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Effect of curing conditions on strength development in an epoxy resin
for structural strengthening
Christoph Czaderski ⇑, Enzo Martinelli 1, Julien Michels, Masoud Motavalli
Empa, Structural Engineering Research Laboratory, Überlandstrasse 129, 8600 Dübendorf, Switzerland
a r t i c l e i n f o
Article history:Received 24 February 2011Received 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 (fibre reinforced polymer)
a b s t r a c t
Civil structures such as bridges and buildings can be strengthened with prestressed fibre reinforced poly-mer (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 dif-
ferent 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 cur-
ing time to reach the maximum tensile strength can be significantly 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 graph-
ically 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 opticalimage 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 stress–slip interface relationships for the different test specimens were identified 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 in-
stance, active reinforcement of existing members through pre-stressing techniques can significantly enhance both stiffness and
strength of those members, with a more rational and efficient
exploitation of the mechanical properties of the reinforcing mate-
rials. Using fibre reinforced polymers (FRPs) for external prestress-
ing of existing reinforced concrete (RC) members is one of the most
innovative active techniques for structural strengthening.
The main advantages derived by employing FRP in structural
strengthening are their low density, ease in mounting and superior
durability. However, similar to the case of external prestressing
with steel cables, FRP prestressed reinforcement needs a suffi-
ciently strong anchorage in order to guarantee a correct force
transfer. Besides the conventional mechanical anchorages, which,
for example, use steel plates doweled against the concrete surface,a fully adhesive anchorage system may be considered to be a more
durable solution, as no permanent steel plates and dowels are
required.
The so-called ‘‘gradient anchorage method’’ [1–3] is a possible
technical solution for avoiding mechanical fasteners and connec-
tors in RC members externally prestressed by FRP strips. This
method reduces the prestressing force at the strip ends to zero over
a certain length while the FRP strips are placed by using a special
stressing and heating device. Currently, such a device consisting
of heating elements is being developed in collaboration with an
industry partner for practical applications. In order to achieve an
efficient application of the gradient anchorage method, detailed
1359-8368/$ - see front matter 2011 Elsevier Ltd. All rights reserved.doi:10.1016/j.compositesb.2011.07.006
⇑ Corresponding author. Tel.: +41 58 765 55 11 11; fax: +41 58 765 44 55.
E-mail address: [email protected] (C. Czaderski).1 Permanent address: University of Salerno, Dept. of Civil Engineering, via Ponte
don Melillo, 84084 Fisciano, Italy.
Composites: Part B 43 (2012) 398–410
Contents lists available at ScienceDirect
Composites: Part B
j o u r n a l h o m e p a g e : w w w . e l s e v i e r . c o m / l o c a t e / c o m p o s i t e s b
http://dx.doi.org/10.1016/j.compositesb.2011.07.006mailto:[email protected]://dx.doi.org/10.1016/j.compositesb.2011.07.006http://www.sciencedirect.com/science/journal/13598368http://www.elsevier.com/locate/compositesbhttp://www.elsevier.com/locate/compositesbhttp://www.sciencedirect.com/science/journal/13598368http://dx.doi.org/10.1016/j.compositesb.2011.07.006mailto:[email protected]://dx.doi.org/10.1016/j.compositesb.2011.07.006
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information on how to prepare, place and cure the adhesive is
essential. Although plenty of experimental and theoretical
studies have been carried out on the structural behaviour of
FRP-strengthened RC structures (see, for instance, Meier [4] and
Teng et al. [5]), the effect of the curing conditions on the develop-
ment of the mechanical properties of epoxy resins generally uti-
lised for structural strengthening is one of the less investigated
issues. In this context, quantifying the effect of curing temperature
and duration on the strength development of epoxy resins could
significantly improve the preparation and installation procedures
for the gradient anchorage or similar applications.
It must be pointed out that the present investigation studied the
effect of curing temperature and duration on the stiffness andstrength evolution of adhesives. As such, it did not consider the ef-
fect of test temperature on the properties of fully cured adhesives,
a subject investigated for example in Klamer et al. [6].
In the first part of this paper, a State-of-the-art section pre-
sents information available in the literature related to the
strength development of epoxy adhesives. Following this, the re-
sults of two different types of experimental tests are presented.
On one hand, a series of direct tensile tests were performed on
samples of epoxy resin cured under different conditions with
the objective of describing the evolution of the adhesive strength.
On the other hand, six pull-off bond tests were carried out on FRP
strips glued on concrete blocks and cured in different conditions
for investigating how the interface relationship between shear
stresses and interface slip is influenced by the curing conditionsin terms of temperature and duration (see also [7]). Full-field
3D-displacements of the test specimens were measured using
an optical image correlation measurement system. Finally, differ-
ent analytical models are developed and applied for deriving the
quantitative information related to the development of the rele-
vant mechanical properties of both the adhesive and the FRP-
to-concrete interface.
2. State-of-the-art on strength development of epoxy adhesives
In general, adhesives can be classified according to either their
origin, method of bonding, end use or chemical composition. De-
tailed information about their possible classification can be foundin Mays and Hutchinson [8]. The present work focuses on the
strength development of epoxy adhesives, which are the most
commonly used for applications in structural strengthening.
