the climatic treatments and different hygrothermal conditions (classes A2–A5, specified in ^SN EN 302-1, Table 1). Tensile-shear tests were performed on the test specimens, for each condition class, and a total of 12 test samples were used. The tests were performed on a Testometric M350-20CT machine (Testometric Company Ltd., UK), digitally recording the test progress at a crosshead speed of 1 mm/min. As an additional evaluation of the bond durability, the wood failures within the shear area (rounded to the nearest value in multiples of 10 %) were visually assessed. Table 1: Types of exposure treatments prior to the tensile-shear testing Treatment Climatic treatment Specification A1 Standard climate 7 d 20 °C/65 % A2 Immersion in coldwater 7 d 20 °C/65 % 4 d in water (15±5 °C) Tested in a wet state A3 Immersion in coldwater 7 d 20 °C/65 % 4 d immersion in water (15±5 °C), conditioning at 20 °C/65 % Tested in a dry state A4 Immersion inboiling water 7 d 20 °C/65 % 6 h in boiling water 2 h immersion in water (15±5 °C), Tested in a wet state A5 Immersion inboiling water 7 d 20 °C/65 % 6 h in boiling water 2 h immersion in water (15±5 °C) 7 d conditioning at 20 °C/65 % Tested in a dry state 2.3 Microstructural analysis To assess the effect of mechanical interlocking as a possible aspect of a bond, the microstructures of all the tested wood adherents were analyzed. The sizes of the main structural elements of the transverse wood microtome samples were assessed. Electron scanning microscopy provided an accurate evaluation of a failed bond based on the loss of adhesion. 2.4 Wood-surface-roughness analysis The surfaces of all the tested wood adherents were scanned using confocal laser microscopy in both the optical and confocal mode. The automatic microscope mode was used to determine the highest and lowest point of the relief of a scanned area. The number of optical sections depended only on the wood, assuming that the other parameters such as magnification and the illumi- nation mode (laser or optical light) remained unchanged. Alternatively, the number of optical sections depended on the illuminated thickness of the wood. Optical cuts from 40 to 60 in the optical mode and from 70 to 90 in the confocal mode were evaluated. The purpose of this analysis was to see if the different surface roughness of each wood species has an impact on the final durability of a FRP/wood bond. The parameters of mean quadratic heights (SRq, SPq) and mean arithmetic heights (SRa, SPa) were assessed in five different appointed places for each tested wood. Surface roughness parameters SRa, SPa, SRq and SPq are based on one-dimensional parameters Ra (the arithmetic mean of roughness), Pa (the arithmetic mean of height of a curve profile), Rq (the root mean square roughness), Pq (the root mean square height of a curve profile). The calculation of these one-dimensional parameters is specified in ^SN EN ISO 4287 and the conversion into surface parameters was calculated based on the data acquired from two perpendicular directions. 2.5 Porosity The pore size and pore distribution within all the tested wood specimens were evaluated with mercury porosimetry using the PASCAL 140/240, Thermo Finnigan equipment. Wood samples with a volume of approx. 0.75 cm3 were used. To avoid an overestimation of the portion of smaller pores, a gradual increase in the rate of pressure during the process was chosen. 3 RESULTS 3.1 Tensile-shear-strength testing The mean strength values obtained are shown in Figures 1a to 1d; it is clear that the sets of dry-wet cycling ageing tests show a reduction in the joint strength. The most significant strength reduction in the dry state for both FRP materials resulted from the specimens subjected to both exposure treatments, providing a significant hygrothermal-stress concentration in the bond line. To compare the test results, variance tests (ANOVA) were analyzed. The influence of the type of exposure was tested using the one-way ANOVA. Based on this analysis, the tensile strength is significantly influenced by the type of exposure. In addition, the two-way ANOVA was used when both the type of exposure and the type of reinforcement were factors. The purpose of J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 890 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 891 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 2: Cross-section of oak wood, apparent vessel elements and libriform cells, magn. 100× Figure 