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Composites: Part B
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a r t i c l e
i n f o
Article history:
Received 24 February 2011
Received in revised form 17 May 2011
Accepted 3 July 2011
Available online 13 July 2011
Keywords:
A. Resins
B. Cure behaviour
B. Stress transfer
D. Mechanical testing
FRP (bre reinforced polymer)
a b s t r a c t
Civil structures such as bridges and buildings can be strengthened with prestressed bre reinforced polymer (FRP) strips to enhance both their stiffness and load-bearing capacity. End anchorage is a crucial
issue for prestressed FRP strips. An innovative anchorage procedure, called the gradient anchorage
method and based on the possible accelerated curing of the epoxy-resin in the end region of the FRP
strip, has recently been conceived with the aim of avoiding more invasive mechanical fastening systems.
An in-depth knowledge of the actual development of the key mechanical properties of resins under different curing conditions (i.e., in terms of curing temperature) is of paramount importance for employing
the above mentioned gradient method in practical applications. This paper presents experimental results
and analytical investigations aimed at developing a better understanding of the strength development of
a commercial adhesive under different curing times and temperatures. Firstly, direct tensile tests on
epoxy specimens were performed at different curing temperatures. It was shown that the necessary curing time to reach the maximum tensile strength can be signicantly reduced from several hours at room
temperature to approximately 30 min at 90 C. Furthermore, higher curing temperatures reduced the
activation time after which strength starts to increase. The experimental observations are shown graphically with both the activation time and reaction duration at different curing temperatures. Secondly,
pull-off bond tests were conducted on 100 mm wide and 1.2 mm thick FRP strips bonded to concrete
using epoxy adhesives cured either at 90 C for different durations or at room temperature. An optical
image correlation system (ICS) allowed the load transfer behaviour of the inhomogeneous cured adhesive
between the FRP strip(s) and concrete to be studied. Finally, using the experimental measurements, the
bond shear stressslip interface relationships for the different test specimens were identied in order to
present the effect of elevated curing temperatures and curing durations.
2011 Elsevier Ltd. All rights reserved.
1. Introduction
The ageing of existing civil structures and the enhancement of
safety standards in structural codes are two important reasons
for the increasing interest of the structural engineering community
in developing cost-effective strengthening techniques. For instance, active reinforcement of existing members through prestressing techniques can signicantly enhance both stiffness and
strength of those members, with a more rational and efcient
exploitation of the mechanical properties of the reinforcing materials. Using bre reinforced polymers (FRPs) for external prestressing of existing reinforced concrete (RC) members is one of the most
innovative active techniques for structural strengthening.
Corresponding author. Tel.: +41 58 765 55 11 11; fax: +41 58 765 44 55.
E-mail address: christoph.czaderski@empa.ch (C. Czaderski).
Permanent address: University of Salerno, Dept. of Civil Engineering, via Ponte
don Melillo, 84084 Fisciano, Italy.
1
1359-8368/$ - see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesb.2011.07.006
399
Nomenclature
F
Fu
f(t)
fa
ta
tr
m
n
t
ttot
tn
th
tc
T
Tavg
smax
s
sel
smax
su
sT
Ef
tf
bf
L
kel
nm
x
xel
heating duration
cooling duration
curing temperature
mean temperature during pull-off test
maximum shear strength (see Fig. 17)
FRP-to-concrete interface slip
slip at end of elastic branch (see Fig. 17)
slip at debonding (see Fig. 17)
ultimate slip
the total number of specimens cured at temperature T
strip elastic modulus
strip thickness
strip width
bond length
elastic stiffness (see Fig. 17)
number of displacement measurements
abscissa of the coordinate axis system
point on the abscissa at which s(xel) = sel
400
Table 1
State-of-the-art summary on curing temperature and time effect on epoxy strength evolution and end strength (RT = room temperature).