2.1. Curing temperature and duration effects on strength development
The current section gives an overview of previous investigations
on the effect of curing temperature and duration on the strength
development of epoxy adhesives as reported in the scientific liter-
ature. A summary of significant contributions is outlinedin Table 1.
Kwan et al. [9] investigated several methods for rapid curing of
structural adhesives. They carried out an experimental campaign
on two kinds of structural adhesives (namely, urethane- and
epoxy-based), considering both ultrasonic and electromagnetic(radio frequency and microwave) heating techniques. The study
was aimed at demonstrating the feasibility of heating procedures
for adhesive curing other than the traditional ones based on ther-
mal heating. Different behaviours were observed for the two types
of adhesives. In particular, all the rapid curing techniques were
successful for the urethane-based adhesive with a fast enhance-
ment of the joint strength observed within a few seconds, when
tested as a single lap shear joint according to ASTM D3163-96
[10]. On the other hand, the epoxy-based resin behaved worse,
resulting in arcing and smoking while heating.
Several researchers have investigated the effect of elevated cur-
ing temperatures on the strength development of structural
adhesives.
Lapique and Redford [11] studied the evolution of some rele-vant mechanical parameters (i.e., viscosity, strength and stiffness)
of a commercial epoxy-adhesive during the curing period. They
investigated the effect of the curing temperature and quantified
the time evolution of both the strength and the elastic modulus
at room temperature. It was demonstrated that when cured at
room temperature, the strength as well as the elastic modulus in-
creased with time. Furthermore, a faster strength evolution was
observed at higher temperatures, as the same mechanical proper-
ties obtained at 23 C after 28 days could be attained at 64 C after
only 4 h.
Dodiuk and Kenig [12] observed increasing flexural strength
and flexural modulus of fibreglass epoxy composites with higher
curing temperatures. For instance, the strength achieved after 1 h
curing at 60 C was higher than that obtained after 10–20 days of curing at room temperature.
Nomenclature
F maximum tensile force during the axial tensile testsF u maximum force at failure or at initiation of debonding
during the pull-off bond test f (t ) time dependent axial tensile stress of the axial tensile
tests f a axial tensile strength of the axial tensile testst a activation time (time which is necessary to start the
curing reaction, see Fig. 15)t r reaction duration (time which is necessary to reach the
end strength, see Fig. 15)m reaction rate (see Fig. 15)n virtual intersection of the ascending branch with the y-
axist curing durationt tot full curing duration, i.e., activation time plus reaction
duration (t a + t r )t n normalized duration for fully curing in reference to
room temperature testing at 22 C
t h heating durationt c cooling durationT curing temperatureT avg mean temperature during pull-off tests
max maximum shear strength (see Fig. 17)s FRP-to-concrete interface slipsel slip at end of elastic branch (see Fig. 17)smax slip at debonding (see Fig. 17)su ultimate slipsT the total number of specimens cured at temperature T E f strip elastic modulust f strip thicknessb f strip widthL bond lengthkel elastic stiffness (see Fig. 17)nm number of displacement measurements x abscissa of the coordinate axis system xel point on the abscissa at which s( xel) = sel
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Similar observations have been made by Matsui [13], who stud-
ied the effects of curing conditions on the development of both
shear strength and stiffness for two kinds of adhesive (namely,
epoxy–polyamideamine and cyanoacrylate, only the first one beingused 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 filler) 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 rang-
ing from 34 to 49 C with different curing durations. Similar con-
clusions as those made by the previous researchers regarding
strength evolution were drawn.Although all experimental observations pointed out the huge
influence of the curing conditions on the development of the rele-
vant 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 resinsat curing time t and the corresponding curing temperature. Onlythe 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 final strength of the
resin is halved for every increase of 10 C in temperature.
2.2. Influence of curing temperature on the end strength of adhesives
In addition to studying the development of the relevantmechanical properties of adhesives, various researchers have ana-
lysed the end strength of resins and its possible relationship with
the curing temperature. For instance, Dutta and Mosallam [16] ob-
served higher end torque strengths for higher curing temperatures.
Cao and Cameron [17] confirmed this observation by investigat-
ing an additional effect. Instead of using isothermal curing, consist-
ing 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 flexural strength
and stiffness of specimens cured at 60 C and 120 C in comparisonto epoxies cured at room temperature.
Moreover, Tu and Kruger [14] obtained higher bond strengths at
20 C than at 10 C for the same curing duration. With further heat-
ing up to 40 C, however, no further enhancement in strength was
obtained. Islam et al. [18], by means of tensile tests, obtained opti-mal values for both tensile strength and elastic modulus at a curing
temperature of 70 C, while both decreased again approaching
120 C.
To summarize, one can say that the adhesive stiffness and
strength development is highly dependent on the curing tempera-
ture and curing duration. In general, stiffness and strength devel-
opment occurs faster with higher curing temperatures.
Furthermore, some indications of higher end strength with increas-
ing curing temperature can be found in the literature. The main
goal of the current research was to investigate and quantify the
influence of curing temperature and duration on strength develop-
ment for the particular epoxy adhesive used in this investigation.
For other adhesive types with different chemical compositions, as
seen in the literature, a different behaviour might be observed.
