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CICE 2010 - The 5th International Conference on FRP Composites in Civil Engineering September 27-29, 2010, Beijing, China

Hygrothermal Ageing of Basalt Fiber Reinforced Epoxy Composites

Bo Xiao, Hui Li & Guijun Xian (gjxian@hit.edu.cn) School of Civil Engineering, Harbin Institute of Technology, Harbin, China

ABSTRACT Due to its low price and high chemical resistance, basalt fiber is emerging as a novel reinforcement for fiber reinforced polymer (FRP) composites used in civil engineering in recent years. Compared to widely applied glass fiber based FRP (GFRP) and carbon fiber based FRP (CFRP), however, much less research works on the durability performances of basalt fiber reinforced polymer (BFRP), have been done by now, which seriously hinders its wide and safe application. In the present study, unidirectional basalt fiber fabric reinforced epoxy composites were prepared with a wet lay-up process. Such BFRP materials are expected to be used for external rehabilitation, strengthening or renewal of structures. Durability studies were performed on cured BFRP strips through water, alkali solution immersion at various temperatures. The evolution of the water uptake and mechanical properties with the ageing time was investigated. The aim of the study is to demonstrate the feasibility of using BFRP in severe civil environments, and to disclose the possible degradation mechanisms. As shown, tensile strength of the BFRP samples shows remarkable degradation due to water and alkaline solution immersion, while the tensile modulus is affected slightly. In addition, the mechanical property degradation of the BFRP samples in water is much less than that in alkaline solutions. The results indicate the current basalt fiber need to be modified in its chemical compositions, surface treat-ment for enhanced durability performance. KEY WORDS


In recent more than twenty years, FRP composites have been widely applied in civil engineering as internal strengthening or external reinforcement for civil structures. The most successful application is externally wrapped or bonded FRP systems to strength, rehabilitate or renew various concrete, even steel structures. The commonly used fiber reinforcements for FRP composites are carbon fiber, glass fiber and Aramide fiber. The basic physical and chemical performances of the above FRP composites have been well demonstrated in various design codes, and published papers. Basalt fiber (BF) is produced from basalt rock through melting process, generally without any other additives in a single process (Sim et al. 2005). The performance of the basalt fiber, which is critically dependent on the basalt rock mine, may be less consistent than the synthetic fibers, such as glass fiber, carbon fiber etc. Up to date, some durability studies in various environmental conditions have been conducted to facilitate the application of BF and BF reinforced FRP (BFRP). Sim et al. studied chemical resistance, elevated temperature performance and tensile properties of BF (produced in Russia) and BF reinforced BFRP (Sim et al. 2005). As reported, BF shows similar alkaline resistance to glass fibers, and far inferior to carbon fibers, while

BF possesses the best fire resistance, even than the carbon fiber. As concluded, BF can be a promising alternative reinforcement among the commonly used fibers. It was found that basalt fiber reinforced epoxy FRP shows a good water and salt solution resistance up to 240 days at room temperatures (Liu et al. 2006). At elevated temperature (i.e., 40 ), however, the ageing in the above conditions resulted in remarkable decrease of the shear strength, may due to the degradation of the interracial strength. As found in a study on the chemical resistance of BF in acid and alkaline solution, after 3 hours boiling treatment, the remaining strength ratio is about 65.5% in 2 mol/L HCl solution and 81.6% in 2 mol/L NaOH solutions (Wang et al. 2008). In 90 days alkaline immersion, epoxy based BFRP shows a remarkable reduction in the flexural strength and a relative stable modulus at room temperature. The maximum strength reduction is about 40% of the original value. In addition, the studied BFRP shows a relatively better alkaline solution resistance compared to the acid solution. In the present paper, BF reinforced epoxy BFRP plates were prepared with a hand wet layup process. After fully curing, BFRP plates were immersed into distilled water, alkaline solution at 23, 40, 60 and 80 . The tensile properties were tracked as a function of ageing time. Based on the degradation rate of the

L. Ye et al. (eds.), Advances in FRP Composites in Civil Engineering Tsinghua University Press, Beijing and Springer-Verlag Berlin Heidelberg 2011

September 2729, 2010, Beijing, China


mechanical properties, the service life of the BFRP under the above conditions was evaluated using Arrhenius model. The study is to assess the application of BFRP in civil engineering under severe environmental conditions.

