Behavior of High-Strength Polypropylene Fiber-Reinforced

Self-Compacting Concrete Exposed to High Temperatures

José D. Ríos 1; Héctor Cifuentes, Ph.D. 2; Carlos Leiva, Ph.D. 3; Celia García, Ph.D. 4; and María D. Alba, Ph.D. 5
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Abstract: In this study we analyzed the use of high-performance structural concrete reinforced with polypropylene fibers in applications
requiring long exposure times to high temperatures, such as thermal energy storage systems. We analyzed the behavior of the concrete
at different temperatures (hot tests: 100°C, 300°C, 500°C and 700°C), cooled-down states (cold tests) and exposure times (6, 24, and
48 h). We also experimentally determined the thermogravimetric analysis, fracture behavior, compressive strength, Young’s modulus,
and tensile strength of concrete. Subsequently, we performed a comprehensive analysis of the thermal and mechanical behavior of
high-performance concrete under different thermal conditions. We applied longer exposure times to broaden the available results on the
behavior of high-performance fiber-reinforced concrete when subjected to high temperatures. Results show that, once thermal and moisture
equilibriums are reached, exposure time does not have any influence on mechanical properties. They also provide useful information about
the influence of high temperatures on the different parameters of fiber-reinforced concrete and its application for thermal energy storage
structures. DOI: 10.1061/(ASCE)MT.1943-5533.0002491. © 2018 American Society of Civil Engineers.
Author keywords: High-strength concrete; Polypropylene fibers; High temperatures; Exposure time; Fracture behavior.

Introduction
The use of renewable energies as a main energy source is a topic of
great interest for those countries lacking fossil energy sources, and
for those seriously committed to the reduction of CO2 emissions.
For this reason, although renewable energy sources are already
being used, their technologies are the subject of ongoing research
(Alotto et al. 2014; Alonso et al. 2016; Chauhan and Saini 2014).
Solar energy is one of the most widespread renewable energy op-
tions worldwide because it is generally abundant, and the predic-
tion of solar radiation hours, and hence of energy production, is
very easy when compared with other renewable energy sources
(Alonso et al. 2016). Additionally, the technology available for
the production of electricity through solar energy is also the only
one that allows for its storage. The development of a solar energy
storage system is therefore crucial to produce energy in a more uni-
form way and would allow this renewable energy to be more com-
petitive against fossil energy sources. Storage system materials
must not only be capable of bearing loads, but also, most impor-
tantly, they must withstand the effects of high temperatures for
1
Ph.D. Student, Grupo de Estructuras, Escuela Técnica Superior de
Ingeniería, Universidad de Sevilla, Sevilla, Andalucia 41092, Spain.
2 ity, and relatively low cost (Alonso et al. 2016); on the other hand,
Associate Professor, Grupo de Estructuras, Escuela Técnica Superior
de Ingeniería, Universidad de Sevilla, Sevilla, Andalucia 41092, Spain
(corresponding author). ORCID: https://orcid.org/0000-0001-6302-418X.
Email: bulte@us.es
3 heat storage material that use a series of pipes filled with water as
Associate Professor, Grupo de Ingeniería de Residuos, Escuela Técnica
Superior de Ingeniería, Universidad de Sevilla, Sevilla, Andalucia 41092,
Spain.
4
Grupo de Ingeniería de Residuos, Escuela Técnica Superior de
Ingeniería, Universidad de Sevilla, Sevilla, Andalucia 41092, Spain.
5
Professor, Instituto de Ciencia de Materiales, Consejo Superior de
Investigaciones Científicas-Universidad de Sevilla, Sevilla 41092, Spain.
Note. This manuscript was submitted on November 9, 2017; approved
on May 2, 2018; published online on August 1, 2018. Discussion period
open until January 1, 2019; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
variable periods of time during plant operation. One of the uses
of concrete in thermal storage systems is in steam collectors. These
systems directly use steam as a means of storing thermal energy:
when liquid water is heated and turned into steam, the steam goes to
the turbine or is alternatively stored in concrete tanks or basins to be
used when solar radiation is interrupted. In these cases, the concrete
is subjected to high temperatures for long periods of time, being in
direct contact with the steam. Therefore, the heat loss factor, heat
storage power, and cost of the containing material are all key as-
pects. A concrete steam collector must be able to withstand a tem-
perature range between approximately 100°C and 300°C.
Basically, energy storage systems must be composed of two
materials. One of them should have high heat storage capabilities,
such as those of certain mixtures of molten salts or phase-change
materials (Alonso et al. 2016; Herrmann et al. 2004; Laing et al.
2009; Pielichowska and Pielichowski 2014; Yang and Garimella
2010); the other one should be a structural material that functions
as a containment vessel for the former, and must be properly insu-
lated through the use of refractory materials to ensure it is not dam-
aged by high temperatures. In this regard, concrete is emerging as a
material with a twofold application: on the one hand, it is one of the
most widely used structural materials because of its mechanical
properties, on-site workability, easy handling, worldwide availabil-
concrete has interesting heat storage capabilities due to its thermal
properties (Alonso et al. 2016). In this regard, examples are found
in the literature of heat storage technologies based on concrete as a
a heat transfer fluid inside a concrete block (Alonso et al. 2016;
Laing et al. 2009) that contains phase-change materials (Fenollera
et al. 2013; Memon et al. 2015).
Normally, the maximum serviceability temperature of structural
concrete is limited by the potential damage caused by the high
temperatures involved. This damage is manifested as microcracks
originated by the pore pressure inside the concrete matrix, due to
the evaporated water (Cifuentes et al. 2012; Zhang and Bicanic
2006). If the concrete has good matrix porosity, as happens in
the case of normal strength concrete, the evaporated water can flow