Author
Adhesives
Experiments
Curing
temperature
Araldite
High-temperature epoxies
18150 C
60 min to
20 days
3.350 h
1040 C
34 to 49 C
114 days
2472 h
25120 C
0.0813.8 h
RT to 150 C
5 h step curing
Similar observations have been made by Matsui [13], who studied the effects of curing conditions on the development of both
shear strength and stiffness for two kinds of adhesive (namely,
epoxypolyamideamine and cyanoacrylate, only the rst one being
used for structural purposes). In general, the author observed that
the minimum curing duration needed for reaching the maximum
shear strain was clearly related to the curing temperature.
Tu and Kruger [14], after testing two different epoxy resins
(with and without silica ller) in pull-out tests according to ASTM
C882-87 [15], observed an increase in bond strength with higher
curing temperature at a constant curing duration (7 days).
A large number of torque tests with a circular FRP composite
laminate bonded to a concrete cylinder were presented by Dutta
and Mosallam [16]. The investigation presented four different
epoxy-based adhesives tested at various curing temperatures ranging from 34 to 49 C with different curing durations. Similar conclusions as those made by the previous researchers regarding
strength evolution were drawn.
Although all experimental observations pointed out the huge
inuence of the curing conditions on the development of the relevant mechanical parameters, no quantitative formulations have
been proposed so far for expressing this relationship between, for
instance, the actual value of the tensile strength f(t) of epoxy resins
at curing time t and the corresponding curing temperature. Only
the following rule of thumb is given by Mays and Hutchinson
[8], who observed that, for curing temperature higher than 5 C,
the curing duration needed for achieving the nal strength of the
resin is halved for every increase of 10 C in temperature.
2.2. Inuence of curing temperature on the end strength of adhesives
In addition to studying the development of the relevant
mechanical properties of adhesives, various researchers have analysed the end strength of resins and its possible relationship with
the curing temperature. For instance, Dutta and Mosallam [16] observed higher end torque strengths for higher curing temperatures.
Cao and Cameron [17] conrmed this observation by investigating an additional effect. Instead of using isothermal curing, consisting of rapidly heating the resin specimen to the desired
temperature, the heating was carried out in various steps, starting
at a low temperature and increasing it in a step-wise manner for
different curing durations. According to the authors observations,
this technique leads to a more uniform curing of the adhesive layer
and, thus, results in a better mechanical performance.
Dodiuk and Kenig [12] observed both higher exural strength
and stiffness of specimens cured at 60 C and 120 C in comparison
to epoxies cured at room temperature.
Curing
duration
401
Experimental investigation
Modulus of elasticity Ef
(GPa)
Modulus of elasticity Ef
(GPa)
Tensile strength fu
(MPa)
Width bf
(mm)
Thickness tf
(mm)
1
2
3
4
5
6
169
173
179
174
171
177
173.9
2975
1.142
100
1.23
Mean
value
174
Fig. 1. Specimens for axial tensile tests, on the left side (Nos. 10 and 11) the
aluminium stamps and plates with applied adhesive in between can be seen, on the
right side (No. 12) the stamp including the xture for the curing process is visible.
Fig. 3. Axial tensile test specimens inside the oven and cables for temperature
measurements.
402
120
Room Temperature
Sensors on the adhesive
Temperature [ oC]
90
60
30
100
200
300
Time [mins]
125
Room Temperature
Sensors on the adhesive
Temperature [C]
100
75
50
25
50
100
150
Time [mins]
Fig. 4. Typical temperature development during curing of the axial tensile test
specimens, including the temperature decrease due to removal of the test
specimens from the oven.
Table 3
Overview of the experimental programme for the axial tensile tests on S&P resin 220
(SH: oven in testing hall, OR: oven in oven room).
Series
[#]
n.
T (C)
n.