3: Cross-section of an early part of the annual ring of spruce wood, magn. 200× Figure 1: Mean tensile-shear strengths of the samples tested after the exposure to climatic treatment according to EN 302-1;  denotes the mean value; the box plot – rectangle shows the interquartile range (IQR) with the median depicted within the box; for each exposure, the value of wood failure is stated Table 2: Mean values of the wood-element size proportion of the used wood species Size (diameter) of wood elements (μm) Lumina Cell-wall thickness tracheids vessels libriform tracheids libriform early wood late wood early wood late wood early wood late wood Pine (Pinus sylvestris) 26.1 9.7 6.0 11.7 Larch (Larix decidua) 30.7 10.1 4.7 9.2 Spruce (Picea abies) 31.2 10.3 4.0 8.9 Oak (Quercus robur) 245.0 41.9 9.0 4.0 this was to establish the individual influences of these factors and the interaction between them. The results of the two-way ANOVA show that each factor is statisti- cally significant for the tensile strength, but the interac- tion between the factors is not significant. All the statistical tests were carried out at a significance level of 0.05. 3.2 Microstructural analysis Results of the size-distribution evaluation did not show any significant difference between the coniferous species; the biggest size of the cell-wall thickness was found for the pine species, concurring with the smallest size of the pores (lumina) of tracheid elements. Details of all the observed elements are shown in Table 2. The photomicrographs of the hardwood and conifer species with the size measurements are shown in Figures 2 and 3. 3.3 Wood-surface-roughness analysis A comparison of the results of the profile parameters (SPa, SPq) indicates deviations from the interspaced centerline of the test surface; the highest deviations were detected on the oak surface, arising from the existence of open vessel elements (Figure 5). The smallest deviation was found on the pine; the drop of the profile-parameter value for the pine was lower by almost 50 % compared to the other coniferous woods. The achieved values of the roughness parameters (SRa, SRq), where the longwave part is eliminated, showed the highest values of the roughness for the oak sample; the highest decrease of nearly 40 % was ob- served for the pine sample, compared to the other softwood species. All the achieved values are shown in Table 3. 3.4 Porosity Among all the other parameters, porosity has the most significant influence on the impregnability of J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 892 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 5: Surface relief of the pine sample used for calculating square roughness parameters (magn. 120×; area of 2560 μm × 1920 μm) Figure 4: Surface relief of the pine sample used for calculating square roughness parameters (magn. 120×; area of 2560 μm × 1920 μm) Table 3: Values of selected roughness parameters of used wood species obtained with confocal microscopy Wood species Mean values and S. D. of roughness parameters SPa SRa SRq SPq Pine 9.14 1.20 5.82 0.18 8.00 0.41 12.31 1.29 Oak 42.89 9.20 9.66 1.04 14.77 1.73 53.68 10.35 Larch 19.95 2.20 8.05 0.95 11.22 1.52 24.84 3.18 Spruce 17.41 3.03 7.47 0.63 11.20 1.26 22.95 3.51 Figure 6: Cumulative pore volume as a function of the pore diameter of softwood and hardwood species Table 4: Achieved results of mercury porosimetry of tested wood samples Wood species Total porosity Specific density Bulk density Cumulative pore volume % kg m–3 kg m–3 mm3 g–1 Oak 47.6 1410.0 738.6 644.7 Larch 54.0 1518.4 699.2 771.6 Pine 60.3 1381.1 549.0 1097.3 Spruce 62.8 1423.6 528.9 1188.1 wood. Consequently, the bulk density and specific density for each tested sample were established from the other parameters. The resulting values are shown in Table 4, confirming the presumption of a decreasing total porosity despite the increasing bulk density. The cumulative pore-volume curves as a function of the pore diameter of oak (hardwood) and pine (softwood) are shown in Figure 6. 