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J. Mater. Civ. Eng., 2018, 30(11): 04018271

 outside the concrete through the pore connection of the matrix.
This effect, combined with medium-high temperatures, causes neg-
ligible effects of the pore pressure and thus results in no damage to
the concrete matrix (Cifuentes et al. 2012; Srikar et al. 2016; Zhang
and Bicanic 2006). However, in the case of dense concrete mixes
such as high-strength concrete or if the concrete is subjected to
very high temperatures, the pore pressure thus originated can be
very harmful for the concrete matrix, causing failure of the material
through spalling (Cifuentes et al. 2012; Zhang and Bicanic 2006).
The only situation in which the behavior of structural concrete
under high temperatures has been studied is in fire conditions
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degradation than normal concrete when exposed to high tempera-
tures, and is more affected by spalling and cracking (Alonso et al.
2016). The addition of polypropylene (PP) fibers reduces these
negative effects and improves the mechanical properties of concrete
at high temperatures (Chauhan and Saini 2014; Yang and Garimella
2010). Fiber length is an important factor in enhancing the fracture
behavior of concrete at room temperature, because longer fibers
provide higher resistance to pull-out failure (Herrmann et al. 2004).
Another important aspect to consider in these applications is
the study of the behavior of concrete over long exposure times
at a constant temperature and in the subsequent cooling process.
Due to the usual limitations in the serviceability temperature of

(Kang et al. 2016; Liu et al. 2008; Zoalfakar et al. 2016). In such
studies, the structural material has been analyzed in an accidental concrete, there are few studies on this topic in the literature, and the
ultimate limit state in accordance with the standards. Standardized exposure times explored are very moderate (Mohamedbhai 1986).
fire-resistance tests of structural materials normally involve gradu- Residual mechanical properties after cooling and exposure time are
ally heating the material to a very high temperature (over 700°C). two essential aspects to study because, in the applications de-
However, in the case of moderate temperatures such as the operat- scribed, concrete is exposed to high temperatures during long peri-
ing temperatures of solar energy storage systems (≤300°C), if the ods and is alternatively subjected to working and resting stages.
concrete has adequate porosity there is no apparent reason to expect The use of self-compacting concrete is widespread, due to its
a dramatic decrease in the strength of the concrete. Below 300°C, benefits for a more efficient production process and the high per-
no major decomposition of the hydration products of the cement formance of the final product. The industry of precast products
should be observed (Cifuentes et al. 2012), and any eventual dam- (Barros et al. 2007) is one of the areas in which this type of concrete
age should only be caused by the pore pressure originated by the is used due to its better fluidity, which improves the final quality of
evaporated water inside the concrete (Srikar et al. 2016). However, the product and reduces construction time. Self-compacting con-
crete, sometimes reinforced with PP or steel fibers, is also used
these pore pressures may well not be high enough to cause any
in high-quality concrete projects such as buildings and industrial
mechanical damage to the concrete; in addition, the energy sup-
structures that need to withstand high temperatures during opera-
plied to the concrete through the heating process contributes to
tion or in case of an accidental fire (Bamonte and Pietro 2016;
hydrate unhydrated cement particles, which actually counteracts
Noumowé et al. 2006; Srikar et al. 2016; Tao et al. 2010).
the effects of thermal damage to the concrete and increases its
In this study, we analyzed the influence of different tempera-
mechanical properties (Kodur 2014).
tures on the mechanical behavior of high-strength self-compacting
In these applications of structural concrete for thermal energy
concrete mixes, both plain and polypropylene fiber-reinforced
storage, the study of the fracture behavior of the concrete is key
(6 and 24 mm fiber lengths), during three different exposure times
to control any potential damage caused. Moreover, it is usually nec- (6, 24, and 48 h) in hot specimens, and only one exposure time
essary to use high-performance concrete with high strength capac- (48 h) in cold specimens (after heating). We paid special attention
ity, especially tensile strength, to prevent premature cracking due to to the fracture behavior of these concrete mixes. Specifically, we
pore pressure. However, this type of concrete undergoes greater conducted standardized tests to characterize the mechanical behav-
ior of the various mixes at different temperatures and exposure
times. These properties were directly measured in heated and cold
Table 1. Chemical composition (%) of the materials concrete specimens.
Chemical
composition PC FA LA CA SF
SiO2 20.69 86.50 86.97 83.35 95.63
Experimental Study
Al2 O3 5.24 5.83 5.56 4.50 0.43
Fe2 O3 2.46 1.33 1.39 2.26 0.10 Materials and Mix Design
MnO 0.10 0.03 0.02 0.05 0.02
MgO 1.50 0.13 0.19 0.36 0.39 A summary of the materials used in the present study and their
CaO 61.89 0.59 0.51 3.42 0.21 characteristics is shown below:
Na2 O 0.36 0.87 0.95 0.09 0.20 1. Portland cement (PC) Type II 32.5 B-L, in accordance with
K2 O 0.73 2.37 1.97 1.04 0.79 the EN 197-1 standard [EN197-1:2000/A3 (CEN 2008)]. Its
TiO2 0.28 0.13 0.15 0.23 <0.01 chemical composition is provided in Table 1. It is essentially
P2 O 5 0.17 0.07 0.02 0.05 0.08 SiO2 and CaO.
SO3 1.11 0.04 0.03 0.03 0.04 2. Fine aggregate (FA) with a maximum size of 2 mm. Its grading
LOI 4.76 1.34 1.51 3.59 1.84
distribution is shown in Table 2. Its chemical composition is
Specific gravity 3.18 2.69 2.58 2.48 2.30
shown in Table 1. FA was essentially SiO2 and Al2 O3 .