3. Materials
All experimental tests were performed with a commercially
available epoxy based adhesive called S&P resin 220. Its measured
glass transition temperature T g was 52 C and 58 C at room and90 C curing temperatures, respectively. According to the declara-
tion of the manufacturer, the tensile bond strength on steel is lar-
ger than 14 MPa.
The FRP strip had a thickness of 1.2 mm and a width of 100 mm
with the mechanical properties listed in Table 2. The elastic mod-
ulus was determined in a loading test for each strip before the
bond tests, which are also reported in Table 2. The measured mod-
ulus of 174 GPa was almost exactly that specified by the
manufacturer.
Aggregate with particle sizes ranging from 0 to 32 mm was em-
ployed for the concrete of the blocks used for the pull-off tests, to
which the FRP strips were glued. At 28 days, a cube compressive
strength f c ,cube of 51.5 MPa was measured, whereas the splittingtensile strength f ct was found to be 3.25 MPa.
4. Experiments
Two different types of tests were carried out with the aim of
investigating both the evolution and the final values of the key
mechanical properties of the adhesives for different curing condi-
tions in terms of both temperature and duration. A commercialepoxy adhesive which can be employed for the ‘‘gradient
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
Curing
duration
Kwan et al. [9] Urethane- and epoxy-based Lap shear test Ultrasonic, radio frequency and
microwave heating
Lapique and Redford
[11]
Araldite Uniaxial tension and 3-point bending test 23–64 C 1–28 days
Dodiuk and Kenig[12]
High-temperature epoxies Bending and lap shear tests RT, 60, 120 C 60 min to20 days
Matsui [13] Epoxy (Araldite)/instant glue
(cyanoacrylate)
Lap shear test 18–150 C 3.3–50 h
Tu and Kruger [14] Unfilled and silica filled epoxies Slant shear test 10–40 C 1–14 days
Dutta and Mosallam
[16]
Four different epoxies Torque tests with circular FRP laminates bonded on concrete 34 to 49 C 24–72 h
Islam et al. [18] Hemp fibre/epoxy composite/neat
epoxy
Fiber pull-out with interfacial shear strength measurements and
uniaxial tension
25–120 C 0.08–13.8 h
Cao and Cameron
[17]
Glass fiber reinforced epoxy Bending and shear tests RT to 150 C 5 h s tep curing
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anchorage method’’ in RC beams externally prestressed by FRP
strips was used for all tests. The experimental campaign can be
subdivided into the two following groups of tests:
– axial tensile tests on adhesive samples, to measure the develop-
ment of the adhesive axial tensile strength at different curing
temperatures;
– pull-off bond tests on FRP-to-concrete joints, aimed at describ-
ing the evolution of the interface behaviour under variable cur-
ing conditions.
The former tests were carried out for curing temperatures rang-
ing between approximately 10 and 90 C, while the latter ones
were performed at a constant mean curing temperature of approx-
imately 90 C and variable curing durations. It should be noted that
the tests were performed approximately 5–10 min after stopping
the heat transfer, which means that the temperature of the test
specimens at testing was still significantly higher than room tem-
perature (Sections 4.1 and 4.2) and therefore could influence the
test results. However, this corresponds approximately to the real
situation at the time when the prestressing force is released during
application of the gradient method.
4.1. Axial tensile tests
A large number of axial tensile tests were performed on speci-
mens as those represented in Fig. 1. The uncured resin was applied
between an aluminium cylinder with a diameter of 20 mm and a
square aluminium plate with dimensions of 60 60 mm. These
test specimens were cured at different temperatures in an oven
and tested with the pull-off tester shown in Fig. 2. The tests were
aimed at measuring the tensile strength of the resin dependingon both curing temperature and duration. It is clear that, due to
the short length of the adhesive sample, this test specimen does
not deliver the real tensile strength. Nevertheless, the actual trend
in the evolution of the tensile strength of the resin can be captured
in these tests, whose specimens are particularly convenient and
can be easily and rather uniformly heated inside a simple oven.
The evolution of the temperature of the air in the oven as well as
the temperature inside the resin layer were monitored in some
of the specimens which underwent an accelerated curing process
by heat transfer (Figs. 3 and 4).
Table 2
Mechanical properties of the FRP strips – comparison between experimental investigation and product certificate.
Test No. Experimental investigation According to S&P certificate
Modulus of elasticity E f (GPa)
Modulus of elasticity E f (GPa)
Tensile strength f u(MPa)
Elongation at 2000 MPa e2000(%)
Width b f (mm)
Thickness t f (mm)
1 169 173.9 2975 1.142 100 1.23
2 173
3 179
4 174
5 171
6 177
Mean
value
174
Fig. 1. Specimens for axial tensile tests, on the left side (Nos. 10 and 11) the
aluminium stamps and plates withapplied adhesive in between can be seen, on theright side (No. 12) the stamp including the fixture for the curing process is visible.
Fig. 2. Set-up for axial tensile tests.
Fig. 3. Axial tensile test specimens inside the oven and cables for temperaturemeasurements.