4
12
90
90
1
2
3
4
5
6
7
8
9
10
11
12
19
7
90
90
16
16
24
24
14
65
45
90
65
90
Total
136
12
48
24
4
24
23
12
8
4
36
168
168
64
Oven
tmax (h)
SH
SH
SH
SH
SH
SH
OR
OR
OR
Six pull-off bond tests were carried out with the aim of measuring the strength of FRP-to-concrete joints. In particular, the time
evolution of the mechanical properties of those joints cured at high
temperature was the key issue of this investigation. Fig. 5 shows a
view of the test layout: a 100 mm wide and 1.2 mm thick FRP strip
was glued to a concrete block and pulled off after either curing at
an elevated temperature (approx. 90 C) or at room temperature.
The bond length was 300 mm and the heating was performed
using three heating elements each with a dimension of
100 mm 100 mm. The pull-off bond tests were prepared following the main phases represented in Fig. 6. The tested specimens
were always equipped with sensors for monitoring the temperature evolution within both the adhesive layer and the heating elements. The preparation of the adhesive layer between the FRP strip
and concrete surface was followed by the heating phase (th), carried out by means of heating elements. After stopping the heating
procedure, a cooling time of 510 min was included before starting
403
Table 5
Results of the axial tensile tests on specimens cured at room temperature (n = number
of tests, T = curing temperature, t = curing time, F = maximum tensile force, fa = axial
tensile strength).
Fig. 6. Adhesive temperature (T1, T2, T3) and force development of Test No. 3 (pulloff bond tests), th: heating duration, tc: cooling duration, Tavg: mean temperature
during pull-off test, Fu: ultimate force, L = bond length, T1, T2, T3 = temperatures in
the adhesive at the positions 1, 2, 3 (see schematic drawing).
Table 4
Overview of the experimental programme for the pull-off bond tests.
Test
No.
Mean
distance
concrete
surfaceupper
strip
surface
(mm)
Strip
thickness
(mm)
Mean
adhesive
thickness
(mm)
Heating
duration
th (min)
Waiting
time to
failure
test tc
(min)
Average test
temperature
Tavg (C)
1
2
3
4
5
6
4.85
5.14
5.00
4.90
4.74
4.93
1.2
1.2
1.2
1.2
1.2
1.2
3.65
3.94
3.80
3.70
3.54
3.73
15
25
20
25
25
5.7
8.6
5.8
7.7
2 days
3 days
45
43
41
42
19
18
Series
T (C)
t (h)
F (kN)
fa (MPa)
1
4
5
7
8a
8b
9
12
24
4
12
4
4
4
2426
22
24
10
10
22
22
4.048.0
4.024.0
7.022.9
6.336.0
48168
48168
48168
0.086.15
0.036.18
1.496.13
0.035.06
4.404.95
5.766.44
5.846.41
0.2519.6
0.119.7
4.719.5
0.116.1
14.015.8
18.320.5
18.620.4
the loading test in order to cool down the adhesive (tc). Afterwards,
one can observe the force increasing up to the maximum value Fu.
It can be observed that the temperature during the experiment was
not constant, but slowly decreased. The heating and cooling times,
as well as the average test temperature (Tavg), are given in Table 4.
The cooling time was chosen so that the existing temperature in
the adhesive was safely below its glass transition temperature.
The full-eld 3D displacements of the test specimen were measured during the experimental investigations with an optical
Fig. 7. Isolines of the surface of the CFRP strip before the start of the pull-off test determined by using the ICS.
404
Table 6
Results of the axial tensile tests on specimens cured in an oven (n = number of tests,
T = curing temperature, t = curing time, F = maximum tensile force, fa = axial tensile
strength).
Series
T (C)
t (h)
F (kN)
fa (MPa)
2
3
5
6
8
9
10
11
12
4
12
19
7
16
16
24
24
14
90
8890
8889
90
65
45
90
65
90
1.01.3
0.84.0
0.73.7
0.40.6
0.72.7
0.74.0
0.252.5
0.522.5
0.30.7
2.873.88
1.365.66
1.287.14
0.232.03
0.056.41
0.06.10
0.07.2
0.315.94
03.4
9.112.35
4.318.0
4.122.7
0.76.5
0.1620.4
0.019.4
0.022.9
1.018.9
010.8
405
Table 7
Results of the pull-off bond tests (Fu = maximum force at failure or at initiation of
debonding, smax = maximum bond strength, sel = slip at maximum bond strength,
smax = maximum slip at full debonding, wt: waiting time to failure test 2 or 3 days).