Table 2. Grading distribution

Sieve size (mm)
Material >16 10 8 4 2 1 0.5 0.25 0.125 0.063 <0.063
FA 0 0 0 0 0 22.20 35.82 26.15 10.33 3.74 1.10
LA 0 0 0 0 11.50 26.50 21.00 17.33 12.00 9.17 2.33
CA 0 19.30 40.13 38.31 2.26 0 0 0 0 0 0

© ASCE 04018271-2 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2018, 30(11): 04018271

 Table 3. Mix design of all concrete types
Quantity (kg=m3 )
Type PC FA LA CA SF SP PPF
D0 657 867 139 1,301 99 23 0 0.20
D1 657 867 139 1,301 99 23 1.2 (PPF-6)
D2 657 867 139 1,301 99 23 1.2 (PPF-24)
3. Limestone sand (LA) with a maximum size of 4 mm (Table 2).
Its chemical composition is shown in Table 1. LA was composed
essentially of SiO2 and Al2 O3 , and its chemical composition
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was very similar to FA.
4. Coarse aggregate (CA) with a maximum size of 10 mm (Table 2).
Its chemical composition is shown in Table 1. CA was composed
essentially of SiO2 and Al2 O3
5. Silica fume (SF) manufactured by Sika, model S92-D, with
90% of particles under 0.1 μm and a SiO2 content above 90%
(Table 1). SF is essentially SiO2.
6. Superplasticizer (SP) (SIKA VISCOCRETE 20 HE), specific
for low water/binder ratio mixes.
7. Polypropylene (PP) fibers with a diameter of 33 μm and two
different lengths, 6 (PPF-6) and 24 mm (PPF-24). The tensile
strength of the PP fibers was 450 MPa.
Table 2 shows the grading distribution of FA, LA, and CA. As
shown in this table, FA was the finest, with an average particle size
of 0.48 mm; LA had an average particle size of 0.66 mm, and CA
had an average particle size of 6.72 mm.
In this study, we analyzed three different self-compacting con-
crete mixes, differentiated only by their respective PP fiber content.
The first mix, called D0, was considered as the reference concrete
mix and was not reinforced with PP fibers. The second and third
concrete mixes, called D1 and D2, respectively, had a PP fiber
content of 1.2 kg=m3 . Fiber length was 6 mm in the D1 concrete
and 24 mm in the D2 concrete. The concrete mix proportions are
specified in Table 3.
A laboratory mortar mixer was used to prepare the different
types of concrete. First, all dry constituents were poured into
the mixer and rotated for 5 min. Next, the PP fibers and the super-
plasticizer were added to the water and then poured into the mixer.
Finally, the mixer was left to rotate for a further 15 min until a fluid
and homogenous mix was obtained. Slump flow tests were con-
ducted on the self-compacting concrete (SCC) mixes in accordance
with EFNARC guidelines (EFNARC 2005), with satisfactory
results. The specimens were immediately cast, subsequently un-
molded, and after 24 h submerged in a water bath at a temperature
of 20°C for 28 days.
Heating Test
To explore the influence of temperature on the fracture behavior of
PP fiber-reinforced SCC, experimental tests were performed on
specimens at high temperatures (hot tests) and also after cooling
them down (cold tests). Additionally, a first batch of specimens
of each mix (D0, D1, and D2) was tested at room temperature,
without undergoing any heating, to serve as control results. In the
so-called hot tests, the second batch of specimens was heated at a
rate of 10°C=min until reaching five different temperatures (100°C,
300°C, 500°C, and 700°C), subjected to three different exposure
times (6, 24, and 48 h) at each of these temperatures, and immedi-
ately tested. In the so-called cold tests, the third batch of specimens
was heated at the same rate and the same temperatures for 48 h and
then cooled for 24 h at room temperature, after which they were
tested. The testing equipment used was specifically designed to
perform high-temperature tests, and made it possible to insert
© ASCE
J. Mater. Civ. Eng., 2018, 30(11): 04018271
the actuator, the specimen and the supporting structure into the
furnace.
W/PC
ratio
Mass Loss and Structural Effects
0.20 The effect of temperature on the concrete was monitored by
0.20 thermal analysis and variable temperature X-ray powder diffrac-
tometry (VTXRD) analysis. VTXRD patterns were recorded at the
CITIUS X-ray laboratory (University of Seville, Spain) by a
Bruker D8 Advance diffractometer (Bruker, Germany) fitted with
a high-temperature camera (Anton Paar XRK 900, Austria) and a
position-sensitive detector (Bruker Vantec PSD, Germany) in the
25°C–900°C temperature range at a heating rate of 10°C · min−1
(target: Cu; voltage: 40 kV; current: 40 mA; θ∶θ geometry com-
bining divergent Göbel mirror configurations; detector: radial
Soller slits; time scans: 5 min).
Simultaneous thermogravimetric (TG/DTA) measurements
were performed at the CITIUS Functional Characterization Service
(University of Seville, Spain) on a TA (model STD-Q600) instru-
ment, using alumina as a reference. The specimens were put into
platinum crucibles in a chamber containing air during the entire
heating period. The temperature was increased at a constant rate
of 10°C=min.
A differential scanning calorimetric analysis (DSC) was carried
out. The specimens, 5 mm in diameter and 3 mm thick, were placed
in nonhermetic aluminum containers and subjected to a heating
program of 2°C=min in a TA Instruments 2920 DSC from 40°C
up to 300°C, using nitrogen as a purge gas (Vilches et al. 2005).
Pore Size Distribution
Pore size was determined using a mercury intrusion porosimeter
with a measuring pressure range of 1.02 × 10−2 to 2.04 × 102 MPa.
The selected contact angle was 141°, so the measurable pore size
ranged from 0.007 to 144 pm. Pellet-shaped specimens about
5 mm in size were used. All specimens were previously heated to
105°C until no moisture was left.
Compressive Strength (f c )
The compressive strength tests of the control concrete mix and the
hot and cold specimens were carried out in accordance with the
EN12390-3 standard (CEN 2009a) in 50 × 50 × 50 mm-sized
cubes. These cubes were obtained by sawing off the 100 × 100 ×
440 mm cast prisms. All the prisms were made with the same con-
crete matrix to avoid any differences in the properties of the
material. The specimens of each batch were all simultaneously
heated in the same furnace to ensure that they were all subjected
to the same thermal cycle. The load was increased continuously at
