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Construction and Building Materials: Mathieu Robert, Brahim Benmokrane
Construction and Building Materials: Mathieu Robert, Brahim Benmokrane
Construction and Building Materials: Mathieu Robert, Brahim Benmokrane
h i g h l i g h t s
" A durability study of GFRP bars submitted to salt solution and concrete is proposed.
" Mechanical and physical characterizations were performed on aged bars.
" GFRP bars have shown high tensile strength retention after aging.
" No chemical degradation of the polymer as detected after aging.
" Prediction of long-term tensile strength were performed.
a r t i c l e i n f o a b s t r a c t
Article history: This paper presents the mechanical, durability, and microstructural characterization of unstressed glass–
Received 18 February 2012 fiber-reinforced-polymer (GFRP) reinforcing bars exposed to concrete environment and saline solutions
Received in revised form 26 July 2012 under accelerating conditions. These conditionings were used to simulate the effect of seawater or deic-
Accepted 11 August 2012
ing salts on GFRP bars. The pre- and postexposure tensile strengths of the bars were used for long-term
Available online 29 September 2012
property predictions based on the Arrhenius theory. The results revealed no significant differences in the
durability of the concrete-wrapped GFRP bars whether immersed in salt solution or tap water and the
Keywords:
very high long-term durability of the GFRP bars in salt solution. According to the predictions, even after
Durability
Glass FRP
a service life of 100 years, the tensile-strength retention of the tested GFRP bar would still be 70% and 77%
Bars for mean annual temperatures of 50 °C (the mean annual temperature and the marine environment of the
Salt Middle East and warm regions) and 10 °C (mean average temperature of northern regions), respectively,
Alkaline which are higher than the design tensile strength according to the ACI 440.1R.
Concrete Ó 2012 Elsevier Ltd. All rights reserved.
Marine
Aging
Mechanical properties
Strength prediction
0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.08.021
M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284 275
2. Background and research to date interface in the fiber direction could be a predominant mechanism
of moisture ingress [19,20]. Nonvisible dissociation between fibers
The strength of glass fibers and the resin matrix—two GFRP con- and matrix could lead to rapid losses of interfacial shear strength
stituents—can decrease when subjected to wet alkaline or saline [9].
environments. Thus, an adequate durability study of GFRP materi- In order to evaluate long-term durability performance of FRP in
als should be performed for FRP reinforcing bars to gain wide harsh environments, extensive studies have been conducted to de-
acceptance in the construction industry. Considerable research velop accelerated aging procedures and predictive models for long-
has been conducted in the past decade to assess the suitability of term strength estimates, especially for GFRP bars [21–24]. These
FRP reinforcement in reinforced-concrete structures [1–4]. The models are based on the Arrhenius model [25]. Research on the ef-
work of these researchers has highlighted the short-term perfor- fects of temperature on the durability of FRP bars in concrete alka-
mance of FRP-reinforced concrete structures or the durability of line environments indicates that an acceleration factor for each
FRP reinforcing bars subjected to aging in alkaline solutions. Some temperature difference can be defined using Arrhenius laws. These
researchers have reported on the durability of GFRP bars embed- factors differ for each product, depending on the types of fiber and
ded in moist concrete, which simulates actual application condi- resin, and bar size. In addition, these factors are affected by envi-
tions, and on the adverse effects of cracks and microcracks in ronmental conditions, such as surrounding solution media, tem-
GFRP bars on their long-term durability [5]. Nevertheless, the data perature, pH, moisture, and freeze–thaw conditions. Predictive
on the durability of GFRP bars subjected to the combined effect of models based on Arrhenius laws make the implicit assumption
moist concrete and saline solution is very limited. that the elevated temperature will only increase the rate of degra-
The resins widely used for FRP composites include polyester, dation without affecting the degradation mechanism or introduc-
vinylester, and epoxy. Weak adhesion of polyester or vinylester ing other mechanisms. Gerritse [26] indicated that at least three
can result in serious deterioration when hydroxyl ions penetrate elevated temperatures were necessary to perform an accurate
the structure [6]. On the other hand, a considerable drawback of predication based on Arrhenius laws. Moreover, the measured data
epoxy is that it can absorb from 1% to 7% moisture by weight, should be in continuous time intervals. We followed those recom-
which plasticizes the matrix, inducing differential swelling stres- mendations for this study.
