Construction and Building Materials 94 (2015) 437447

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Thermal stability of PVA ber strain hardening cement-based

composites
Margareth da Silva Magalhes a,, Romildo Dias Toledo Filho b, Eduardo de Moraes Rego Fairbairn b
a
Department of Civil Construction and Transport, Universidade do Estado do Rio de Janeiro, rua So Francisco Xavier, 524, 5005-A, Rio de Janeiro, RJ CEP 20550-900, Brazil
b
Department of Civil Engineering, COPPE, Universidade Federal do Rio de Janeiro, P.O. Box 68506, Rio de Janeiro, RJ CEP 21941-972, Brazil

h i g h l i g h t s

 Inuence of pre-heating on the mechanical behavior of PVA-SHCC is studied.

 Cracking patterns under tensile and bending loads are measured after pre-heating.
 A change in SHCC mechanical behavior is observed after pre-heating up to 250 C.

a r t i c l e i n f o a b s t r a c t

Article history: This paper reports the results of an investigation on the inuence of pre-heating on the mechanical
Received 1 December 2014 behavior of PVA strain hardening cement-based composites (PVA-SHCC) by using uniaxial tensile, bend-
Received in revised form 24 April 2015 ing and compression tests. Tests were conducted on specimens that were previously heated to temper-
Accepted 12 July 2015
atures ranging from 90 C to 250 C and unheated specimens. The temperatures were selected based on
Available online 16 July 2015
the results of thermal analyses tests carried out to investigate the thermal degradation of the PVA ber.
The results indicated that specimens preheated to 90 C presented a strain hardening behavior with a
Keywords:
pronounced multiple cracking pattern. This response is nearly the same as observed for the unheated
Strain hardening cement-based composites
PVA ber
specimens. After heating to 110 C and 145 C, although the composite still presented a strain hardening
Degradation behavior the strain capacity was reduced. At 190 C the strain capacity of the SHCC is even smaller and at
Residual properties 250 C no further typical strain hardening behavior was observed; the reinforcing ber failed suddenly
after the cracking of the matrix. A similar behavior was observed for the samples submitted to bending
loads, indicating that bending test was also efcient to indicate the composite degradation under thermal
loads. Compressive strength of the composite has indicated an increase up to 190 C due to a renement
of the matrix pore structure as indicated by the microstructural studies.
2015 Elsevier Ltd. All rights reserved.

1. Introduction SHCC promise to nd a wide variety of civil engineering appli-

There is a growing interest in using Strain Hardening
Cement-based Composites (SHCC) in infrastructure systems due
to the benets derived from its higher tensile ductility when com-
pared to those of the unreinforced concrete. SHCC can resist the full
tensile load with tensile strain capacity up to 5.0%, leading to a
high energy absorption capacity. During the increase of strain
under tensile loading, a constant strain hardening effect is found
and many, closely spaced, micro cracks (generally less than
80 lm in width) are formed in the material [1,2].
Corresponding author.
E-mail addresses: margarethsm@yahoo.com.br (M.S. Magalhes), toledo@coc.
ufrj.br (R.D. Toledo Filho), eduardo@coc.ufrj.br (E.de.M.R. Fairbairn).
cations [38]. Amongst them, one of the most promising applica-
tion areas of this material lies in the repairing of concrete
structures. Due to a growing interest in SHCC, applications are dis-
covered and new structural forms are conceived. Although a large
amount of research has been carried out on this composite family
[9], the behavior of SHCC when subjected to elevated temperatures
has been scarcely studied.
Residual compression properties of ECC (a particular type of
SHCC) specimens after exposure to temperatures up to 800 C were
assessed by Sahmaran et al. [10], and in that study it was con-
cluded that the residual mechanical behavior of ECC specimens is
similar to or better than that of conventional concrete incorporat-
ing polypropylene or steel bers. Although there was a signicant
reduction in compressive strength and stiffness, no explosive spal-
ling was observed in any ECC specimens. According to Sahmaran et

http://dx.doi.org/10.1016/j.conbuildmat.2015.07.039
0950-0618/ 2015 Elsevier Ltd. All rights reserved.
438 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447

al. [10], the behavior of ECC after exposure to high temperature Table 2
could be attributed to the presence of PVA bers and high volume Chemical and physical properties of cement and y ash.