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A complete overview of the tested resin specimens is reported
in Table 3. The number of specimens cured at room temperature
as well as those which underwent an accelerated curing process
at different temperatures is also shown in the table. For the tem-
perature curing, two different ovens were used. In particular, a to-
tal of 200 tests were carried out in several sessions with variable
curing conditions: 136 tests were carried out on specimens with
accelerated curing in an oven with temperatures ranging between
45 and 90 C, and 64 tests were carried out on specimens cured at
different room temperatures, with curing durations ranging from a
few hours to 7 days.
Most of the tests were performed on specimens cured at 90 C,
which is considered as the reference temperature for the present
investigation. However, this was only the ‘‘nominal temperature’’
of the air inside the oven. The temperature development in the
adhesive resin was generally slower than that in the air and the fi-
nal temperature was slightly lower than the nominal one. A typical
temperature development observed is shown in Fig. 4, emphasis-
ing the different measurements inside the adhesive and in the oven
air. Additional tests on specimens cured at 120 C were also carried
out, but the results are not reported herein as their failure was al-
ways controlled by the loss of bonding between the resin and the
aluminium plate, possibly as a result of the difference in relative
expansion of the two materials at that temperature.
Fig. 4 also shows the cooling curve for test specimens taken out
of the oven. All the axial tensile tests were carried out after a min-
imum of 5 min of cooling outside the oven at room temperature.
Therefore, from Fig. 4, it can be concluded that the resin of the
tested specimens had a maximum temperature ranging between
60 and 75 C at the time that the tests were actually performed.
4.2. Pull-off bond tests on FRP strips glued on concrete through a layer of epoxy resin
Six pull-off bond tests were carried out with the aim of measur-
ing 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 follow-
ing the main phases represented in Fig. 6. The tested specimens
were always equipped with sensors for monitoring the tempera-
ture evolution within both the adhesive layer and the heating ele-
ments. The preparation of the adhesive layer between the FRP strip
and concrete surface was followed by the heating phase (t h), car-ried out by means of heating elements. After stopping the heating
procedure, a cooling time of 5–10 min was included before starting
0
30
60
90
120
0 100 200 300
Time [mins]
T e m
p e r a t u r e [ o C ]
Room Temperature Air temp. in the oven
Sensors on the adhesive
Oven in testing hall (SH)
0
25
50
75
100
125
0 50 100 150
Time [mins]
T e m
p e r a t u r e [ ° C ]
Room Temperature Air temp. in the oven
Sensors on the adhesive
Oven room (OR)
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 Tests with heating Tests w/o heating Oven
[#] n. T (C) n. t max (h)
1 12 48 –
2 4 90 SH
3 12 90 SH
4 24 24 –
5 19 90 4 23 SH
6 7 90 SH
7 12 36 –
8 16 65 8 168 SH
9 16 45 4 168 SH
10 24 90 OR
11 24 65 OR
12 14 90 OR
Total 136 64
Fig. 5. Test setup for pull-off bond tests.
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the loading test in order to cool down the adhesive (t c ). Afterwards,one can observe the force increasing up to the maximum value F u.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 (T avg ), 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-field 3D displacements of the test specimen were mea-
sured during the experimental investigations with an optical
image correlation measurement system (ICS) [19]. A description
of the measurement system used can be found in Czaderski et al.
[20], Czaderski and Rabinovitch [21]. With the ICS, the shape of
the surface was also measured. Fig. 7 shows the isolines of the sur-
face of the strip and concrete before starting the test. It can be seen
that the surface of the strip was not planar, but was curved with a
maximum vertical value at the surface centre. This was the result
of the application process. Hence, a larger adhesive quantity can
be observed in the strip centre. Over the whole bonding area, an
average value can be obtained. The latter can subsequently be
transformed into the mean adhesive thickness by subtracting the
strip thickness. A summary of the measured adhesive thicknesses
is given in Table 4.
The heating duration range of 15–25 min was chosen based on
the results observed in the previous campaign, while the waiting
time for cooling was chosen so that the adhesive temperature
was lower than approximately 50 (Table 4). Comparing Figs. 4
and 6, a key observation is the temperature development, and con-
sequently, the rate of the heat transfer in the axial tensile tests and
pull-off bond tests. In particular, the temperature developed much
faster in the second series of tests as a result of greater heat trans-
fer by using heating elements in contact with the CFRP strips com-
pared to heating the air in the oven.
5. Results
The large number of axial tensile tests produced plenty of
experimental results useful for understanding the development
of the axial strength of the epoxy-resin used in this study at differ-
ent curing temperatures. The strength was simply obtained by
dividing the failure load by the nominal cross-sectional area of
the adhesive layer.
On the other hand, analysing the pull-off bond tests performed
on the FRP-to-concrete adhesive joints was much more demanding
because the properties of the adhesive interface could not be
Fig. 6. Adhesive temperature (T 1, T 2, T 3) and force development of Test No. 3 (pull-off bond tests), t h: heating duration, t c : cooling duration, T avg : mean temperatureduring pull-off test, F u: ultimate force, L = bond length, T 1, T 2, T 3 = temperatures inthe 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
surface-
upper
strip
surface
(mm)
Strip
thickness
(mm)
Mean
adhesive
thickness
(mm)
Heating
duration
t h (min)
Waiting
time to
failure
test t c (min)
Average test
temperature
T avg (C)
1 4.85 1.2 3.65 15 5.7 45
2 5.14 1.2 3.94 25 8.6 43
3 5.00 1.2 3.80 20 5.8 41
4 4.90 1.2 3.70 25 7.7 42
5 4.74 1.2 3.54 25 2 days 19
6 4.93 1.2 3.73 – 3 days 18
Fig. 7. Isolines of the surface of the CFRP strip before the start of the pull-off test determined by using the ICS.