4 DISCUSSION 4.1 Tensile-shear-strength testing A stronger effect of the thermal exposure ensuring the hygrothermal exposure for condition classes A4 and A5 compared to the exposure without a thermal effect (A2, A3) was not proven (Table 5). Regarding the type of fabrics, there was no indication of any dependency on the durability aspect. The requirements of the EN standard for strength limits (related to the beech/beech bond) for all the exposures were not exceeded by any of the tested samples. The most significant result of durability was achieved with the pine as an adherent when no losses in the strength occurred under all the severe exposures. Furthermore, the values of the cohesive failure expressed with a higher wood failure (WF) for the pine/FRP bonds supported this durability aspect. The values of the wood failure showed that the minimum limit of 80 % was not reached for the dry test samples of larch as a softwood; also, the WF percentage dropped below the 80 % criterion for the FRP/larch samples tested in a wet condition. Comparing the effects of the strength and wood-failure parameters, it can be clearly indicated that the more decisive criterion for the durability aspect shows exceptional values for the type of failure as shown for the larch/FRP bonds. 4.2 Porosity The microscopy analysis of the main structural ele- ments showed similar sizes of tracheids for all the soft- wood species; the highest porosity was established for spruce, the lowest for larch. But differences occurred between the results for the pore distribution as a function of the pore diameter. The differences occurred between the distributions of pores for the softwood species where the biggest drop in the distribution occurred for the pore diameters of 10 μm, contrary to the shape of the distri- bution curves for the oak as the ring-porous wood, which showed a consistent increase in the pore volume for pore diameters from 12 nm to 100 μm. The distribution of pore diameters for softwood is affected by the amount of tracheids elements, which form the main structure of softwoods. The lowest value of the porosity was estab- lished for the oak-wood sample; however, this had no effect on the final durability of the FRP/wood bond. Similar strength decreases were found when comparing the FRP/oak samples with the samples of the other wood species. The values of the pore distribution correlate with similar results,6 performed for the European wood species. 4.3 Bond-line failure After the accelerated tests, the FRP/wood bond lines were assessed at the macroscopic and microscopic levels. At the macroscopic level, the adhesive failure occurred mostly in the late part of the annual ring, despite the cohesive failure in the early part of the annual ring for the soft-wood species. For oak as a hardwood, the most cohesive failures were detected at the shear areas of the specimens tested in a dry state. To precisely specify the mechanism of failure, elec- tron microscopy (SEM) was performed to observe the microscopic structure of the wood at the FRP/wood interphase region. For the softwood species, the adhesion failure did not show the existence of structural tracheid elements in the early parts of the annual rings. Never- theless, the existence of ray elements filled with resin was observed (Figure 7); a deeper penetration of the adhesive was observed due to their perpendicular orien- tation to the application area, which was wetted by the adhesive. This clearly indicates that the existence and quantity of rays partake in the tensile-shear strength of the softwood species. For the hardwood species, a good adhesive penetra- tion into the lumina of all the conductive elements (vessel, libriform) was observed. This phenomenon was proven by a higher wood-failure percentage for the specimens tested in a dry state after a hygrothermal J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 893 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Table 5: Resulting values of decreasing strength after exposing the test samples to different exposure criteria Decreasing-strength and wood-failure values (%) Exposure A1 A2 (wet) A3 (dry) A4 (wet) A5 (dry) Standard requirements for beech 10 MPa -40 -20 -40 -20 Oak/CFRP (WF) 9.3 (98) -34.3 (45) -6.0 (73) -21.1 (93) -6.4 (93) Oak/GFRP (WF) 8.6 (100) -20.8 (59.2) -0.5 (98.3) -18.0 (70.8) -4.6 (100.0) Pine/CFRP (WF) 8.3 (100) -29.7 (98) 7.5 (100) -29.7 (70) 13.0 (100) Pine/GFRP(WF) 7.9 (100) -29.3 (95.0) 1.9 (98.3) -29.5 (70.8) 6.1 (91.7) Larch/CFRP (WF) 8.3 (97.0) -22.0 (22.5) 28.0 (60.0) -22.3 (38.0) 2.9 (86.0) Larch/GFRP (WF) 7.9 (92.5) -24.7 (0) -1.4 (46.7) -28.6 (56.3) 12.1 (78.3) Spruce/CFRP (WF) 8.1 (100) -36.8 (100) -6.5 (84) -22.3 (74.0) -1.1 (85.0) Spruce/GFRP (WF) 7.7 (80.0) -37.0 (88.3) -15.2 (100.0) -28.6 (43.3) -8.2 (81.7) this was to establish the individual influences of these factors and the interaction between them. The results of the two-way ANOVA show that each factor is statisti- cally significant for the tensile strength, but the interac- tion between the factors is not significant. All the statistical tests were carried out at a significance level of 0.05. 