Test
No.
Heating
duration (min)
Fu
(kN)
smax
(MPa)
sel
(mm)
smax
(mm)
Failure
mode
1
2a
3
15
25
20
18.4
60.4
34.4
0.8
5.1
1.4
0.602
0.205
0.803
0.652
0.408
0.803
4
5
6
25
25 + wt
wt
75.7
62.0
57.6
4.4
7.7
7.9
0.426
0.020
0.031
0.712
0.248
0.218
Adhesive
Concrete
Mainly
adhesive
Concrete
Concrete
Concrete
Fu is not the force at failure, due to problems with the test set-up.
60
15
25
25*
Test No.6
20
Test No.5
Test No.2*
Test No.4
20
Test No.3
40
Test No.1
80
25 + 2 days no heating +
waiting time
3 days
waiting time
the test specimens after failure. For test specimen No. 1, the resin
was not completely cured after only 15 min, which resulted in a
failure process in the adhesive layer without any cracks developing
in the concrete. A substantially similar behaviour was observed for
the specimen cured for 20 min (Test No. 3), although a small concrete failure area is visible. On the contrary, the other specimens
failed with a fracture developing throughout the concrete substrate (Test Nos. 2, 4 and 5) as was the case for the reference test
(No. 6).
Another interesting observation is presented in Fig. 11, where
the isolines of the displacements in the direction of the applied
pulling force (x-direction) determined with the ICS for specimens
Nos. 4 and 6 are shown. One can observe a signicant difference
between the behaviours in terms of displacements measured.
Whereas the displacement throughout the central axis is signicantly lower than the one on the outer borders for Test No. 4, the
opposite occurs for the reference Test No. 6. A reason for this discrepancy lies in the inhomogeneous heating process over the strip
width. During curing with the heating elements, a lower temperature develops at the strip edges leading to a lower stiffness and
strength compared to the central part of the strips. Therefore, higher displacements can develop at the strip edges. The reference Test
No. 6 shows the typical behaviour given in the literature, e.g., [23],
whereby the centre part of the strip exhibits higher displacements
than the edge parts of the strip.
In addition to the direct measurement of the ultimate load leading to the failure of the FRP-to-concrete joint, the pull-off bond
tests are analysed in the next section with the aim of deriving
the bond shear stressslip interface law of the FRP-to-concrete
interface and their evolution depending on the heating duration.
Fig. 10. Pull-off bond tests at different curing temperatures: observed failure
modes at the concrete-FRP interface.
6. Analytical calculations
6.1. Axial tensile tests
The experimental observations derived by the axial tensile tests
show that the strength fa is negligible in the rst stages of the curing phase. The chemical reactions resulting in the hardening of the
resin and the development of its mechanical properties actually
begin after a certain time span, referred to here as the activation
time ta. After this time, the mechanical properties (i.e., the axial
strength f(t)) develop quickly, with rates depending on the curing
temperature, up to a maximum asymptotic value (the end
strength) which is almost independent of the curing conditions.