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, f a = axial
tensile strength).
Series n T (C) t (h) F (kN) f a (MPa)
1 12 24–26 4.0–48.0 0.08–6.15 0.25–19.6
4 24 22 4.0–24.0 0.03–6.18 0.1–19.7
5 4 24 7.0–22.9 1.49–6.13 4.7–19.5
7 12 10 6.3–36.0 0.03–5.06 0.1–16.18a 4 10 48–168 4.40–4.95 14.0–15.8
8b 4 22 48–168 5.76–6.44 18.3–20.5
9 4 22 48–168 5.84–6.41 18.6–20.4
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directly measuredby those tests, but had to be derived by means of
an indirect identification procedure [20,22].
This section presents the ‘‘raw results’’ obtained by the experi-
mental tests; only a few phenomenological observations are re-
ported. An analytical model for deriving the key parameters of
the corresponding interface bond law is discussed in Section 6.
5.1. Axial tensile tests
The results of the axial tensile tests carried out on the adhesive
specimens cured at room temperature are reported in Table 5. The
table reports both the minimum and maximum nominal curing
temperatures and the duration (in hours) of each series. Further-
more, the minimum and maximum axial forces at failure F andthe corresponding mean axial strengths f a are given for each series.Here, axial strengths were evaluated under the assumption of a
uniform distribution of axial stresses on the circular transverse
section of the adhesive layer. As discussed before, this mean axial
strength is not the correct tensile strength because of the short
length of the test specimen. However, it allows the strength devel-
opment at different curing temperatures to be studied. The results
for the specimens cured at higher temperatures are reported in
Table 6 following the same procedures explained above.
Several observations may be made on the basis of these exper-
imental results. Firstly, the maximum values of the axial strength f aobtained from the specimens cured either at room temperature or
within the oven are quite close to one another, being in both cases
about 18–20 MPa. However, a closer comparison between the dif-
ferent curing conditions reveals slightly lower end strength
reached at 10 C. This temperature resulted in an end strength of
16 MPa, whereas higher temperatures led to higher resistances of
about 18–22 MPa. This is in accordance with the findings of the
researchers mentioned above, especially Tu and Kruger [14], who
found a very similar bond strength enhancement from about 15
to 18.5 MPa in the same curing temperature range of 10–20 C.
However, in order to verify this finding, further detailed experi-
mental investigation is needed. In general, the presented strength
range corresponds to the declaration of the distributor of the mate-
rial, as previously described in Section 3.
On the other hand, the key difference between the various cur-
ing temperatures lies in the time span necessary for reaching the
end strength. For the case of specimens cured at room temperature
it is in the order of 12 h to a few days, whereas it drops to a few
hours in the case of specimens cured in the oven at higher temper-
atures (45–90), see Fig. 12. Consequently, the effect of heat trans-
fer on the curing process of resins is quantitatively relevant andthe
relationships between the curing temperature and the develop-
ment of strength in the resin should be approximated with expo-
nential or linear functions, as reported in detail in Section 6.
In all the tests, failure developed throughout the adhesive layer
with no significant loss of adhesion observed at the aluminium-to-
resin interface. Consequently, the strength values strictly refer to
the adhesive and are not significantly affected by the testing sys-
tem. Fig. 8 illustrates two relevant failure modes of the resin layer,
the first observed either at low curing temperature or short curing
duration (Fig. 8a), and the second observed after the activation of
the chemical reactions resulted in the hardening of resin ( Fig. 8b).
5.2. Pull-off bond tests
The results of the pull-off bond tests carried out on the six FRP-
to-concrete specimens are given in Table 7 as a function of the
heating duration and waiting time before the test started. Fig. 9
shows the maximum measured force or the force at initiation of
debonding as a function of the curing duration. The characteristic
‘‘initiation of debonding’’ stage was defined as the decisive stage
to determine the bond shear stress–slip relationship, although
the force can slightly increase afterwards. A discussion related to
that topic can be found in Czaderski et al. [20]. The result of Test
No. 6, carried out on a specimen cured at room temperature for
3 days, is considered as a reference. As indicated in Fig. 9 and Table
7, the absolute strength and displacement values of Test No. 2 have
to be excluded from a detailed analysis, as problems occurred with
the test setup (complete concrete block displacement occurred in-
stead of a relative movement between the concrete and FRP strip).
It can be observed that the specimens cured at an elevated temper-
ature for 15 or 20 min exhibit significantly lower strengths. More-
over, all the specimens cured for 25 min (tested either a few
minutes after the heating procedure or after 2 days) failed at forces
higher than that observed for the reference specimen cured at
room temperature.
The failure modes observed in the various tests confirm the
above quantitative observations. Fig. 10 shows the interfaces of
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, f a = axial tensile
strength).