a rate of approximately 0.5 MPa=s until the specimen ruptured
completely. Four cube specimens were tested in each case.
Tensile Strength (f t )
The tensile strength of concrete is an important mechanical prop-
erty for the analysis of its fracture behavior. Cylindrical specimens
100 × 200 mm in size (diameter × height) were manufactured with
each concrete mix. Due to the complexity of direct-tension testing
in concrete, indirect tensile strength tests such as the Brazilian split-
cylinder strength test were used (Planas 2007). The experimental
tests were performed on specimens at room temperature (i.e., con-
trol concrete and cold specimens). In the hot tests, due to limitations
of the testing machine, tensile strength evolution was estimated
from the maximum load value of three-point bending tests. It is
noted that the right determination of the tensile strength from
04018271-3 J. Mater. Civ. Eng.
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Fig. 1. Three-point bending test of a notched specimen.
three-point bending tests requires a more sophisticated procedure
(see Guan et al. 2016, 2017; Hu et al. 2017; Wang et al. 2016);
however, as the main objective is the analysis of the evolution
of the tensile strength with temperature, a direct relationship be-
tween f t and the peak load of the three-point bending (TPB) tests
was assumed. This simplified procedure was verified by using
specimens at room temperature (i.e., control concrete and cold
specimens) and obtaining tensile strength values in agreement with
their corresponding experimental results. The procedure proved to
be a reasonable way to estimate this material property in hot tests,
given the difficulty of experimental testing.
The Brazilian strength tests were carried out on the 100 ×
200 mm cylinders following the procedures recommended by the
EN 12390-6 standard (CEN 2009b). Plywood strips 15 mm wide ×
4 mm thick were placed between the specimens and the actuator.
The displacement velocity of the machine actuator was 2.8 kN=s,
and four specimens were tested in each case.
Determination of the Fracture Energy (G F )
Notched beams 50 × 50 × 220 mm (width × depth × length ¼
B × D × L) were used to determine the hot and cold fracture
energy. The fracture energy was assessed with stable TPB tests in
accordance with the RILEM work-of-fracture method (RILEM
1985). Certain modifications such as the recommendations pro-
posed by Guinea et al. (Elices et al. 1992; Guinea et al. 1992) were
considered to obtain a size-independent value. Four specimens
were tested in each case. Specimen length was L ¼ 220 mm, so
specimen span length was S ¼ 200 mm. It was equal to four times
the depth of the cross section; therefore, the influence of the span/
depth ratio (Karihaloo et al. 2003) was avoided. Initial notch depth
was a ¼ 25 mm, so relative notch depth was α ¼ 0.5 in all cases.
The notches were prepared with a diamond saw prior to the heating
process.
The three-point bending tests were performed in a 200 kN
dynamic machine, as illustrated in Fig. 1. The vertical displacement
at the midpoint in specimens at room temperature (i.e., control
concrete and cold specimens) was measured with a linear voltage
displacement transducer (LVDT) mounted on a rigid frame fixed to
the specimen. In hot specimens, however, this measurement was
obtained from the actuator position recording, because the high
temperatures in the hot tests made it impossible to use any meas-
uring instrument. Loading was conducted using an actuator, at a
rate of 0.01 mm=min until the peak load was reached; after this,
the velocity was increased to 0.05 mm=min during the postpeak
branch of the load-displacement (P-δ) curve. The supporting brack-
ets were mounted on steel ball bearings to allow them to freely
rotate around the beam’s major axis.
© ASCE 04018271-4
J. Mater. Civ. Eng., 2018, 30(11): 04018271
From the P-δ curve, the fracture energy of concrete was calcu-
lated using Eq. (1) specified in the RILEM (1985), applying the
corrections corresponding to the adjustment of the tail of the load-
displacement curve proposed by Guinea et al. (Cifuentes et al.
2017; Guinea et al. 1992).
WF
GF ¼ ð1Þ
BðD − aÞ
where GF = fracture energy (N=m), W F = total work of fracture,
and BðD − a0 Þ is the ligament area. The total work of fracture is
given by:
W F ¼ W m þ W nm ð2Þ
W m = measured work of fracture corresponding to the total area
below the P-δ curve recorded until the end of the test at δ u .
W nm = nonmeasured work of fracture, obtained by means of the
remote tail constant, A, taking into account the influence of cutting
the P-δ curve (Elices et al. 1992)
2A
W nm ¼ ð3Þ
δu
Young’s Modulus (E c )
The Young’s modulus of the specimens tested at room temperature
(i.e., control concrete and cold specimens) was experimentally cal-
culated in accordance with the EN 12390-13:2014 standard (CEN
2014). This was done by gradually loading a cylindrical specimen
in compression to approximately a third of its failure load and
measuring the corresponding strain with 30 mm strain gauges.
By contrast, it was impossible to use measuring instruments in the
hot tests, so the Young’s modulus was calculated based on the com-
pliance method proposed by Jenq and Shah (Shah 1990) for these
specimens. This method requires previous knowledge of the
initial slope of the load-crack mouth opening displacement curve
(P-CMOD), which was not measured in the hot specimens. The
initial slope of the P-CMOD curve is related to the Young’s modu-
lus, as shown in Eq. (5). As a result, the initial slope of the load-
displacement curve (P-δ) is also related to material stiffness, so it
is possible to obtain an initial slope of the P-CMOD curves and
establish their relationship with the P-δ curves. In the hot tests, the
P-CMOD curve was estimated from load-actuator-position curves,
applying the aforementioned rate. The estimated P-CMOD was
used to calculate the Young’s modulus by means of Jenq and Shah’s
compliance method (Shah 1990).
According to these indications, after obtaining the initial compli-
ance (Ci ) of the P-CMOD curves for all hot specimens, the elastic
modulus of concrete was obtained using the following expression:
J. Mater. Civ. Eng.
 6SaV 1 ðα 0 Þ
Ec ¼ ð4Þ
Ci BD2