2.1 Materials An epoxy resin system, including epoxy resin and hardeners, is developed at our lab used for saturation of fiber clothes to strengthen, repair and rehabilitate concrete or other civil engineering structures. This epoxy resin system has a low viscosity and thus can easily saturate fiber fabrics. The resin can be cured at room temperature and reach a high deflection temperature. Unidirectional basalt fiber fabrics are commercially available. As indicated, fiber diameter is 13 micron; the area density of the fabric is 360 g/m2; tensile strength is 2.1GPa and modulus is 105GPa. BFRP prepared with a hand wet layup process. First, a pre-cut fabric, laid on a flat surface, was saturated with enough epoxy resin system. The more resin was pressed out from the fabric with a plastic trowel. Two layers of fabric was used for a samples of the dimensions of 300 300 mm2. After cured in the lab (around 23 ) for 7 days, the plate was cut into 25mm250mm strips completely along the fiber direction. Those strips used for tensile testing will be post-cured at an oven of 110 for 2 hours. Figure 1 shows cut strip for following testing.

for 5 coupons for each condition. Tensile testing: The tensile properties of the strips are tested according to ASTM D3039 with a WDW-100D electronic tensile machine, which produced by Shandong Shidai Company. The tensile strain was measured with a strain gauge. The alkaline solution is prepared according to ACI 440 standards, whose pH value about 13.5.

Figure 2 Caption of a typical figure. Photographs will be scanned by the printer. Always supply original photographs


3.1 Basic physical and mechanical properties The fiber volume content of the cured samples was determined through burning method. As calculated that the fiber content is about 47 vol.%. The glass transition temperature of the BFRP is determined with differential scanning calorimetry (DSC) technology with 10 /min heating rate. The fully cured system has a glass transition temperature 82 . Figure 3 shows a typical tensile curve of a BFRP strip,

Figure 1 BFRP strips used for tensile testing



Water uptake testing: The cured sample coupons were cut into 2525 mm2 with the original thickness for water sorption tests. Samples were soaked in distilled water baths or alkaline solution at 23, 40, 60 and 80 , respectively. Figure 2 shows the samples immersion in the distilled water. The moisture uptake was detected by periodically measuring the mass of the samples. For specimens aged in water, samples were taken out of the baths, swiped off the surface water using tissue papers and weighted using an electronic balance with an accuracy of 0.01 mg. The presented data are an average

Figure 3 Typical tensile stress vs. strain curve of BFRP according to ASTM D3039


Proceedings of the 5th International Conference on FRP Composites in Civil Engineering

which exhibits a good linearity. The tensile strength, modulus and elongation are averaged from 10 samples, listed in Table 1.
Table 1 Tensile properties of BFRP tested according to ASTM D3039 Strength (MPa) 602.9 STD 29.2 Modulus (GPA) 29.7 STD 2.8 Elongation at break (%) 2.2 STD 0.22

indicates that the degradation of the BFRP samples is faster in alkaline solution than in water. The result further supports the aforehand state.

It is worth noting that the tensile properties of BFRP wet layups are about 10% higher than the glass fiber reinforced FRP composites, which using the same epoxy resin system and curing process. 3.2 Water uptake
Figure 5 Water uptake vs. square time of BFRP samples immersed in distilled alkaline solution

Figures 4 and 5 give the water uptake curves of the BFRP samples immersed in water or alkaline solutions at various temperatures. As shown, some important phenomena can be found and summarized below.


Degradation of the tensile properties

The variation of the tensile strength and tensile modulus of BFRP samples immersed in alkaline solution are presented in Figures 6 and 7, respectively. Clearly, alkaline solution immersion brings in a dramatically reduction of the tensile strength, especially at elevated temperatures (Figure 6). After 3 months immersion, the remaining tensile strength only about 1/3 of the original value at high immersion temperatures. Even at room temperature, the strength decreased by about 23%.