y ash. In a further research [11], they tried to understand the role Chemical composition (%) Cement Fly ash
of PVA ber and different replacement levels of y ash on the Na2O 0.33 0.26
microstructural damage and residual mechanical properties of MgO 1.34 0.50
ECC after exposure to high temperatures. It was concluded that Al2O3 3.71 28.24
adding micro PVA ber to the ECC matrix signicantly improves SiO2 15.33 57.78
P2O5 0.10 0.06
its resistance to thermally induced explosive spalling. In addition, SO3 3.33
increasing y ash content from 55% to 70% provides ECC with bet- Cl 0.09
ter residual mechanical properties after exposure to temperatures K2O 0.19 2.54
from 200 C to 600 C. On the other hand, the effect of the addition CaO 71.48 1.26
MnO 0.045 0.03
of y ash was diminished when the exposure temperature was
Fe2O3 3.78 4.76
raised to 800 C. ZnO 0.03
Wu et al. [12,13] have studied three different types of SHCC SrO 0.26
after exposure to temperatures up to 200 C and concluded that TiO2 0.95
SHCC made with quartz sand is more temperature sensitive than BaO <16
Loss on ignition (%) 4.93 3.55
SHCC made with regional river sand and the maximum crack width
Density (g/cm3) 3.08 2.35
increases after exposure to temperature.
Other studies have also reported the temperature inuence on
SHCC. The specimen size effect and temperature inuence on the
residual compression properties of ECC specimens were studied
by Erdem [14]. Mechtcherine et al. [15] have studied the effect of
temperatures up to 150 C, with different strain rates and combi-
nations of these parameters on the mechanical behavior of SHCC.
Differently from previous studies, the purpose of the research
described in this paper is to gain a better understanding of the
effects of elevated temperatures on the mechanical behavior of
SHCC. In this research, uniaxial tension, bending and compression
tests were used to analyze and characterize the mechanical prop-
erties of SHCC after exposure to elevated temperatures. The strain
characteristics and crack pattern including number, position, den-
sity and width of cracks, were also monitored and quantied.
Mercury intrusion porosimetry was used to investigate the effects
of temperature in the composite microstructure. Furthermore, this
study also explored the potential relationship between bending
and tensile behavior.
Fig. 1. Particle size distribution of cement, y ash and sand.
2. Experimental program

2.1. Materials melting temperature at about of 244 C (see Fig. 2(a)). The value of Tg was deter-
mined by the point on the thermal curve corresponding to1/2 the heat ow differ-
The mixture proportion used in this study is shown in Table 1. Portland cement ence between the extrapolated onset temperature (Tf) and temperature of return to
CPII F-32, dened by the Brazilian standard [16], composed of ller (in mass: baseline (Tr) in the DSC curve (Fig. 2(b)), according to recommendation of ASTM
610%) with a 28 days compressive strength of 32 MPa; y ash; silica sand with a E1356 [18]. In addition, the onset degradation temperature of PVA ber is about
maximum diameter of 0.212 mm and density of 2.60 g/cm3; and a superplasticizer, 239 C (see Fig 2(a)). More information about the thermal durability of polyvinyl
CC583 (manufactured by Cognis) based on melamine with 100% solid content and alcohol bers can be found in [17].
density 0.73 g/cm3 were used. The physical and chemical properties of Portland
cement and y ash are shown in Table 2 and the particle size distribution of aggre-
gates and cementitious materials can be seen in Fig. 1.
The bers used in this study were PVA bers (trademark REC15), manufactured 2.2. Composite manufacturing, curing and heating of specimens
by Kuraray Co Japan, with a diameter of 40 lm, density of 1.31 g/cm3, elastic
modulus of 39.93 1.90 GPa, tensile strength of 1576.20 60.90 MPa [17]. To produce the mixtures, all dry raw materials except bers were mixed for
According to thermal analysis reported in Fig. 2, the used PVA ber presents the 3 min in a mechanical mixer with a 20 l capacity. Water was added to form the
glass transition temperature (Tg) at approximately 66 C (see Fig. 2(b)) and a basic matrix. The mixture was stirred for another 8 min to allow appropriate
workability of the matrix. In the last step, bers were added manually to the
cementitious matrix and the mixture was stirred for 5 more minutes.
The specimens were cast in steel molds and demolded 24 h after casting, always
Table 1
covered with damp cloths. The specimens were cured for 28 days in a curing cham-
Mix design and fresh state properties of composite.
ber with 100% relative humidity and temperature of 21 1 C. Three bending and
Mix design (kg/m3) compressive specimens and ve tensile specimens were tested immediately after
the curing period, which are referred to in this study as the reference or unheated
Cement 505
specimens.
Fly ash 605
The specimens submitted to thermal treatment were maintained in ambient
Sand 404
temperature (22 1 C) for 24 h before they were heated. The heating equipment
Water 404
used in the investigation was an electrically heated furnace, in which the specimens
Superplasticizer 15
were heated at a constant rate of approximately 1 C/min, until the prescribed
PVA ber 26
temperature was reached. When the targeted peak temperature was reached, the
Fly ash/cement ratio 1.20
furnace temperature was maintained constant for 60 min and then the furnace
Water/(cement + y ash) ratio 0.36
was turned off and specimens were allowed to cool down to room temperature.
Air content (%) 2.80
In this research, ve temperature levels (90 C, 110 C, 145 C, 190 C and 250 C)
Density (g/cm3) 1.96
were considered. Tests were performed when the specimens were cooled down
Table ow (mm) 290
to room temperature (22 1 C).
 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447 439