3.2 Microstructural analysis Results of the size-distribution evaluation did not show any significant difference between the coniferous species; the biggest size of the cell-wall thickness was found for the pine species, concurring with the smallest size of the pores (lumina) of tracheid elements. Details of all the observed elements are shown in Table 2. The photomicrographs of the hardwood and conifer species with the size measurements are shown in Figures 2 and 3. 3.3 Wood-surface-roughness analysis A comparison of the results of the profile parameters (SPa, SPq) indicates deviations from the interspaced centerline of the test surface; the highest deviations were detected on the oak surface, arising from the existence of open vessel elements (Figure 5). The smallest deviation was found on the pine; the drop of the profile-parameter value for the pine was lower by almost 50 % compared to the other coniferous woods. The achieved values of the roughness parameters (SRa, SRq), where the longwave part is eliminated, showed the highest values of the roughness for the oak sample; the highest decrease of nearly 40 % was ob- served for the pine sample, compared to the other softwood species. All the achieved values are shown in Table 3. 3.4 Porosity Among all the other parameters, porosity has the most significant influence on the impregnability of J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 892 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 5: Surface relief of the pine sample used for calculating square roughness parameters (magn. 120×; area of 2560 μm × 1920 μm) Figure 4: Surface relief of the pine sample used for calculating square roughness parameters (magn. 120×; area of 2560 μm × 1920 μm) Table 3: Values of selected roughness parameters of used wood species obtained with confocal microscopy Wood species Mean values and S. D. of roughness parameters SPa SRa SRq SPq Pine 9.14 1.20 5.82 0.18 8.00 0.41 12.31 1.29 Oak 42.89 9.20 9.66 1.04 14.77 1.73 53.68 10.35 Larch 19.95 2.20 8.05 0.95 11.22 1.52 24.84 3.18 Spruce 17.41 3.03 7.47 0.63 11.20 1.26 22.95 3.51 Figure 6: Cumulative pore volume as a function of the pore diameter of softwood and hardwood species Table 4: Achieved results of mercury porosimetry of tested wood samples Wood species Total porosity Specific density Bulk density Cumulative pore volume % kg m–3 kg m–3 mm3 g–1 Oak 47.6 1410.0 738.6 644.7 Larch 54.0 1518.4 699.2 771.6 Pine 60.3 1381.1 549.0 1097.3 Spruce 62.8 1423.6 528.9 1188.1 wood. Consequently, the bulk density and specific density for each tested sample were established from the other parameters. The resulting values are shown in Table 4, confirming the presumption of a decreasing total porosity despite the increasing bulk density. The cumulative pore-volume curves as a function of the pore diameter of oak (hardwood) and pine (softwood) are shown in Figure 6. 4 DISCUSSION 4.1 Tensile-shear-strength testing A stronger effect of the thermal exposure ensuring the hygrothermal exposure for condition classes A4 and A5 compared to the exposure without a thermal effect (A2, A3) was not proven (Table 5). Regarding the type of fabrics, there was no indication of any dependency on the durability aspect. The requirements of the EN standard for strength limits (related to the beech/beech bond) for all the exposures were not exceeded by any of the tested samples. The most significant result of durability was achieved with the pine as an adherent when no losses in the strength occurred under all the severe exposures. Furthermore, the values of the cohesive failure expressed with a higher wood failure (WF) for the pine/FRP bonds supported this durability aspect. The values of the wood failure showed that the minimum limit of 80 % was not reached for the dry test samples of larch as a softwood; also, the WF percentage dropped below the 80 % criterion for the FRP/larch samples tested in a wet condition. Comparing the effects of the strength and wood-failure parameters, it can be clearly indicated that the more decisive criterion for the durability aspect shows exceptional values for the type of failure as shown for the larch/FRP bonds. 