Series n T (C) t (h) F (kN) f a (MPa)
2 4 90 1.0–1.3 2.87–3.88 9.1–12.35
3 12 88–90 0.8–4.0 1.36–5.66 4.3–18.0
5 19 88–89 0.7–3.7 1.28–7.14 4.1–22.7
6 7 90 0.4–0.6 0.23–2.03 0.7–6.58 16 65 0.7–2.7 0.05–6.41 0.16–20.4
9 16 45 0.7–4.0 0.0–6.10 0.0–19.4
10 24 90 0.25–2.5 0.0–7.2 0.0–22.9
11 24 65 0.52–2.5 0.31–5.94 1.0–18.9
12 14 90 0.3–0.7 0–3.4 0–10.8
Fig. 8. Axial tensile tests: typical failure modes.
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the test specimens after failure. For test specimen No. 1, the resinwas 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 con-
crete failure area is visible. On the contrary, the other specimens
failed with a fracture developing throughout the concrete sub-
strate (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 specimensNos. 4 and 6 are shown. One can observe a significant difference
between the behaviours in terms of displacements measured.
Whereas the displacement throughout the central axis is signifi-cantly 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 dis-
crepancy lies in the inhomogeneous heating process over the strip
width. During curing with the heating elements, a lower tempera-
ture develops at the strip edges leading to a lower stiffness and
strength compared to the central part of the strips. Therefore, high-
er 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 lead-
ing 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 stress–slip interface law of the FRP-to-concreteinterface and their evolution depending on the heating duration.
6. Analytical calculations
6.1. Axial tensile tests
The experimental observations derived by the axial tensile tests
show that the strength f a is negligible in the first stages of the cur-ing 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’’ t a. After this time, the mechanical properties (i.e., the axialstrength f (t )) develop quickly, with rates depending on the curingtemperature, 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 (t a = n/m), reaction rate (m) and asymptoticstrength value f a (end strength):
f ðt Þ ¼ m t þ n with 0 6 f ðt Þ 6 f a: ð1Þ
Table 7
Results of the pull-off bond tests (F u = 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)
F u(kN)
smax
(MPa)
sel(mm)
smax(mm)
Failure
mode
1 15 18.4 0.8 0.602 0.652 Adhesive
2a 25 60.4 5.1 0.205 0.408 Concrete
3 20 34.4 1.4 0.803 0.803 Mainlyadhesive
4 25 75.7 4.4 0.426 0.712 Concrete
5 25 + wt 62.0 7.7 0.020 0.248 Concrete6 wt 57.6 7.9 0.031 0.218 Concrete
a F u is not the force at failure, due to problems with the test set-up.
0
20
40
60
80
15 20 25 25* 25 + 2 days
waiting time
no heating +
3 dayswaiting time
Curing duration [min]
M a x i m u m
f o r c e F u
[ k N ]
T e s t N o . 1
T e s t N o . 3
T e s t N o . 4
T e s t N o . 2
*
T e s t N o . 5
T e s t N o . 6
Fig. 9. Maximum force at failure or at initiation of debonding according to the
applied curing duration and waiting time before testing (⁄F u of Test No. 2 is not theforce at failure, due to problems with the test set-up).
Fig. 10. Pull-off bond tests at different curing temperatures: observed failure
modes at the concrete-FRP interface.
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A least-squares calibration of Eq. (1) was performed for every set of
sT experimental results reported in Tables 5 and 6 and derived at thevarious temperatures T reported in Table 8:
ð m; nÞT
¼ argminðm;nÞ
XsT
i¼1
ð f ðt i;m;nÞ f a;iÞ2" #; ð2Þ
where t i is the duration of curing and f a,i the observed axial strengthof the ith specimen cured at temperature T (out of the total sT curedat the same temperature).
The results of the calibrations in terms of m, n, and other relatedparameters, are reported in Fig. 12 for the six relevant tempera-
tures T considered in the curing process of the test specimens.The diagrams are sorted in Fig. 12 from lower to higher curing tem-
peratures and the effect of the heating process on the time evolu-
tion of the axial strength f a is clearly visible. For instance, theactivation time, which is about 6 h in the case of roomtemperature
(T = 22 C), is sharply reduced to less than half an hour in the caseof the higher oven temperature (T = 90 C). Fig. 13 shows the expo-
nential reduction of the activation time t a as a function of the cur-ing temperature T ; the corresponding exponential interpolation is
Fig. 11. ICS image of displacement in x-direction (pulling direction) of the FRP strip and the concrete surface.
Table 8
Results of the calibration of the tri-linear model for the different temperatures
(T = curing temperature, m = reaction rate, n = virtual intersection of the ascending
branch with the y-axis, t a = activation time, t r = reaction duration, t tot = full curing
duration, t n = normalized duration for full curing relative to room temperature testing
at 22 C, f a = axial tensile strength).