Fig. 2. Thermal analysis of PVA ber: (a) TG/DTG and DSC curves and (b) DSC of the region I selected in (a).

3. Test procedure
60
3.1. Uniaxial tension, bending and compression tests

80
All mechanical tests were performed in a Shimadzu AGX
Universal Testing Machine with a capacity of 100kN. The tests
were performed at a cross-head displacement rate of 0.1 mm/min.

45
LVDT
Five specimens with the dimensions of 330  30  30 mm
(length  width at the center x thickness) were tested under uni-

gauge length
axial tension. The tensile specimen and test set-up are shown in

330
70
80
Fig. 3(a) and (c). Two LVDTs were used to measure displacements
(a)
between two points on the specimen at a gauge length of
80 mm. The tensile loads and corresponding displacements were LVDT
continuously recorded during the tests. The stress was obtained 30

45
by dividing the load by the nominal area of the cross section, while
the strain was obtained by dividing the elongation of the specimen
by the gauge length.

Three samples measuring 400  60  12.5 mm (length 
width  thickness) were tested under four-point bending loads at
a span of 255 mm (see Fig. 3(b)). Deections at mid-span were
measured using an electrical transducer (LVDT). The loads and
corresponding deections were continuously recorded on a com-
puterized data recording system.
Compression tests were performed on cylindrical specimens of
50  100 mm (diameter  height). The complete loaddisplace-
ment data was recorded. The reported data are the average values
from three specimens. The elastic modulus was calculated accord-
ing to NBR 8522 [19].
3.2. Crack patterns characterization method
Crack patterns were evaluated at regular time intervals during
the uniaxial tension and bending tests. A digital Nikon camera,
model D90, with 12.3 effective megapixels and AF-S DX Nikkor
lens (see Fig. 3(a)) was used to capture images at 60s intervals,
which were used to evaluate the crack formation (crack width
and crack density) during tests. The image of the face subjected
to tension in the bending tests was taken using a mirror positioned
at 45 to the specimen (see Fig. 3(b)).
To quantitatively measure crack width in uniaxial tension tests,
an image processing was carried out by the digital processing tool-
box of Image J 1.38x software and correlated with the applied ten-
sion strain. The crack width was measured in pixels and the image
was calibrated using conventional techniques to convert the size of
a pixel to length measures. For the purpose of crack identication
and crack width calculation, a set of three lines was selected along
the specimen gauge area (see Fig. 3(c)). The crack was computed
80
(c)
(b)
Fig. 3. Set-up of the (a) tension and (b) bending tests and (c) tensile specimen
(dimensions in mm).
only when it passed through all three lines. The number of cracks
was counted as seen on the image at a gauge length of 70 mm for
the tensile specimens (see Fig. 3(c)) and 85 mm for the bending
specimens, located at the central part of the specimen.
The crack density (number of cracks per meter) of each tensile
or bending specimen was obtained by dividing the number of
cracks by the gauge length. The reported data are the average
values from three specimens.
3.3. Pore structure characterization of unheated and heated SHCC
specimens
To obtain an insight into the residual properties, the pore size
distribution was determined by the Mercury Intrusion
Porosimetry (MIP) technique. Pore structure data from MIP allows
quantication of the changes in the structure and understanding
the mechanisms of SHCC deterioration due to elevated tempera-
tures exposure. The investigation was made using the porosi-
meters PASCAL 140 and PASCAL 240, company Thermo Fisher,
Italy by assuming the surface tension and the contact angle
440 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447

Fig. 4. Typical tensile stressstrain and average crack widthstrain curves of unheated composite (22 C) and after heating to 90 C, 110 C, 145 C, 190 C and 250 C.