where V 1 ðα 0 Þ = geometric function given by

0.66
V 1 ðα 0 Þ ¼ 0.8 − 1.7α 0 þ 2.4α 02 þ
ð1 − α 0 Þ2
4D
þ ð−0.04 − 0.58α 0 þ 1.47α 02 − 2.04α 03 Þ
S
a þ HO
α0 ¼ ð5Þ
D þ HO
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and HO = clip gauge holder thickness. In this case, HO was 1 mm

and there was no accuracy loss if α 0 ≈ α.
Obviously, according to Eq. (4), materials with higher initial
P-CMOD compliance curves have lower elastic modulus values.

Fig. 3. Mineral composition of D0.

Results and Discussion

Mass Loss
The thermogravimetric analysis of D0 from room temperature to
1,000°C after 28 days is shown in Fig. 2. As observed, D0 exhibited
three different weight losses. The first was observed at 100°C,
represented a mass loss of 4.2% wt and was due to the moisture
present in D0. The second, observed between 200°C and 500°C,
represented a mass loss of only 1.5% wt. It was due to the dehy-
dration of chemically bound water in several hydrates of the con-
crete (i.e., calcium silicate, carboaluminates, ettringite), although
primarily to the dehydration of calcium silicate hydrates at 450°C.
The third was observed between 650°C and 750°C, represented
a mass loss of 3.5% wt and was caused by the decarbonation of
calcium carbonate from the clinker and the filler (Alarcon-Ruiz
et al. 2005).
The mineral composition of a D0 specimen portion at different
temperatures (i.e., from room temperature to 900°C) after 28 days
is shown in Fig. 3. The main mineral compounds at room temper-
ature were quartz, PDF 01-085-0335; (q), calcite: CaCO3 , PDF
01-083-0578; (c), C3 S: Ca3 SiO5 , PDF 00-055-0738; and (s), albite:
NaAlSi3 O8 , PDF 01-089-6427 (a). When the temperature of D0
reached 700°C, the calcite disappeared, because it decomposed into
CO2 and CaO, as shown in Fig. 2.
Fig. 4 shows the DSC analysis of the polypropylene fibers. The
melting process took place over a range of temperatures between
145°C and 180°C, as seen from the width of the melting endotherm.
The melting point, that is, the peak of the melting endotherm, was
165°C.
As shown in Fig. 5, the fibers showed only one mass loss at
460°C, because at that point they were transformed into water
and CO2 .
Fracture Energy
The fracture energy values measured in each hot and cold test at the
different exposure times are presented in Fig. 6. In D0 hot tests
[Fig. 6(a)], the fracture energy showed a decreasing trend at
100°C. At that point, the concrete matrix still did not show any
relevant microcracking, so the vapor could not be freely evacuated.
This led to high moisture gradients in the matrix, entailing a reduc-
tion in the fracture energy (Zhang and Bicanic 2006). Above
100°C, the fracture energy rose until a temperature of 500°C was
reached, as shown by the increased area under the load-deflection
curves [Figs. 7(b and c)], which increased along with the temper-
ature. Although the maximum load decreased due to microcracking
by spalling, deflection increased (Zhang and Bicanic 2006). At
700°C, a significant amount of microcracking occurred due to the

Fig. 2. TG of concrete: D0 (without PP fibers). Fig. 4. DSC of PP fibers.