T (C) m(MPa/h)
n(MPa)
t a = n/m(h)
t r (h)
t tot (h)
t n(–)
f a(MPa)
10 1.12 12.72 11.37 13.53 24.90 1.63 15.15
22 2 11 5.49 9.77 15.26 1.00 19.57
25 2.32 10.57 4.56 8.11 12.67 0.83 18.82
45 9.37 14.13 1.51 2.00 3.51 0.23 18.8
65 13.06 8.03 0.61 1.34 1.95 0.13 17.68
90 18.99 5.36 0.28 0.88 1.16 0.08 16.79
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0
5
10
15
20
25
0 10 20 30 40 50 0 10 20 30 40 50
0 10 20 30 40 50
Curing Duration [h]
S t r e n g t h [ M P a ]
Test results
Tri-Linear Model
Nominal Temperature
~10o
C
0
5
10
15
20
25
Curing Duration [h]
S t r e n g t h [ M P a ]
Test results
Tri-Linear Model
Room Temperature
22o
C
0
5
10
15
20
25
Curing Duration [h]
S t r e n
g t h [ M P a ]
Test results
Tri-Linear Model
Room Temperature25
oC
0
5
10
15
20
25
0 1 2 3 4 5
Curing duration [h]
S t r e n
g t h [ M P a ]
Test results
Tri-Linear Model
Nominal Oven Temp.T=45ºC
0
5
10
15
20
25
0 1 2 3 4 5
Curing duration [h]
S t r e n g t h [ M P a ]
Test results
Tri-Linear Model
Nominal Oven Temp.
T=65ºC
0
5
10
15
20
25
0 1 2 3 4 5
Curing duration [h]
S t r e n g t h [ M P a ]
Test results
Tri-Linear Model
Nominal Oven Temp.
T=90ºC
Fig. 12. Axial tensile strength evolution and calibration of the tri-linear law for the specimens cured in an oven at different temperatures.
tstart = 20.828e-0.0574 T
R2 = 0.9843
0.1
1.0
10.0
100.0
0 10 20 30 40 50 60 70 80 90 100
T [oC]
t a [ h ]
Fig. 13. Axial tensile tests: calibrated relationship between curing temperature andactivation time.
m = 0.0332 T1.4143
R2 = 0.9545
0.1
1.0
10.0
100.0
100101
T [oC]
m [ M P a / h ]
Fig. 14. Axial tensile tests: calibrated relationship between curing temperature andreaction rate.
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drawn as well as its analytical expression and the corresponding
coefficient of determination R2 with respect to the experimentaldata. In addition, Fig. 14 displays the relationship between the
reaction rate m and the curing temperature T , suggesting the expo-nential interpolation shown along with the corresponding value of
the coefficient R2. In both cases, the proposed interpolations are invery good agreement with the observed data and the correspond-
ing coefficients of determination are rather close to unity.
Finally, the relationship (1) between the actual strength f (t )developed in the resin at time t and the curing temperature can
be utilised for generating a complete chart representing the evolu-tion of the ratio f (t )/ f a as a function of time t at different curingtemperatures T (see Fig. 15).
The duration necessary for developing the final asymptotic
strength can be obtained by adding the activation time to the reac-
tion duration. Fig. 16 presents the normalised duration for com-
plete curing (room temperature of 22 C is taken as the reference
value) compared to the earlier mentioned ‘rule of thumb’ by Mays
and Hutchinson [8]. A good agreement between the experimental
results and the suggested rule of thumb found in the literature
can be observed.
6.2. Pull-off bond tests
The key objective of this part of the investigation was to identifythe general bilinear bond shear stress–slip relationship repre-
sented in Fig. 17 [24] . Three mechanical parameters completely
define the relationship between the shear stresses s f and the inter-
face slip s:
– the maximum shear strength smax;
– the interface slip sel at the end of the elastic branch of the inter-face relationship;
– the interface slip smax at debonding.
Displacements were monitored during the tests by means of an
advanced optical measurement system [19]. The slip was
calculated from the difference between the displacements of the
CFRP strip (section 0 in Fig. 11) and the concrete surface (Sections5 and 6 in Fig. 11) beside the strip.
The maximum observed displacement at the last stage before
failure or initiation of debonding was taken as smax. In particular,three load stages were considered in the present study at three dif-
ferent load levels F (i) (i = 1, 2, 3) (see Fig. 18).
Fig. 15. Calibrated relationship for strength development depending on heating duration at different curing temperatures (the activation time and reaction duration asindicated 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 incomparison with the rule ‘rule of thumb’ according to Mays and Hutchinson [8].
Fig. 17. General bi-linear relationship for the FRP-to-concrete interface.
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The following equations and descriptions explain the modelling
approach for both the elastic and the post-elastic stages.
6.2.1. Elastic stage
The elastic stiffness kel =s
max/sel (Fig. 17) can be identified bymeans of a numerical calibration of the following relationship, rep-resenting the interface displacement field due to an axial force F applied at the end of a bonded joint behaving elastically through-
out its length L [22]:
sð x;x; F Þ ¼ F
xE f b f t f
coshx x
sinhxL ; ð3Þ
where E f is the Young’s modulus of the composite strip, b f and t f arethe width and thickness of its transverse section and the parameter
x is defined as follows:
x ¼
ffiffiffiffiffiffiffiffikelE f t f
s : ð4Þ
Considering the first load level F (1) andassuming that the behav-iour under this load remains elastic, the optimal value of x (and the
corresponding value of the elastic stiffness kel) can be derived bysolving the following least-squares minimization problem:
x ¼ argminx
Xnmi¼i
½sð xi;x; F ðiÞÞ si;exp
2
( ); ð5Þ
where nm is the number of displacement measurements si,exp avail-able at the same load stage.