ses, and generally degrades the physical properties [7]. In general,
the matrix could be damaged through cracking and microcracking 2.1. Research gaps and statement of the problem
due to volume expansion during moisture absorption, whereas its
stiffness could be reduced by plasticization. A subsequent mecha- Several studies have addressed the durability of GFRP reinforc-
nism of degradation resulting from the breaking of polymer chains ing bars [1,2,24], including FRP-wrapped concrete cylinders [27–
triggered by hydrolysis and the leaching out of low molecular- 30]. Very limited studies, however, have been conducted on the
weight material from the bulk resin could further damage the ma- durability of GFRP reinforcing bars subjected to saline solution or
trix [8–10]. The matrix formed by vinylester, which contains much to the combined effect of saline solution and the alkaline environ-
fewer ester units compared to polyester, is hardly deteriorated by ment of the concrete surrounding the bar. The properties of the
hydroxyl ions compared to a polyester matrix. pultruded products (void content, interface quality, and fiber dis-
E-glass fibers are the most susceptible to degradation due to tribution) and the nature of the aggressive environment can lead
moisture and alkalinity [11]. Dejke [12] reported that glass fibers to important changes in the behavior and durability of the final
are known to degrade in the presence of water, and that moisture product. As such, the available knowledge on the durability of
can decrease the glass transition temperature (Tg) of the resin and GFRP reinforcing bars subjected to typical alkaline solutions as
act as a plasticizer, potentially having significant effect on the specified by ACI 440.3R-04 [31] may not be directly applicable to
strength of GFRP materials. The reaction of GFRP composite with GFRP bars subjected to salt and concrete at the same time. In fact,
the alkali in concrete is a major durability concern. Typically, con- FRP reinforcing bars can be subjected to aggressive alkaline envi-
crete environments have high alkalinity, depending on the design ronments from the concrete and to an aggressive external saline
mixture and type of cement used [13,14]. This alkaline environ- environment in marine applications or from deicing salts. No stud-
ment damages glass fibers through loss in toughness and strength ies have focused on this possible combined effect. In addition, engi-
and through embrittlement. Glass fibers are damaged due to the neers now aim to design structures with service lives of from 75 to
combination of two processes: (1) chemical attack on the glass fi- 150 years, thereby requiring studies that predict the durability and
bers by the alkaline cement environment, and (2) concentration service life of the new GFRP materials used in concrete
and growth of hydration products between individual filaments infrastructure.
[15]. Fiber embrittlement is due to the nucleation of calcium
hydroxide on the fiber surface. Hydroxylation can cause fiber sur- 3. Experimental approach
face pitting and roughness, which act as flaws, severely reducing
fiber properties in the presence of moisture. In addition, calcium, 3.1. Material
sodium, and potassium hydroxides in the concrete pore solution
Sand-coated GFRP bars were used in this study. The bars were made of contin-
are aggressive to glass fibers [16]. Therefore, the degradation of
uous E-glass impregnated in a vinylester resin using the pultrusion process. The fi-
glass fibers depends not only on a high pH level, but also on the ber mass fraction was 77.9% as determined by thermogravimetric analysis
combination of alkali salts, pH, and moisture. according to ASTM E1131 [32]. The relative density of the GFRP bars according to
The deterioration at the interfaces between the fibers and the ASTM D792 [33] was 1.99. The bars had a nominal diameter of 12.7 mm. The
matrices involves a much more complex mechanism [17]. The mechanical and physical properties of the GFRP reference bars are summarized in
Table 1. All bars were cut into 1440 mm lengths, as specified by ACI 440.3R-04
interface is a nonhomogeneous region about 1 lm thick. This layer B2 [31]. The bars were divided into two series: (1) unconditioned reference sam-
is weakly bonded and most vulnerable to deterioration [17]. The ples; and (2) conditioned samples (130 bars) embedded in concrete and aged in a
three dominant deterioration mechanisms include matrix osmotic saline solution. The mortar mixture consisted of 3 parts sand, 1 part type I cement
cracking, interfacial debonding, and delamination [18]. The mois- (according to ASTM C150 [34]), and a water–cement ratio of 0.40, which yielded a
concrete pH of 12.15, measured by extracting interstitial solution after the aging
ture diffusion into FRP composites could be influenced by the
process. The concrete (or mortar) was cast only around the middle third of the bars
material’s anisotropic and heterogeneous character. Along with to avoid any degradation at the ends, which were used as grips during tensile test-
diffusion into the matrix, wicking through the fiber/matrix ing according to ACI 440.3R-04 B2 [31]. The concrete mold was made of wood with
276 M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284
Table 1
Tensile properties and physical properties of the 12.7-mm-diameter GFRP bars.