between mercury and pore wall as 0.485 N/m and 140 respec-
tively. The maximum pressure of the porosimeter was 200 MPa.
Table 3
Tensile properties of the unheated composite and after heating to temperatures The samples of approximately 1 cm3 were dried at about 40 C
ranged from 90 C to 250 C (standard deviation in parenthesis). before the analysis.
The Environmental Scanning Electron Microscope (ESEM)
Temperature First- Maximum post- Strain Toughness,
(C) cracking cracking tensile capacitya, kJ/m3 model XL30-ESEM (FEI Philips Company, Netherlands) was used
strength, stress, MPa % to investigate the condition of SHCC samples for various testing
MPa conditions. The ESEM was operated under low vacuum. All the
22 2.12 (0.23) 2.97 (0.14) 2.98 99.83 micrographs were taken under the gaseous secondary electron
(0.69) (20.43) (GSE) detector mode at accelerating voltages of 2030 kV and
90 2.20 (0.16) 2.91 (0.14) 2.70 85.43 chamber pressure of 0.60.7 mBar. No coating with carbon or gold,
(0.38) (8.89)
as is usually done for high vacuum SEM, was required.
110 2.21 (0.13) 2.64 (0.05) 1.40 55.50
(0.19) (6.71)
145 2.22 (0.08) 2.65 (0.09) 1.41 56.20
(0.15) (3.23)
4. Experimental results
190 2.22 (0.03) 2.42 (0.14) 0.47 20.20
(0.09) (2.50) 4.1. Residual tensile and bending behavior
250 2.19 (0.16) 0.92 (0.13) 0.24 4.78 (0.78)
(0.04)
Typical tensile stressstrain curves of the tested specimens are
a
The strain capacity refers to the strain at which the localization of failure occurs. shown in Fig. 4 along with the average crack width-strain curves.
 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447
Fig. 5. Average crack density (a) and maximum crack width (b) under tensile loads as a function of imposed strain for unheated and preheated SHCC.
Fig. 6. Typical crack pattern observed at the end of uniaxial tension and bending
tests for the unheated composite (22 C) and after heating to 90 C, 110 C, 145 C,
190 C and 250 C.
Table 3 summarizes the tests results with regards to rst-cracking
strength, maximum post-cracking tensile stress, strain capacity
and toughness. The rst crack strength was read as the maximum
stress before the rst drop in the stressstrain curve, strain capa-
city was reported as the strain at which the failure occurred and
the toughness was computed as the total area under the tensile
stressstrain curve up to a post-peak strain corresponding to 40%
of the peak load. In the table, each value represents the mean result
of ve specimens.
As seen in Fig. 4, the tensile properties are slightly altered at
90 C. For instance, the mean rst-crack strength of the composite
increased from 2.12 MPa to 2.20 MPa (or + 3.8%), while the
maximum post-cracking tensile stress, the strain capacity and
the toughness decreased from 2.97 MPa to 2.91 MPa (or 1.8%),
2.98% to 2.70% (or 9.1%) and 99.83 kJ/m3 to 85.43 kJ/m3
(or 14.4%). This strain capacity reduction resulted in reduction
of crack density (number of cracks per meter) by approximately
441
26% (see Fig. 5(a)), but no further changes in average crack width
values can be observed when pre-heating temperature is increased
to 90 C.
Its important to observe that although the PVA bers did not
show any mass loss at 90 C (see TG/DTG curves in Fig. 2(a)) the
specimens were exposed to temperatures that are higher than
the PVA glass transition temperature (66 C), as seen in
Fig. 2(b), which can have inuenced the strain capacity and tough-
ness. Another important factor to be noted is that, since the PVA
bers used in this study are coated with an oiling agent, it is likely
that this agent is sensitive to temperature increases already at
moderate levels. Thus, the physical and, possibly, the chemical
properties of the agent may have changed when exposed to 90 C.
Specimens preheated to 110 C and 145 C showed similar
behavior. For example, mean rst crack strength of both specimens
increased approximately 4.4% compared to unheated specimens,
while the maximum post-cracking tensile stress, strain capacity
and the toughness decreased by approximately 11%, 53% and 44%
as seen in Table 3.
A look at Fig. 5(a) reveals that the crack density-strain curve
was also substantially affected by the pre-heating. The maximum
crack density of specimens preheated to 110 C and 145 C were
reduced respectively by 50.6% and 56.6% as compared to the max-
imum crack density of unheated specimens, but, up to 1% strain,
the crack density was not signicantly modied by the
temperature.
In terms of average crack width, the specimens preheated to
110 C and 145 C presented a steady state crack value of around
68 lm (Fig. 4) similar to unheated specimens. However, this steady
state crack only remained up to approximately 0.60.7% strain
(see Fig. 4), when the crack grew abruptly.
The maximum crack widths in the unheated and preheated spe-
cimens are shown in Fig. 5(b) as a function of imposed strain. The
curves in Fig. 5(b) indicate that the maximum crack widths
increased with the imposed strain, in opposite as seen in
Fig. 4(a)(d). However, at lower strain level (up to approximately
0.5%), the average and maximum crack widths results do not differ
signicantly.
Good consistency in the maximum crack widths was observed
between unheated SHCC and preheated to 90 C, where the
differences presented were relatively small. In contradiction, the
maximum crack widths of SHCC preheated to 110 C and 145 C
were affected by temperature. For instance, the maximum crack
widths of specimens preheated to 110 C and 145 C reach 80 lm
at a strain level of around of 0.50% and 100 lm at a strain level
442 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447