6.2.2. Post-elastic stageThe post-elastic response of an adhesive joint can be modelled
by a more complicated analytical relationship, where the depen-
dent variables are smax and smax = su. The explicit analytical expres-sion of that relationship is omitted here, but can be found in
Czaderski et al. [20] or Faella et al. [22]; it can be written symbol-
ically as follows:
s ¼ sð x;smax; su; xelÞ; ð6Þ
indicating that the value of the interface slip s at a point on the ab-scissa x throughout the bonded length L depends on both the post-elastic branch of the bi-linear law represented in Fig. 17 (namely, on
the maximum shear strength smax and the ultimate slip su) and thepoint on the abscissa xel throughout the adhesive interface at whichs( xel) = sel.
The resulting external force F can be evaluated through anotherrelationship whose expression is reported below as a function of
the same variables:
F ¼ F ðsmax; su; xelÞ: ð7Þ
Consequently, the optimal values of the parameters smax and xelcan be derived imposing the following two conditions:
– the interface slips evaluated using Eq. (6) result in values as
close as possible to the observed values si,exp;– the external force F evaluated using Eq. (7) is as close as possible
to that applied during the experimental test.
The above conditions can be mathematically stated through the
following least-squares optimization problem with reference to
the third load stage F (3) (namely, resulting in specimen failure)[22]:
ðsmax; xelÞ ¼ argminðsmax ; xelÞ
Xnmi¼i
½sð xi; smax; su; xelÞ si;exp2
s2u
(
þ F ðsmax; su; xelÞ F
ð3Þ
F ð3Þ
" #29=;: ð8Þ
The results of the optimization procedure are reported in Table
7 in terms of the resulting values of smax, sel, and smax = su.The bilinear interface relationships corresponding to the above
calibrations are presented in Fig. 19, which demonstrates the effect
of accelerated curing on the mechanical properties of the FRP-to-
concrete interface. The relationships derived from Test Nos. 1
(15 min heating duration) and 3 (20 min) are characterized by a
very low stiffness and no decreasing branch, as the resin is not fully
cured. On the other hand, a significantly higher value of the
stiffness is observed in Test No. 4 (25 min heating duration), but
the stiffness is still clearly lower than that of the fully cured pull-
off tests. Also, the value of the strength smax in Test No. 4 is lower
than that for Test Nos. 5 and 6. Finally, the interface relationships
derived for Test Nos. 5 and 6 are rather close to one another, con-
firming the fact that the accelerated curing procedure (carried out
0.0
0.1
0.2
0.3
0 50 100 150 200 250 300
0 50 100 150 200 250 300
x [mm]
I n t e r f
a c e s l i p - s [ m m ]
62.0 kN 62.0 kN
40.5 kN 40.5 kN
20.1 kN 20.1 kN
Test no.5
Experimental
results
Calibrated
model
load increase
x
Pulling directionStrip
Concrete
0.0
0.1
0.2
0.3
x [mm]
I n t e r f a c e s l i p - s [ m m ]
57.6 kN 57.6 kN
40.1 kN 40.1 kN
20.1 kN 20.1 kN
Test no.6
Experimental
results
Calibrated
model
load increase
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.
0
1
2
3
4
5
6
7
8
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Interface slip - s [mm]
B o n d s h e a r s t r e s s - τ [
M P a ] Test. no.1
Test. no.3
Test. no.4
Test. no.5
Test. no.6
fully cured
25 mins
20 mins
15 mins
Fig. 19. Pull-off bond tests: resulting interface relationships between shear stressesand slips.
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for Test No. 5) does not affect the final behaviour of the resin (as
obtained in Test No. 6, the reference test).
7. Conclusions
The presented experimental and analytical results lead to sev-
eral conclusions. As expected, the axial tensile tests revealed a con-
siderable influence of the curing temperature on strength evolutionof the epoxy adhesive. The necessary curing duration for com-
pletely developing the end strength of the adhesive, composed of
the reaction duration and the activation time, was significantly re-
duced at higher curing temperatures. On the basis of the axial ten-
sile tests, a complete chart representing the evolution of the
normalized tensile strength f (t )/ f a as a function of time t at differentcuring temperatures T was presented (Fig. 15). The tests demon-strated that to develop almost the same end strength, curing dura-
tions ranging from approximately 1 day at 10 C to a slightly more
than one hour at 90 C were required. Moreover, the values of cur-
ing duration obtainedat the various temperatures were foundto be
in good agreement with a ‘rule of thumb’ estimate available in the
scientific literature (see Section 2.1). No significant variation in end
strength was found at higher curing temperatures. However, fur-
ther experiments are needed in order to confirm this observation.
The investigations on the FRP-to-concrete interface at 90 C cur-
ing temperature showed that 15–20 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 temper-
ature. 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 tem-
perature. 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 stress–interface 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 optimis-
ing 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]). Defining 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 financial support of the Swiss innovation promotion agency
(CTI) of Switzerland is acknowledged (Project Number KTI Nr.
10493.2 PFIW-IW). Furthermore, the financial support and delivery
of the test materials of the industrial partner of the project, S&P
Clever Reinforcement from Seewen, Switzerland, is also
appreciated.
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