4.2 Porosity The microscopy analysis of the main structural ele- ments showed similar sizes of tracheids for all the soft- wood species; the highest porosity was established for spruce, the lowest for larch. But differences occurred between the results for the pore distribution as a function of the pore diameter. The differences occurred between the distributions of pores for the softwood species where the biggest drop in the distribution occurred for the pore diameters of 10 μm, contrary to the shape of the distri- bution curves for the oak as the ring-porous wood, which showed a consistent increase in the pore volume for pore diameters from 12 nm to 100 μm. The distribution of pore diameters for softwood is affected by the amount of tracheids elements, which form the main structure of softwoods. The lowest value of the porosity was estab- lished for the oak-wood sample; however, this had no effect on the final durability of the FRP/wood bond. Similar strength decreases were found when comparing the FRP/oak samples with the samples of the other wood species. The values of the pore distribution correlate with similar results,6 performed for the European wood species. 4.3 Bond-line failure After the accelerated tests, the FRP/wood bond lines were assessed at the macroscopic and microscopic levels. At the macroscopic level, the adhesive failure occurred mostly in the late part of the annual ring, despite the cohesive failure in the early part of the annual ring for the soft-wood species. For oak as a hardwood, the most cohesive failures were detected at the shear areas of the specimens tested in a dry state. To precisely specify the mechanism of failure, elec- tron microscopy (SEM) was performed to observe the microscopic structure of the wood at the FRP/wood interphase region. For the softwood species, the adhesion failure did not show the existence of structural tracheid elements in the early parts of the annual rings. Never- theless, the existence of ray elements filled with resin was observed (Figure 7); a deeper penetration of the adhesive was observed due to their perpendicular orien- tation to the application area, which was wetted by the adhesive. This clearly indicates that the existence and quantity of rays partake in the tensile-shear strength of the softwood species. For the hardwood species, a good adhesive penetra- tion into the lumina of all the conductive elements (vessel, libriform) was observed. This phenomenon was proven by a higher wood-failure percentage for the specimens tested in a dry state after a hygrothermal J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 893 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Table 5: Resulting values of decreasing strength after exposing the test samples to different exposure criteria Decreasing-strength and wood-failure values (%) Exposure A1 A2 (wet) A3 (dry) A4 (wet) A5 (dry) Standard requirements for beech 10 MPa -40 -20 -40 -20 Oak/CFRP (WF) 9.3 (98) -34.3 (45) -6.0 (73) -21.1 (93) -6.4 (93) Oak/GFRP (WF) 8.6 (100) -20.8 (59.2) -0.5 (98.3) -18.0 (70.8) -4.6 (100.0) Pine/CFRP (WF) 8.3 (100) -29.7 (98) 7.5 (100) -29.7 (70) 13.0 (100) Pine/GFRP(WF) 7.9 (100) -29.3 (95.0) 1.9 (98.3) -29.5 (70.8) 6.1 (91.7) Larch/CFRP (WF) 8.3 (97.0) -22.0 (22.5) 28.0 (60.0) -22.3 (38.0) 2.9 (86.0) Larch/GFRP (WF) 7.9 (92.5) -24.7 (0) -1.4 (46.7) -28.6 (56.3) 12.1 (78.3) Spruce/CFRP (WF) 8.1 (100) -36.8 (100) -6.5 (84) -22.3 (74.0) -1.1 (85.0) Spruce/GFRP (WF) 7.7 (80.0) -37.0 (88.3) -15.2 (100.0) -28.6 (43.3) -8.2 (81.7) exposure. Despite this, the proper penetration of the adhesive into the lumina did not show a positive effect on the durability for the A2 and A4 condition classes. 5 CONCLUSIONS The durability of FRP/wood bonds with different wood adherents was established using accelerated durability tests. According to the EN standard (declared for the beech/beech bond), all the tested samples of GFRP and CFRP fabrics met the standard criterion regardless of the wood species as the adherent. The wood species did not affect the durability of the FRP/wood bonds. The achieved strength for all the tested specimens in the conditions with a thermal exposure (A4, A5) was not significantly different from the one achieved in the conditions without a thermal exposure (A2, A3). Therefore, the inability of epoxy to withstand the volume changes of a wood adherent plays a more dominant role than the temperature influence on a possible resin degra- dation. The wood failure percentage proved to be a better