The following trilinear relationship was considered, as it clearly
represents the key features of the observed behaviour in terms of
activation time (ta = n/m), reaction rate (m) and asymptotic
strength value fa (end strength):
f t m t n with 0 6 f t 6 fa :
406
Fig. 11. ICS image of displacement in x-direction (pulling direction) of the FRP strip and the concrete surface.
m
(MPa/h)
n
(MPa)
ta = n/m
(h)
tr
(h)
ttot
(h)
tn
()
fa
(MPa)
10
22
25
45
65
90
1.12
2
2.32
9.37
13.06
18.99
12.72
11
10.57
14.13
8.03
5.36
11.37
5.49
4.56
1.51
0.61
0.28
13.53
9.77
8.11
2.00
1.34
0.88
24.90
15.26
12.67
3.51
1.95
1.16
1.63
1.00
0.83
0.23
0.13
0.08
15.15
19.57
18.82
18.8
17.68
16.79
"
n
T arg min
m;
m;n
#
sT
X
f ti ; m; n fa;i 2 ;
i1
where ti is the duration of curing and fa,i the observed axial strength
of the ith specimen cured at temperature T (out of the total sT cured
at the same temperature).
The results of the calibrations in terms of m, n, and other related
parameters, are reported in Fig. 12 for the six relevant temperatures T considered in the curing process of the test specimens.
The diagrams are sorted in Fig. 12 from lower to higher curing temperatures and the effect of the heating process on the time evolution of the axial strength fa is clearly visible. For instance, the
activation time, which is about 6 h in the case of room temperature
(T = 22 C), is sharply reduced to less than half an hour in the case
of the higher oven temperature (T = 90 C). Fig. 13 shows the exponential reduction of the activation time ta as a function of the curing temperature T; the corresponding exponential interpolation is
407
25
25
20
20
Strength [MPa]
Strength [MPa]
15
10
Nominal Temperature
~10 oC
Test results
Tri-Linear Model
15
Room Temperature
22 oC
10
5
Test results
Tri-Linear Model
0
0
10
20
30
40
50
10
25
25
20
20
15
Room Temperature
25 oC
10
5
Test results
Tri-Linear Model
30
40
50
15
10
Test results
Tri-Linear Model
10
20
30
40
50
25
25
20
20
Strength [MPa]
Strength [MPa]
20
Strength [MPa]
Strength [MPa]
15
10
Test results
15
10
Test results
Tri-Linear Model
Tri-Linear Model
0
0
Fig. 12. Axial tensile strength evolution and calibration of the tri-linear law for the specimens cured in an oven at different temperatures.
100.0
100.0
tstart = 20.828e-0.0574 T
m = 0.0332 T1.4143
R2 = 0.9545
R2 = 0.9843
ta [h]
m [MPa/h]
10.0
1.0
10
20
30
40
50
60
70
80
90
10.0
1.0
1
100
10
100
0.1
0.1
T [oC]
Fig. 13. Axial tensile tests: calibrated relationship between curing temperature and
activation time.
T [oC]
Fig. 14. Axial tensile tests: calibrated relationship between curing temperature and
reaction rate.
408
Fig. 15. Calibrated relationship for strength development depending on heating duration at different curing temperatures (the activation time and reaction duration as
indicated in the graph are only valid for T = 60 C).
Fig. 16. Normalized duration for complete curing (activation time plus reaction
duration) dependent on the curing temperature: experimental measurements in
comparison with the rule rule of thumb according to Mays and Hutchinson [8].
409
0.3
Experimental
results
0.2
Calibrated
model
62.0 kN
62.0 kN
40.5 kN
40.5 kN
20.1 kN
20.1 kN
Czaderski et al. [20] or Faella et al. [22]; it can be written symbolically as follows:
Pulling direction
Strip
Test no.5
Concrete
0.1
load increase
0.0
0
50
100
150
200
250
300
x [mm]
indicating that the value of the interface slip s at a point on the abscissa x throughout the bonded length L depends on both the postelastic branch of the bi-linear law represented in Fig. 17 (namely, on
the maximum shear strength smax and the ultimate slip su) and the
point on the abscissa xel throughout the adhesive interface at which
s(xel) = sel.