Fig. 7. Typical bending stressdeection curves of unheated composite (22 C) and after heating to 90 C, 110 C, 145 C, 190 C and 250 C.

between 0.60% and 0.80%. It has been shown that if crack widths
Table 4 are less than 100 lm, no signicant additional durability degrada-
Bending properties of the unheated composite and preheated to temperatures ranged
from 90 C to 250 C (standard deviation in parenthesis).
tion occurs. [20,21].
These results indicated that pre-heating affected the individual
Temperature First- Ultimate Deection Toughness, components of the SHCC system (matrix, ber and bond). PVA
(C) cracking bending capacitya, % kJ/m2
stress, MPa strength, MPa
bers have progressive loss in tensile strength from 90 C [17],
are very strongly deformed at 150 C [15], which can be traced
22 5.61 (0.21) 10.25 (0.29) 24.20 214.34
(1.06) (12.18)
back to very high deformability and low strength of PVA bers at
90 5.67 (0.37) 10.63 (0.14) 18.33 183.02 this relatively high temperature, although the thermal degradation
(1.53) (30.38) process of PVA bers only starts at 256 C, as shown in Fig. 2(a),
110 6.11 (0.03) 9.35 (0.43) 17.49 159.72 and bond strength is likely to improve due to densication of the
(1.04) (16.59)
bermatrix interface during pre-heating. Thus, ber cannot take
145 7.70 (0.26) 9.32 (0.36) 13.53 128.95
(0.50) (23.84) over the tensile load when the matrix fails, which explains why
190 8.25 (0.35) 8.61 (0.83) 3.90 (0.79) 36.29 the maximum crack density was reduced in the experiments at
(14.56) 110 C and 145 C.
250 7.76 (0.52) 5.26 (1.11) 1.46 (0.10) 13.03 At 190 C, the composite was still capable of load-bearing after
(4.30)
cracking (maximum post-cracking tensile stress is higher than
a
The deection capacity refers to the deection at which the localization of rst-cracking strength). However, Fig. 6 indicates that the speci-
failure occurs. mens exhibited only one single crack formation. The results also
 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447
Fig. 8. Fracture surfaces of unheated specimen and after heating to 250 C.
Fig. 9. Average crack density (number of cracks per meter) curves under bending
loads.
indicated that the maximum post-cracking tensile stress, strain
capacity and toughness reduced respectively by about 18.4%,
84.2% and 80%, while the rst-cracking strength increased about
of 4.7%. The interpretation of this behavior is given in Section 4.2.
When exposed to 250 C, a strain softening behavior was
observed after rst cracking, as seen in Fig. 4. Because of the
strain-softening behavior after heating to 250 C, a single crack
developed in the tensile specimen (see Fig. 6) and the strain capa-
city, toughness and maximum post-cracking tensile stress were
reduced by 92%, 95.3% and 69% respectively. The reduction in
strain capacity of the composite with increasing temperature could
be explained by changes occurring in the ber structure at this
relatively high temperature, since the PVA bers used in this study
present a melting temperature at about of 244 C (see Fig. 2a).
For a clearer analysis of the effect of the temperature on the
ductility of SHCC, bending tests were carried out on preheated
and reference (unheated) specimens and the results correlated
with the tensile tests. The bending performance of the SHCC speci-
mens was assessed based on the four-point bending test in terms
of rst-cracking stress, ultimate bending strength, ultimate mid-
span deection at peak stress, which will be referred to as deec-
tion capacity, and toughness. The toughness of the composites
was calculated from the area under the bending stressdeection
curves up to a post-peak deection corresponding to 40% of the
443
peak load, while the rst cracking point is dened as the point
where nonlinearity in the bending stressdeection curve becomes
evident.
Typical bending stressdeection curves are shown in Fig. 7.
The results of the evaluation of all curves are given in Table 4.
Each result in Table 4 is the average of three specimens. Fig. 7 indi-
cates various changes in SHCC performance after heating. The
curves show reductions in deection capacity, toughness and ulti-
mate bending strength while the rst cracking stress seems to
increase slightly.
The results presented in Table 4 indicate that at 90 C the mean
rst-crack stress and ultimate bending strength of the specimen
increased slightly (about +1.1% and +3.7%), while the deection
capacity and the toughness decreased 24.3% and 14.6%
respectively.
When exposed to temperatures from 110 C to 190 C the mean
rst-crack stress increased up to 47%, while the ultimate bending
strength, deection capacity and toughness decreased by up to
16%, 84% and 83% respectively. However, the composite still pre-
sented deection hardening behavior (ultimate bending strength
is higher than rst-cracking stress).
When pre-heating to 250 C the composite loses load-bearing
capacity in the post-cracking stage, due to the melting of PVA ber
at this temperature level (see Fig. 2(a)), evidenced by the absence
of bers as shown in Fig. 8. In this case, the composite is therefore
considered to be a quasi-brittle material with deection softening
behavior (Fig. 7) with reduced deection capacity (about 94%),
toughness (about 94%) and ultimate bending strength (about
49%) as compared to unheated specimens. However, the
rst-cracking stress was increased by about of 39%.
The macroscopic observations of the crack pattern of the speci-
mens revealed that the specimens preheated at 90 C, 110 C,
145 C, 190 C and unheated specimens presented a multiple
cracking pattern during the inelastic deection process (see Fig.
6) with crack saturation appearing in the constant moment region
(region II) of the specimen, although some ne cracks appear on
both sides outside the constant moment region. In contrary, the
specimens preheated at 250 C had only one crack as seen in Fig. 6.
Concerning the average crack density, Fig. 9 indicates that the
maximum crack density of specimens preheated to 90 C, 110 C,
145 C and 190 C were reduced respectively by 7%, 38.2%, 65%
and 84.2% when compared to unheated specimens. However,
pre-heating to 90 C and unheated specimens presented similar
crack density for deections up to 18 mm. The crack density of
each bending specimen was obtained by dividing the number of
444 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447