J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 894 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 10: SEM micrograph of adhesive failure for FRP/oak, existence of cohesive failure of vessels, predominant adhesive failure of the FRP/oak bond line, magn. 200× Figure 8: SEM micrograph, typical existence of rays (R) and tracheids (Tr) filled with resin, FRP/pine, magn. 500× Figure 9: SEM micrograph of adhesive failure for FRP/oak, existence of the adhesive in the lumina of vessels (V) and libriform (L), magn. 200× Figure 7: SEM micrograph of the border between early and late larch wood, different types of failure, magn. 300× means to assess the durability of bonded specimens compared to strength-loss aspects. The principle of a good adhesion of the FRP/wood bonds via a mechanical interlocking process was con- sidered for the experimental work. The size of the pores is dominant for the permeability of the adhesive into the cell lumina. Therefore, the surface roughness, porosity and size distribution of pores for all the tested wood samples were analyzed. The dependency between the porosity and the FRP/wood bond durability was not proven. The spruce wood having the highest porosity did not exhibit the lowest drop in the strength, or even the biggest value of the cohesive failure. Furthermore, the FRP/wood durability of all the tested softwoods showed no dependency on the pore-size distribution. According to the laser confocal microscopy analysis, it was found that good durability of the FRP/pine wood bonds exhibits a good relationship with the parameters of the surface roughness. A plain surface and elimination of any debris on the surface allow proper adhesive wetting. All the results showed that the mechanical inter- locking of the FRP/wood bond does not have the domi- nant role anticipated; on the contrary, the chemical bonds of the adhesive contribute to the higher durability of the epoxy/wood bonds. This is because an interpenetrating polymer (adhesive) network occurs in the cell walls and in the mesopores between the cellulose fibers in the cell walls. A proper application technique, ensuring a proper diffusion of the epoxy adhesive between the cellulose microfibrils in the cell walls seems to be necessary for more durable FRP/wood bonds. Acknowledgment This paper was prepared with the financial help of project TA04010425 “A complex system of special repair materials using secondary raw materials for industries” supported by The Technology Agency of The Czech Republic; and the internal project of specific research No. FAST-S-16-3772 “Research of an adhesive modification increasing the durability of FRP/wood bonds at moisture exposure“ supported by Brno University of Technology, Faculty of Civil Engineering. 6 REFERENCES 1 B. S. Trimble, Durability and mode-I fracture of fiber-reinforced plastic (FRP)/wood interface bond, Doctoral dissertation, West Virginia University, 1999, 192 2 H. V. S. Ganga Rao, Sawn and laminated wood beams wrapped with fiber reinforced plastic composites, Wood Design Focus, 8 (1997) 3, 13–18 3 D. J. Gardner, J. F. Davalos, U. M. Munipalle, Adhesive Bonding of Pultruded Fiber-Reinforced Plastic to Wood, Forest Products Journal, 44 (1994) 5, 62–66 4 G. M. Raftery, A. M. Harte, P. D. Rodd, Bond quality at the FRP- wood interface using wood-laminating adhesives, International Journal of Adhesion & Adhesives, 29 (2009) 2, 101–110, doi:10.1016/j.ijadhadh.2008.01.006 5 J. P. Alexander, S. M. Shaler, D. J. Gardner, Evaluating wood/FRP bond durability through chemical kinetics, Proc. of Wood Adhesive, Madison WI, 2000, 289–299 6 M. Plötze, P. Niemz, Porosity and pore size distribution of different wood types as determined by mercury intrusion porosimetry, European Journal of Wood and Wood Products, 69 (2011) 4, 649–657, doi:10.1007/s00107-010-0504-0 J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS exposure. Despite this, the proper penetration of the adhesive into the lumina did not show a positive effect on the durability for the A2 and A4 condition classes. 