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Fig. 5. TGA of the PP fibers.

Fig. 6. Evolution of the fracture energy with temperature for each exposure time: (a) D0 hot tests; (b) D1 hot tests; (c) D2 hot tests; and (d) cold tests.

decarbonation of the calcium carbonate (Figs. 2 and 3), signifi-
cantly reducing the resistance of the material (Cifuentes et al. 2012;
Tufail et al. 2017) and dramatically reducing the fracture energy.
In the D1 and D2 hot tests performed on the PP fiber-reinforced
mixes [Figs. 6(b and c), respectively], the fracture energy was
slightly higher at 25°C and 100°C because the fibers compensated
the effects of the high pressure and moisture gradients within the
concrete (Cifuentes et al. 2012, 2013). At low temperatures such as
25°C and 100°C, the condition of the PP fibers was not affected by
temperature (Fig. 4), and their main role was the stitching of even-
tual cracks. At the aforementioned temperatures, the fibers gave the
concrete higher ductility, as inferred from the higher fracture energy
values [Figs. 6(b and c)]. The fracture energy values increase in the
D1 and D2 hot tests at 300°C, because the PP fibers had partially

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Fig. 7. Load-deflection curves in D0 hot tests: (a) 100°C; (b) 300°C; (c) 500°C; and (d) 700°C.
melted at this point (Fig. 4). Thus, internal vapor was evacuated
more easily, and the area under the load-deflection curves in-
creased. Due to the reproducibility of results, only the load-
deflection curves for D0 tests have been shown. At 500°C, the
fracture energy was still high for the same reasons that affected
D0. At 700°C, in addition to the decarbonation process, the PP
fibers were completely transformed into gaseous water and CO2 ,
and the pore level in the concrete matrix significantly increased
to 33 μm (the diameter of the fibers), as Fig. 10 shows. The use
of longer fibers increased the ductility of the material, as inferred
from the higher fracture energy values in Fig. 6(c) when compared
with Fig. 6(b). Moreover, the longer fibers generated a greater net-
work of channels through which vapor could be more efficiently
discharged, reducing damage to the concrete and increasing the
fracture energy (Cifuentes et al. 2012).
Regarding the D0 cold test, the trend was similar to that of D0
hot tests, with a difference: additional microcracking occurred due
to the cooling process, resulting in an earlier damage to the matrix
[Fig. 6(d)] (Cifuentes et al. 2012; Zhang and Bicanic 2006).
Comparing the D1 and D0 cold tests, at 100°C the addition of
PP fibers increased the ductility of the material, as shown by the
growing deflection in Fig. 9. The D1 and D2 load-deflection curves
of cold tests have not been represented due to the reproducibility of
results. It is worth noting that they showed qualitatively a similar
trend with a more pronounced deflection. At 300°C, the maximum
load noticeably decreased as the PP fibers partially melted (Fig. 4).
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The deflection increased because the matrix had more pores due to
the melting of the fibers, which, in turn, led to higher ductility
(Fig. 8) (Cifuentes et al. 2012). Both effects (i.e., a light decrease
in maximum load and an increase in deflection) led to a higher
fracture energy [Fig. 6(d)]. At 500°C and 700°C, the trend of the
load-deflection curves was the same as at 300°C (Fig. 9). The main
difference was that the fibers were completely melted at that tem-
perature, so the damage level was higher (Fig. 5).
Regarding the D1 cold test [Fig. 6(d)] in comparison with the
D1 hot test, the maximum load increased at 100°C, as two effects
happened simultaneously: the effect of temperature on the cement
paste, improving its hydration (Cifuentes et al. 2012; Zhang and
Bicanic 2006), and the reduction in internal pressure because there
was more time for it to be released during the cooling process
(Zhang and Bicanic 2006). As a result, the fracture energy was
higher in the D1 cold test [Fig. 6(b)]. At higher temperatures
(300°C, 500°C, and 700°C), the pore level and microcracking in the
cement paste increased, owing to the heating process and the addi-
tional effect of the thermal gradient during cooling (Cifuentes et al.
2012; Tufail et al. 2017; Zhang and Bicanic 2006). A similar effect
was observed by Tufail et al. (2017) through the compressive
stress-strain curves after high temperature exposition.
The addition of longer fibers weakened the bearing capacity of
the material at room temperature and 100°C, as seen from the com-
parison between D1 and D2 in hot and cold tests [Figs. 6(b–d),
respectively]. At 300°C, when the fibers were partially melted,
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Fig. 8. Pore size distribution of D1 concrete.
Fig. 9. Load-deflection curves in D0 cold tests.
the network of channels in the matrix was larger, which entailed a
noticeable reduction in spalling. As a result, the peak loads in the
load-deflection curves were higher. At 500°C and 700°C, when the
fibers had completely melted, the damage level was similar in
D1 and D2.
Exposure time to a given temperature had no influence on the
fracture energy, because the core of the specimens reached the
target temperature in less than 6 h; hence, the thermal effects were
similar at the different exposure times (6, 24, and 48 h).
Compressive Strength
The compressive strength of all the mixes is shown in Fig. 10. The
effects of temperature, the cooling process, and exposure time on
specimens with different PP fiber lengths in hot and cold tests can
be analyzed from these results.
As shown in Figs. 10(a–c) (hot tests), a decrease-increase-
decrease trend was observed in all three concrete types (D0, D1,
and D2 mixes) at the three exposure times (6, 24, and 48 h). This
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behavior was similar to that reported in previous studies by Zhang
and Bicanic (2006). As regards D0 hot tests [Fig. 10(a)], when the
specimens were heated up to 100°C the compressive strength de-
creased, owing to vapor pressure in the concrete matrix (Cifuentes