Table 5
Compressive properties of the unheated composite and after heating to temperatures
ranging from 90 C to 250 C (standard deviation in parenthesis).

Temperature Elastic Compressive Strain at Toughness

(C) modulus, strength, MPa peak stress, rate, MPa/%
GPa
22 19.00 (0.40) 37.00 (0.57) 3587.31 0.24 (0.18)
(6.47)
90 15.00 (0.26) 39.52 (0.60) 4952.73 0.25 (0.00)
(13.36)
110 15.00 (0.74) 39.71 (1.35) 4489.22 0.35 (0.17)
(86.18)
145 14.77 (0.29) 43.46 (0.57) 4422.31 0.42 (0.02)
(62.16)
190 14.73 (0.38) 44.04 (1.44) 3898.30 1.13 (0.08)
(75.99)
250 11.80 (0.26) 35.92 (0.90) 3483.44 1.69 (0.28)
(196.10)

unheated and preheated to 90 C, 110 C, 145 C and 190 C was

respectively equal to 4.9, 4.9, 4.2, 4.2 and 3.9. In contrast, for quasi
brittle materials, such as preheated specimens to 250 C, the ratio
of bending strength to rst-cracking strength was lower than 3 due
to strain softening behavior [22]. These results are in agreement
with an earlier study by Maalej and Li [23], in which a value of 5
was observed for strain hardening PE-ECC with tensile strain of
5.4%.
Regarding the inuence of temperature in deection capacity
and toughness under bending loads, the tendency was similar as
reported in tensile tests. Both were reduced with increasing tem-
perature as seen in Fig. 10(a) and (b). Similar tendency was also
observed in crack density curves under bending and tensile loads
(see Fig. 10c). The curves indicate that there are relatively good
correlations between the results of the bending and uniaxial
tension tests with linear correlation coefcient equal to 0.85,
0.97 and 0.90 for strain capacity, toughness and crack density,
respectively. Generally, the strong correlation between bending
deection and tensile strain is in agreement with the ndings of
earlier studies [24,25]. According to Qian and Li [24], tensile strain
capacity can be derived from bending deection capacity by a sim-
plied inverse method, which shows a linear relation between ten-
sile strain capacity and deection capacity when the material
presents a true strain-hardening behavior. Therefore, the bending
test was efcient to map the composite degradation.