Eq. (2) expresses the Arrhenius relation in terms of the degradation rate [39]:
Ea
k ¼ A exp ð2Þ
RT
where k is the degradation rate (1/time); A the constant relative to the material and
degradation process; Ea the activation energy of the reaction; R the universal gas
constant; and T is the temperature in Kelvin. The primary assumption of this model
is that only one dominant degradation mechanism of the material operates during
the reaction and that this mechanism will not change with time and temperature
during the exposure [24]. Only the rate of degradation accelerated with the temper-
ature increase. Eq. (2) can be transformed into:
1 1 Ea
¼ exp ð3Þ
k A RT
1 Ea 1
Fig. 2. Wood container built for aging of the cement mortar-wrapped GFRP bar ln ¼ lnðAÞ ð4Þ
k R T
specimens.
M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284 277
From Eq. (3), the degradation rate k can be expressed as the inverse of time Table 2
needed for a material property to reach a given value [24]. Eq. (4) further shows that Experimental tensile strength of the reference GFRP bars and GFRP bar specimens
the logarithm of time needed for a material property to reach a given value is a lin- aged in the saline solution at 23 °C, 40 °C, 50 °C, and 70 °C.
ear function of 1/T with a slope of Ea/R [24]. Ea and A can be easily calculated with
the slope of the regression and the point of intersection between the regression and Immersion Temperature Mean tensile Standard
the Y-axis, respectively. duration (d) (°C) strength (MPa) deviation (MPa)
0 23 788 54
3.6. Differential scanning calorimetry (DSC) 60 23 781 32
40 777 42
DSC was used to obtain information on the thermal behavior and characteristics 50 764 23
of polymer materials and composites, such as glass transition temperature (Tg),
120 23 772 26
melting point, curing process, crystallinity, thermal stability, and relaxation. In
40 760 43
our study, specimens weighing 12–15 mg were cut from different GFRP samples
50 753 20
(unconditioned GFRP specimens aged in saline solution and moist mortar at 50 °C
70 744 34
for 365 d, and GFRP specimens aged in saline solution and moist mortar at 70 °C
for 120 d), placed in aluminum pans, and were analyzed using a TA Instruments 210 23 763 38
DSC Q10 calorimeter. Specimens were heated from 25 °C to 195 °C at a rate of 40 745 38
5 °C/min. The glass transition temperature of the specimens was determined in 50 744 40
accordance with ASTM E1356 [40]. A decrease in Tg observed for the conditioned
365 23 726 13
samples was deemed an indication of the plasticizing effect or chemical degrada-
40 712 53
tion. Aged samples maintaining Tg lower than the reference displayed irreversible
50 702 22
chemical degradation.
4. Experimental results
Fig. 5. Elastic modulus of GFRP bars aged in the saline solution at 23 °C, 40 °C, 50 °C,
and 70 °C.
was observed on bar surfaces before testing. Micelli and Nanni [4]
observed similar tensile failure modes with GFRP bars.