et al. 2012; Zhang and Bicanic 2006). Between 100°C and 300°C,
the temperature affected the cement paste by improving its hydra-
tion, thus leading to an increase in the compressive strength. At
temperatures above 300°C, the matrix showed considerable micro-
cracking; as a result, the compressive strength decreased with the
increase in temperature.
In the D1 and D2 hot tests [Figs. 10(b and c)], in which the
specimens were reinforced with PP fibers (short and long fibers,
respectively), the results were qualitatively and quantitatively sim-
ilar to those obtained by the D0 [Fig. 10(a)]. The fibers did not
bring any improvement to the compressive mechanical properties
(Ramezanianpour et al. 2013). Moreover, the inclusion of fibers in
the matrix reduced the compressive strength at 700°C, when they
were completely melted.
Regarding the D0 cold tests [Fig. 10(d)], the evolution of the
results showed a decrease-increase-decrease trend, in keeping with
the findings of previous studies (Zhang and Bicanic 2006). At
100°C, the compressive strength was slightly greater than in the
hot tests because this temperature did not generate high vapor pres-
sure. At 300°C, the microcracking caused by the heating and cool-
ing processes prevented any increase in resistance, as was the case
in the hot tests [Fig. 10(a)], leading to a decrease in the compressive
strength (Nielsen and Bicanic 2003). At 500°C, the compressive
strength decreased because the damage sustained during the heat-
ing and cooling processes was more significant, due to the higher
temperature reached (Zhang and Bicanic 2006). At 700°C, the very
high temperature caused the decomposition process of the cement
paste (Cifuentes et al. 2012; Zhang and Bicanic 2006) along with
microcracking during the cooling process.
As for the PP fiber-reinforced specimens, that is, D1 and D2
[Fig. 10(d)], the compressive strength was similar to that of D0
at 100°C, although it decreased in some cases when the proportion
of fibers was very high, as shown in Fig. 10(d), due to the worm
effect of fibers, leading to more pores in the concrete matrix
(Ramezanianpour et al. 2013). At 300°C, the fibers were partially
melted, the fiber channels were not completely free, and vapor
discharge was consequently more difficult, generating spalling.
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Fig. 10. Evolution of compressive strength with temperature at each exposure time: (a) D0 hot tests; (b) D1 hot tests; (c) D2 hot tests; and (d) cold
tests.
Because of this, the concrete matrix sustained further damage, in
comparison with room temperature and the same mixes in hot tests.
At 500°C and 700°C, the fibers were melted, and the behavior was
similar to that observed in the D0 cold tests.
Exposure time to a given temperature had no influence on the
compressive strength, because the core of the specimens reached
the target temperature in less than 6 h; hence, the thermal effects
were similar at the different exposure times (6, 24, and 48 h).
Young’s Modulus
The hot and cold tests showed a decreasing trend from 25°C to
700°C, so rigidity always decreased. The decrease in Ec with tem-
perature in all mixes was due to the microcracking of the cement
paste caused by the heating procedure [in hot tests, Figs. 13(a–c)]
and the additional effect of the cooling process [in cold tests,
Fig. 11(d)] (Cifuentes et al. 2012). Compared with the hot tests,
the Young’s modulus of the material at 25°C (Cifuentes et al.
2013; Gencel et al. 2011) was improved by adding PP fibers
[Figs. 11(b and c)]. Nevertheless, there was a sharp drop of approx-
imately 50% at 100°C, which shows how the vapor pressure
quickly affected this property. However, from 100°C to 700°C
the evolution of Ec was less marked and almost linear (Cifuentes
et al. 2012; Tufail et al. 2017; Zhang and Bicanic 2006). As the
temperature rose, thermal microcracking took place, which entailed
a reduction in the rigidity of the concrete (Cifuentes et al. 2012).
The effect of the fibers was barely noticeable at temperatures below
500°C. The highest values were obtained by the PP fiber-reinforced
concrete.
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J. Mater. Civ. Eng., 2018, 30(11): 04018271
The effect of the PP fibers was only slightly noticeable, but it is
worth noting that both the D2 mixes (reinforced with long fibers)
and D1 mixes (reinforced with short fibers) achieved better results.
The reason for this is that the addition of PP fibers increases the
ductility of the material, and this effect is more noticeable when
the PP fibers are longer (Gencel et al. 2011). At higher tempera-
tures, internal vapor pressure is reduced by means of the canal con-
nections generated by the melting PP fibers, so that vapor pressure
can be more efficiently evacuated (Cifuentes et al. 2012).
Tensile Strength
The trend observed in the hot tests [Figs. 12(a–c)] responds to a
three-stage decrease-increase-decrease pattern, in accordance with
that proposed by Zhang and Bicanic (2006).
The effect of the PP fibers was not very noticeable on the split-
ting tensile strength [Figs. 12(b and c)] in the tests conducted at
25°C (Ramezanianpour et al. 2013). For all mixes in hot tests
(D0, D1, and D2), the tensile strength decreased when the mixes
reached 100°C, in keeping with the trend shown by the compressive
strength (Cifuentes et al. 2012; Zhang and Bicanic 2006). When the
temperature rose above 100°C, the tensile strength of concrete in-
creased because of the hydration effect caused by the temperature
on the cement paste. In fiber-reinforced mixes, a more noticeable
decrease took place between 500°C and 700°C due to dehydration,
the decomposition of the cement paste (Cifuentes et al. 2012;
Zhang and Bicanic 2006), and the melting of the fibers, which cre-
ated more voids in the concrete matrix than in the D0 mix (Bei and
Zhixiang 2016; Cifuentes et al. 2012; Sideris and Manita 2013).
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Fig. 11. Evolution of Young’s modulus with temperature at each exposure time: (a) D0 hot tests; (b) D1 hot tests; (c) D2 hot tests; and (d) cold tests.