4.3. Behavior under compression

The compressive behavior of unheated and preheated

Fig. 10. Comparison and relationship between tensile and bending tests: (a) tensile
strain capacity and bending deection capacity, (b) toughness and (c) crack density.
cracks by the gauge length (85 mm). The reported data is the aver-
age values from three specimens.
4.2. Relationship between bending and tensile tests results
It is well known that the bending properties of cement-based
materials are dependent on their tensile characteristics [22,23].
According to Maalej and Li [22] the ratio of ultimate bending
strength to tensile rst-strength of quasi-brittle ber cementitious
composites lies between 1 and 3. The boundary ratios 1 and 3
correspond to elastic brittle material and perfect elasticplastic
material, respectively.
For the current research, the ratio of bending strength to
rst-cracking tensile strength in strain hardening composites
specimens was determined experimentally at an age of 28 days.
Fig. 11 shows the typical stressstrain relationship measured from
the compression tests and mean results with standard deviation
(in parenthesis) are summarized in Table 5. The reported data is
the average value from three specimens. Toughness rate was calcu-
lated as the slope of the descending branch of the compressive
stressstrain curve, in post-cracking region, up to a post-peak
stress corresponding to 70% of the peak stress.
The results in Table 5 indicate that the elastic modulus was
reduced (after heating to 90 C) by about 21% remaining approxi-
mately constant until the temperature of 190 C. However, the
compressive strength was slightly increased by about 7% after
heating to 90 C. When pre-heating to 110 C the compressive
strength was not signicantly changed as compared to composite
heated to 90 C. At 145 C and 190 C the compressive strength
increased about 19% as compared to unheated specimens. This
nding is consistent with the works of other researchers. Several
hypotheses have been proposed to explain this increase in
strength. Nasser and Marzouk [26] have reported an increase of
 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447 445

Fig. 11. Typical compressivestrain curves of unheated SHCC (22 C) and after heating to 90 C, 110 C, 145 C, 190 C and 250 C.

compressive strength for concrete containing 25% of y ash con-
tent by weight exposed to temperatures ranging from 121 C to
149 C for periods of over 6 months. They have suggested that this
increase is due to the formation of tobermorite gel (a product of
hydrated lime and y ash at high pressure and temperature),
which was reported to be two to three times stronger than the
CSH gel. A similar increase in strength was reported by
Diederichs et al. [27], between 200 C and 250 C in a concrete
incorporating Class F y ash. Dias et al. [28] attributed the increase
in the compressive strength between 150 C and 300 C to a
rehydration of the paste due to the migration of the water in the
pores. In another study, Castillo and Durrani [29] have assigned
the compressive strength gains at 200 C to the increase in the
Van der Walls forces between the gel particles due to the water
removal.
When pre-heating to 250 C, the deterioration of composite is
more evident. The elastic modulus and residual compressive
strength were reduced by about 38% and 3% respectively compared
to unheated specimens.
With regard to post-peak behavior, the results presented in
Table 5 and Fig. 11 indicate that, at 90 C, the toughness rate is
similar to the unheated specimen. However, after heating to
110 C and 190 C, the compressive toughness rate of the compo-
site was increased up to 371%, which indicates a reduction in com-
pressive ductility of the composite. Specimens preheated to 250 C
were characterized by post-peak fragility due to melting and
degradation of the PVA ber.
For a clearer presentation of the effect of temperature on the
compressive response of SHCC, Fig. 12 provides the variations of
cumulative pore volume and its distribution as inuenced by
446 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447

Fig. 12. Pore size distributions of SHCC before and after exposure to elevated temperatures.