Table 2 provides the experimental results from tensile testing
Fig. 3. Typical failure mode of GFRP bars for: (a) an unconditioned GFRP
specimen;(b) a mortar-wrapped GFRP bar aged in the saline solution for 365 d at
related to the ultimate strength of aged GFRP bars tested after
50 °C; and (c) a mortar-wrapped GFRP bar aged in the saline solution for 120 d at accelerated aging at 23 °C, 40 °C, and 50 °C. Table 2 shows that
70 °C. the tensile strength for unconditioned the GFRP bars was
278 M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284
Table 3
Water absorption at saturation before and after conditionings in the solution.
Fig. 6. Micrograph of the bar/coating interface (50) of: (a) an unconditioned GFRP bar; (b) a mortar-wrapped GFRP bar aged in the saline solution for 365 d at 50 °C; and (c) a
mortar-wrapped GFRP bar aged in the saline solution for 120 d at 70 °C.
788 ± 54 MPa. Note that the tensile strength dropped to reaction of degradation with immersion temperature, leading to a
702 ± 22 MPa for bars immersed for 365 d in salt solution at higher absorption rate of the solution for the same time of immer-
50 °C. Robert et al. [2] reported that the tensile strength of similar sion and accelerated degradation reaction. The absorption of solu-
bars dropped to 665 ± 62 MPa after 240 d of exposure to water at tion can lead to degradation of the fibers and fiber/matrix interface,
50 °C, indicating that immersion in the saline solution had no more leading to a loss in ultimate tensile strength. In a similar study,
impact on the durability of GFRP bars than immersion in tap water. Robert et al. [2] recorded losses of resistance of 16%, 10%, and 9%
The tensile strength of the GFRP bars subjected to very high after 240 d of aging of embedded GFRP bars immersed in tap water
temperatures (70 °C) for 120 d decreased to 744 MPa ± 34 MPa, at 50 °C, 40 °C, and 23 °C, respectively.
which is similar to the tensile strength (747 ± 11 MPa) of similar
bars embedded in concrete and aged in tap water under the same 4.2. Effect on Young’s modulus
immersion conditions.
Fig. 4 shows the retention of the ultimate strength of aged GFRP Fig. 5 shows the change in the elastic modulus of the aged GFRP
bars according to the duration of immersion at various tempera- bars according to length of immersion at various temperatures. In-
tures. Fig. 4 shows a slight decrease in the ultimate tensile strength deed, the measured results show that, even after 365 d, the losses
of GFRP bars as the length of immersion increased. Furthermore, in elastic modulus of the GFRP bars were negligible and that all
immersion temperature clearly affected loss of strength. The aged bars were not affected by the higher temperatures or the
Fig. 4 shows that the loss of strength was 14%, 12%, and 10% at exposure to the saline solution when embedded in concrete. This
50 °C, 40 °C, and 23 °C, respectively, for 12 months of immersion. result indicates that the elastic modulus of GFRP bars is not af-
This phenomenon is due to the increasing diffusion rate of the fected by aging in a concrete environment with saline solution
solution inside the sample and to the acceleration of the chemical simulating seawater or deicing salts.
M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284 279
Fig. 7. Micrograph of the bar/coating interface (5000) of: (a) an unconditioned GFRP bar; (b) a mortar-wrapped GFRP bar aged in the saline solution for 365 d at 50 °C; and
(c) a mortar-wrapped GFRP bar aged in the saline solution for 120 d at 70 °C.
4.3. Results of water-immersion testing at 50 °C, and (c) a mortar-wrapped GFRP bar aged in the saline
solution for 120 d at 70 °C.