Figure 4 Water uptake vs. square time of BFRP samples immersed in distilled water

With increased immersion temperature, the water uptake in the same period increased also. It is because the water diffusion process is thermal activated. The higher immersion temperature, the high water diffusion rate reaches(Xian et al., 2007, Wrosch et al., 2008, Karbhari et al., 2009). At the same immersion temperature (except 80 ), the sample immersed in water shows a less water uptake ratio compared to the sample immersed in alkaline solution. This indicates that BFRP suffered more degradation in alkaline solutions. At 80 , BFRP samples reach the maximum water uptake after one month immersion, and display an observable weight loss (Figure 4 and 5). More weight loss is found in the case of alkaline immersion. As believed, such weight loss is related to the hydrolysis of epoxy resin or the fibers (Wrosch et al. 2008). More remarkable weight loss of the sample in alkaline solution

Figure 6 Variation of tensile strength of BFRP samples as a function of immersion time in alkaline solution

During the beginning immersion period (e.g., less than one month), the tensile strength degraded quickly at high temperatures. After that, the degradation slows down. For 23 alkaline solution immersion condition, the tensile strength firstly increases after first 7 days immersion, which is attributed to the possible stress release effect. As regarding the tensile modulus, on the contrary, alkaline solution immersion shows a slightly effect.

September 2729, 2010, Beijing, China


water or alkaline solution, the water uptake increased with immersion temperature. The weight loss after maximum absorption of water at 80oC indicates a possible hydrolysis of resin system and damage of basalt fibers. BFRP samples shows a remarkable decrease in tensile strength after immersion in distilled water or alkaline solutions for a short period (e.g., 1 month), while the modulus is less affected. In addition, BFRP is vulnerable to the alkaline solution attack, which is reflected by a more serious degradation in the tensile properties and more water uptake when immersed in alkaline solution.
Figure 7 Water uptake vs. square time of BFRP samples immersed in distilled alkaline solution

Karbhari, V. M. and Xian, G. J. (2009). Hygrothermal effects on high V-F pultruded unidirectional carbon/epoxy composites: Moisture uptake. Composites Part B-Engineering 40(1): 41-49. Liu, O., Shaw, M. T. Parnas, R. S and McDonnell, A. M. (2006). Investigation of basalt fiber composite aging behavior for applications in transportation. Polymer Composites 27(5): 475-483. Sim, J., Park C. and Moon D. Y. (2005). Characteristics of basalt fiber as a strengthening material for concrete structures. Composites Part B-Engineering 36(6-7): 504-512. Wang, M. C., Zhang Z. G., Li, Y., Li, M. and Sun, Z. J. (2008). Chemical durability and mechanical properties of alkali-proof basalt fiber and its reinforced epoxy composites. Journal Of Reinforced Plastics And Composites 27(4): 393-407. Wrosch, M., Xian, G. J. and V.M.Karbhari. (2008). Moisture absorption and Desorption in a UV cured urethane acrylate adhesive based on radiation source. Journal Of Applied Polymer Science 107(6): 3654-3662. Xian, G. J. and Karbhari. V. M. (2007). DMTA based investigation of hygrothermal ageing of an epoxy system used in rehabilitation. Journal of Applied Polymer Science 104(2): 1084-1094.

Especially, there is no a clear temperature effect. The 60 alkaline solution aged samples do not exhibit decreases in the modulus, while 23 alkaline solution aged ones display the lowest modulus. As believed, the modulus are measured in the low strain range, e.g., <0.4%. The possible damage of the fiber surface or the resins may not affect the stiffness in this stage. Similar trends of the tensile properties are found for BFRP samples immersed in distilled water at various time. It should be noted that the degradation degree is much less than that immersed in alkaline solution. This is consistent with the result of water uptake testing. The resin or the fibers may be vulnerable to the alkaline solution attack, which is responsible for the above results.

BFRP wet layups were prepared with an epoxy resin system and basalt fiber fabric. The tensile properties of un-aged samples are superior to those of glass fiber reinforced FRP composites. When immersed in distilled