The signicant increase in the volume of pores lower than

Table 6
50 nm for the SHCC specimens after heating up to 190 C found
Total intruded porosity, average pore diameter and pore size distribution of unheated
specimens and after heating to temperatures ranging from 90 C to 250 C. in this study strongly suggests that this renement of the pore
structure may be responsible for the signicant increase in com-
Temperature Total Average Volume of pores (%)
pressive strength, as discussed previously. On the contrary, pores
(C) intruded pore
<50 nm 50100 nm >100 nm lower than 50 nm and 50100 nm of specimens preheated to
porosity diameter
(%) (nm) 250 C increased respectively 13.4% and 6.4% due to melting and
22 24.67 32.30 9.55 6.12 9.00 degradation of PVA ber, which results in additional void space
90 24.10 28.80 10.27 5.81 8.02 as seen in Fig. 8.
110 24.09 25.20 12.08 4.08 7.93 Another evidence of pore rening in the material can be seen in
145 25.84 24.20 13.81 3.52 8.51 Table 6 which indicate a reduction in the volume of pores larger
190 26.07 29.10 11.45 6.09 8.52
250 30.23 33.90 10.84 6.52 12.87
than 100 nm in specimens preheated up to 190 C which gener-
ally inuences the strength of concrete [30]. According to Khoury
[31], the reduction of cumulative volume of pores larger than
100 nm may be attributable to further hydration of unhydrated
different heating levels. Porosimetric data, such as average pore cement particles and the pozzolanic reaction of unhydrated y
diameter, pore size distribution and total intruded porosity are ash particles with portlandite to produce more CSH phases that
summarized in Table 6. deposit in the pore system.
Results in Table 6 indicate that the total intruded porosity of the
specimens preheated at 90 C and 110 C had a slight decrease of 5. Conclusions
about 2.5% when compared to unheated specimen. However, when
the specimens were preheated to 145 C, 190 C and 250 C, the The experiments carried out provide additional information for
total intruded porosity increased respectively 4.8%, 5.7% and 22.5%. the SHCC material behavior after exposure to elevated tempera-
These results highlight that although total intruded porosity tures. These results are of great importance for this material
had increased at 145 C and 190 C, the pore structure became ner application on a large scale, since it represents a valuable contribu-
in specimens preheated up to 190 C, as illustrated by an average tion to the study of SHCC material. From the results, the following
pore diameter decrease in Table 6. The results showed a decrease conclusions can be drawn:
in the average pore diameter of 11%, 22%, 25% and 10% when the
specimens were preheated to 90 C, 110 C, 145 C and 190 C It is clear that temperature affects the mechanical properties of
respectively. However, at 250 C, due to melting and degradation SHCC after exposure to temperatures up to 250 C. The dete-
of PVA ber, the average pore diameter indicated a slight increase rioration of the composite was observed in terms of reduced
of 5% when compared to the unheated composite. stiffness, tensile strength, ductility and several changes in the
Comparative analysis of the pore size distribution in Table 6, also cracking pattern;
indicates renement of the pore structures in the specimens after At 90 C the residual tensile properties are slightly altered. The
heating to 190 C. In this research, the pore structure was divided composite presented a strain hardening behavior with a pro-
into three groups: lower than 50 nm, 50100 nm and higher than nounced multiple cracking pattern, strain at failure of around
100 nm, and the distribution of pore volume in those ranges was 2.7% and crack width equal to 68 lm. However, the toughness
calculated. The results presented show an increase of approxi- and crack density were reduced as compared to unheated speci-
mately 44.5% in the mercury intruded volume in pores lower than mens due to changes in ber microstructure.
50 nm and a reduction up to 42.6% in the mercury intruded volume Heating to 110 C showed similar tendencies as specimens
in pores with 50100 nm for the specimens preheated up to 145 C. heated to 145 C. For example, mean rst crack strength of both
At 190 C was observed increase of approximately 20% in the mer- specimens increased when compared to unheated specimens,
cury intruded volume in pores lower than 50 nm and a reduction of while the maximum post-cracking tensile stress, strain capacity
approximately 1% in pores with 50100 nm. and toughness decreased. In terms of crack width, unlike
 M.S. Magalhes et al. / Construction and Building Materials 94 (2015) 437447
unheated specimens, the specimens preheated to 110 C and
145 C presented a steady state crack value of around 68 lm
only up to 0.6% strain, when the crack grew abruptly leading
to crack opening.
At 190 C, the composite was still capable of load-bearing after
cracking. However, the specimens exhibited only one single
crack and the maximum post-cracking tensile stress, strain
capacity and toughness were strongly reduced, while the
rst-cracking strength was slightly increased.
At temperatures of 250 C the composite loses load-bearing
capacity in the post-cracking stage, due to the melting and
decomposition of PVA ber. In this case, the composite is there-
fore considered to be a quasi-brittle material with strain soften-
ing behavior with reduced strain capacity (about 92%),
toughness and post-cracking tensile stress. However, the
rst-cracking strength was slightly increased as compared to
unheated specimens;
Regarding the bending performance, the tendency was similar
as reported in tensile tests. The results also indicated that there
are relatively good correlations between the results of bending
and uniaxial tension tests;
Concerning compressive behavior, the strength increased up to
19% when preheated up to 190 C due to renement of the pore
structures in the specimens at this temperature level. However,
at 250 C, the deterioration of SHCC is most evident in terms of
reduction of compressive strength and elastic modulus.
Acknowledgments
The authors acknowledge the Brazilian National Council of
Research and Development (CNPq), the Scientic and
Technological Research Agency of Rio de Janeiro State (FAPERJ)
and the Quality Improvement Program for Universities of the
Ministry of Education and Culture (CAPES) for the nancial
support.
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