Table 3 presents water uptake at saturation of GFRP bars Observation of these interfaces and the microstructure in gen-
embedded in mortar before and after conditioning in saline solu- eral demonstrate that conditioning of mortar-wrapped bars in
tion. The results presented in Table 3 are the average values ob- water did not affect the microstructural properties of the GFRP
tained from five test specimens. These results show that the bars. This is in accordance with what Robert et al. [2] reported
moisture absorption at saturation of the GFRP bars was not af- when similar mortar-wrapped GFRP bars were immersed in tap
fected by aging in saline solution. The measured moisture uptake water. This phenomenon clearly illustrates that GFRP bars are
at saturation of the GFRP bars was 0.14%, 0.15%, and 0.13%, before not significantly affected by accelerated aging in saline solution.
immersion in the saline solution, after immersion in the saline
solution for 365 d at 50 °C, and after immersion in the saline solu- 4.5. Bar/concrete interface
tion for 120 d at 70 °C, respectively. The slight variation of mois-
ture absorption is related to the precision of the balance used for If there were any degradation in the GFRP-bar resin or fibers at
the measurement. the interface between the bar and concrete, it is expected that
bond mechanisms and the durability of reinforced member would
4.4. Microstructural effects be affected. Fig. 8 shows the GFRP bar/concrete interface for (a) an
unconditioned reference bar, (b) a specimen embedded in concrete
The visual and microstructural observations of the GFRP bars and aged in saline solution at 50 °C for 365 d, and, (c) a specimen
showed no significant damage after 365 d of immersion in the sal- embedded in concrete and aged in saline solution at 70 °C for
ine solution at 50 °C or after 120 d of immersion at the highest 120 d. Moreover, there was no significant damage to the bar/con-
temperature (70 °C). The micrographs in Fig. 6 show the interface crete interface after aging in saline solution, even at high temper-
between the mixture of fibers and resin and the silica coating of ature (70 °C).
the GFRP bars for (a) an unconditioned GFRP bar, (b) a mortar-
wrapped GFRP bar aged in the saline solution for 365 d at 50 °C, 4.6. Effects on polymer matrix
and (c) a mortar-wrapped GFRP bar aged in the saline solution
for 120 d at 70 °C. Fig. 7 shows micrographs of the fiber/matrix FTIR analysis of unconditioned bars and 12.7-mm mortar-
interface for the GFRP bars for (a) an unconditioned GFRP bar, (b) wrapped bars aged in saline solution at 50 °C for 365 d was con-
a mortar-wrapped GFRP bar aged in the saline solution for 365 d ducted (Fig. 9). This analysis was performed to determine if
280 M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284
Fig. 8. Micrographs of the GFRP bar/concrete interface of: (a) an unconditioned specimen; (b) a conditioned bar specimen aged in the saline solution at 50 °C for 365 d; and
(c) a conditioned bar specimen aged in the saline solution at 70 °C for 120 d.
Table 4
Results of differential-scanning-calorimetry (DSC) analysis.
Conditioning Temperature (°C) Duration (d) Tg run 1 (°C) Tg run 2 (°C) Cure ratio (%)
Unconditioned 116 117 99
Embedded in concrete and immersed in the saline solution 50 365 115 118 99
Embedded in concrete and immersed in the saline solution 70 120 117 118 99
than the design tensile strength according to the ACI 440 [41]
(guaranteed tensile strength multiplied by the environmental
reduction factor = C E ffu ).
Acknowledgments
A.1. Introduction
of 10 °C and 50 °C, respectively. It was shown that the service
life needed to reach a tensile-strength retention of less than The model used in this study to predict the tensile strength of
70% at 10 °C should be infinite. aged specimens is based on the Arrhenius relation and is similar
6. Civil engineers currently aim at designing structures for service to that used for glass–fiber reinforced concrete (GRC) by Litherland
lives of up to 100 years. According to the predictions, even after et al. [25] and described by Bank et al. [23]. The procedure provides
a service life of 100 years, the tensile-strength retention of the a predicted service life for the FRP composite material at a desired
tested GFRP bar would still be 70% and 77% for mean annual level of strength retention, or provides the level of strength re-
temperatures of 50 °C and 10 °C, respectively, which are higher tained at a desired service life. The method is based on the Arrhe-
Fig. A2. Arrhenius plots for (a) service life as a function of temperature and percent retention and (b) property retention as a function of temperature and service life.
M. Robert, B. Benmokrane / Construction and Building Materials 38 (2013) 274–284 283
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