The resulting external force F can be evaluated through another
relationship whose expression is reported below as a function of
the same variables:
F Fsmax ; su ; xel :
0.3
Test no.6
Experimental Calibrated
model
results
0.2
57.6 kN
57.6 kN
40.1 kN
40.1 kN
20.1 kN
20.1 kN
load increase
0.0
0
50
100
150
200
250
300
x [mm]
Fig. 18. Measured relative displacements for different loading steps in x-direction
(longitudinal to the strip direction) between the strip and the concrete surface
referred to as interface slip and simulated slips after the calibration procedure.
(
nm
X
sxi ; smax ; su ; xel si;exp 2
s2u
smax ;xel
ii
9
"
#2
Fsmax ; su ; xel F 3 =
:
;
F 3
F
cosh xx
;
xEf bf tf sinh xL
s
kel
x
:
Ef t f
Considering the rst load level F(1) and assuming that the behav (and the
iour under this load remains elastic, the optimal value of x
corresponding value of the elastic stiffness kel) can be derived by
solving the following least-squares minimization problem:
(
)
nm
X
arg min
x
sxi ; x; F i si;exp 2 ;
ii
where nm is the number of displacement measurements si,exp available at the same load stage.
6.2.2. Post-elastic stage
The post-elastic response of an adhesive joint can be modelled
by a more complicated analytical relationship, where the dependent variables are smax and smax = su. The explicit analytical expression of that relationship is omitted here, but can be found in
sx; x; F
0.1
fully cured
Test. no.1
Test. no.3
Test. no.4
Test. no.5
25 mins
Test. no.6
3
2
20 mins
1
15 mins
0
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
410
for Test No. 5) does not affect the nal behaviour of the resin (as
obtained in Test No. 6, the reference test).
7. Conclusions
The presented experimental and analytical results lead to several conclusions. As expected, the axial tensile tests revealed a considerable inuence of the curing temperature on strength evolution
of the epoxy adhesive. The necessary curing duration for completely developing the end strength of the adhesive, composed of
the reaction duration and the activation time, was signicantly reduced at higher curing temperatures. On the basis of the axial tensile tests, a complete chart representing the evolution of the
normalized tensile strength f(t)/fa as a function of time t at different
curing temperatures T was presented (Fig. 15). The tests demonstrated that to develop almost the same end strength, curing durations ranging from approximately 1 day at 10 C to a slightly more
than one hour at 90 C were required. Moreover, the values of curing duration obtained at the various temperatures were found to be
in good agreement with a rule of thumb estimate available in the
scientic literature (see Section 2.1). No signicant variation in end
strength was found at higher curing temperatures. However, further experiments are needed in order to conrm this observation.
The investigations on the FRP-to-concrete interface at 90 C curing temperature showed that 1520 min of curing resulted in an
adhesive failure, which means that the strength of the adhesive
layer had not completely developed for that duration and temperature. On the other hand, the specimen cured for 25 min at 90 C
exhibited the same failure mode observed in the pull-off test on
the reference specimen, which was cured for 3 days at room temperature. The experimental results in terms of the distribution of
interface slip throughout the bond length at different load levels
were used to identify the shear stressinterface slip relationships
for the various specimens cured at 15, 20 and 25 min and for the
reference one cured in the usual way. Besides the above mentioned
adhesive failure at the shortest two curing durations, curing for
25 min induced a lower elastic stiffness, a lower maximum bond
strength and a larger total slip displacement as compared to the
fully cured specimens. The displacement measured over the strip
width by optical image correlation revealed the need for optimising the performance of the heating elements in order to obtain a
more homogeneous heat transfer and temperature within the
adhesive layer.
Finally, the quantitative results obtained in the present study
are of key importance for enhancing the practical implementation
of the gradient anchorage method for prestressed FRP strips in RC
beams (Czaderski and Motavalli [1], Aram et al. [2]). Dening the
optimal anchorage length, the number of steps and the heating
temperature and duration to be used for implementing the above
mentioned procedure are among the next objectives of this
research.
Acknowledgements
The nancial support of the Swiss innovation promotion agency
(CTI) of Switzerland is acknowledged (Project Number KTI Nr.