5 CONCLUSIONS The durability of FRP/wood bonds with different wood adherents was established using accelerated durability tests. According to the EN standard (declared for the beech/beech bond), all the tested samples of GFRP and CFRP fabrics met the standard criterion regardless of the wood species as the adherent. The wood species did not affect the durability of the FRP/wood bonds. The achieved strength for all the tested specimens in the conditions with a thermal exposure (A4, A5) was not significantly different from the one achieved in the conditions without a thermal exposure (A2, A3). Therefore, the inability of epoxy to withstand the volume changes of a wood adherent plays a more dominant role than the temperature influence on a possible resin degra- dation. The wood failure percentage proved to be a better J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN 894 Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS Figure 10: SEM micrograph of adhesive failure for FRP/oak, existence of cohesive failure of vessels, predominant adhesive failure of the FRP/oak bond line, magn. 200× Figure 8: SEM micrograph, typical existence of rays (R) and tracheids (Tr) filled with resin, FRP/pine, magn. 500× Figure 9: SEM micrograph of adhesive failure for FRP/oak, existence of the adhesive in the lumina of vessels (V) and libriform (L), magn. 200× Figure 7: SEM micrograph of the border between early and late larch wood, different types of failure, magn. 300× means to assess the durability of bonded specimens compared to strength-loss aspects. The principle of a good adhesion of the FRP/wood bonds via a mechanical interlocking process was con- sidered for the experimental work. The size of the pores is dominant for the permeability of the adhesive into the cell lumina. Therefore, the surface roughness, porosity and size distribution of pores for all the tested wood samples were analyzed. The dependency between the porosity and the FRP/wood bond durability was not proven. The spruce wood having the highest porosity did not exhibit the lowest drop in the strength, or even the biggest value of the cohesive failure. Furthermore, the FRP/wood durability of all the tested softwoods showed no dependency on the pore-size distribution. According to the laser confocal microscopy analysis, it was found that good durability of the FRP/pine wood bonds exhibits a good relationship with the parameters of the surface roughness. A plain surface and elimination of any debris on the surface allow proper adhesive wetting. All the results showed that the mechanical inter- locking of the FRP/wood bond does not have the domi- nant role anticipated; on the contrary, the chemical bonds of the adhesive contribute to the higher durability of the epoxy/wood bonds. This is because an interpenetrating polymer (adhesive) network occurs in the cell walls and in the mesopores between the cellulose fibers in the cell walls. A proper application technique, ensuring a proper diffusion of the epoxy adhesive between the cellulose microfibrils in the cell walls seems to be necessary for more durable FRP/wood bonds. Acknowledgment This paper was prepared with the financial help of project TA04010425 “A complex system of special repair materials using secondary raw materials for industries” supported by The Technology Agency of The Czech Republic; and the internal project of specific research No. FAST-S-16-3772 “Research of an adhesive modification increasing the durability of FRP/wood bonds at moisture exposure“ supported by Brno University of Technology, Faculty of Civil Engineering. 6 REFERENCES 1 B. S. Trimble, Durability and mode-I fracture of fiber-reinforced plastic (FRP)/wood interface bond, Doctoral dissertation, West Virginia University, 1999, 192 2 H. V. S. Ganga Rao, Sawn and laminated wood beams wrapped with fiber reinforced plastic composites, Wood Design Focus, 8 (1997) 3, 13–18 3 D. J. Gardner, J. F. Davalos, U. M. Munipalle, Adhesive Bonding of Pultruded Fiber-Reinforced Plastic to Wood, Forest Products Journal, 44 (1994) 5, 62–66 4 G. M. Raftery, A. M. Harte, P. D. Rodd, Bond quality at the FRP- wood interface using wood-laminating adhesives, International Journal of Adhesion & Adhesives, 29 (2009) 2, 101–110, doi:10.1016/j.ijadhadh.2008.01.006 5 J. P. Alexander, S. M. Shaler, D. J. Gardner, Evaluating wood/FRP bond durability through chemical kinetics, Proc. of Wood Adhesive, Madison WI, 2000, 289–299 6 M. Plötze, P. Niemz, Porosity and pore size distribution of different wood types as determined by mercury intrusion porosimetry, European Journal of Wood and Wood Products, 69 (2011) 4, 649–657, doi:10.1007/s00107-010-0504-0 J. VANÌREK et al.: DURABILITY OF FRP/WOOD BONDS GLUED WITH EPOXY RESIN Materiali in tehnologije / Materials and technology 51 (2017) 6, 889–895 895 MATERIALI IN TEHNOLOGIJE/MATERIALS AND TECHNOLOGY (1967–2017) – 50 LET/50 YEARS