Fig. 12. Evolution of splitting tensile strength with temperature at each exposure time: (a) D0 hot tests; (b) D1 hot tests; (c) D2 hot tests; and (d) cold tests.

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Fig. 13. Evolution of the characteristic length with temperature for each exposure time: (a) D0 hot tests; (b) D1 hot tests; (c) D2 hot tests; and
(d) cold tests.
The evolution of the results in the cold tests [Fig. 12(d)] showed
a decreasing trend, as in previous studies (Cifuentes et al. 2012;
Zhang and Bicanic 2006). The splitting tensile strength results
at 100°C were better than in the hot tests because vapor pressure
had more time to be evacuated during the cooling process. At
temperatures above 100°C, the concrete matrix, which was already
damaged by the previous heating process, showed a further increase
in internal damage due to the cooling process, which generated
more microcracks and propagated already existing ones (Zhang
and Bicanic 2006).
The effect of the PP fibers on the splitting tensile strength was
more noticeable than their effect on the residual compressive
strength, but the behavior was similar. The addition of PP fibers
to the concrete matrix created a worm effect that increased the num-
ber of pores. This effect was more remarkable when the amount of
fibers and their length increased. When concrete mixes reached
temperatures above 300°C, the fibers were partially or completely
melted, and the proportion of voids in the concrete matrix signifi-
cantly rose. As a result, the splitting tensile strength decreased. This
effect was more remarkable in mixes reinforced with longer fibers
[D2, Fig. 12(d)].
Characteristic Length
Characteristic length, lch , was assessed in both the hot and cold
mixes. This fracture parameter provides information about the in-
trinsic brittleness of the cohesive material (Hillerborg et al. 1976;
Rosselló et al. 2006). It is also directly related to the fracture
process zone (FPZ), although it does not indicate its exact length
[ACI Committee 446 (ACI 1991)]. Therefore, a material with
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J. Mater. Civ. Eng., 2018, 30(11): 04018271
higher characteristic length will also have a greater FPZ length
and thus a higher ductility (Bazant and Planas 1998).
Because all specimens were of the same size, there was no size
effect, and it was consequently possible to directly analyze the
ductility of the mixes by means of the characteristic length values.
The characteristic length is defined as
Ec G F
lch ¼ ð6Þ
f2t
where ft = tensile strength and was, in this case, considered equal
to the splitting tensile strength fti .
The hot tests [Figs. 13(a–c)] showed a decrease-increase trend,
in which the lowest point was reached at 300°C. If the temperature
rose to 300°C, this affected the cement paste, improving its hydra-
tion and leading to an increase in the splitting tensile strength
[Figs. 12(a–c)] (Cifuentes et al. 2012; Zhang and Bicanic 2006)
and a decrease in the characteristic length. From 500°C to 700°C,
the porosity level increased significantly, softening the material and
increasing its ductility. Postpeak softening significantly increased,
as shown in Figs. 7(c and d), which led to higher characteristic
length and FPZ values. In the PP fiber-reinforced hot mixes
[Figs. 13(b and c)], the characteristic length was higher than in non-
reinforced specimens [Fig. 13(a)], as this increased when the PP
fibers were partially or completely melted, resulting in a softer con-
crete matrix with higher ductility. However, this effect became
more noticeable at temperatures above 500°C, because the porosity
level was higher (Fig. 8).
In the cold tests [Fig. 13(d)], at 100°C the trend was similar to
that of the hot tests, but the lowest characteristic length values were
reached because the damage was sustained during the cooling
J. Mater. Civ. Eng.
 process. At 300°C, the matrix of cold mixes was more damaged
than that of hot tests at the same temperature. This led to a more
ductile material with a higher characteristic length. At temperatures
above 300°C, the level of damage in the matrix increased (Fig. 8),
and the PP fibers melted. The addition of fibers increased ductility
at any temperature, as in the hot tests; this effect was more notice-
able when longer fibers were used.
Conclusions
In this study, we explored the effects of temperature on the fracture
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behavior and other mechanical properties of high-strength polypro-
pylene fiber-reinforced self-compacting concrete, at a range of tem-
peratures up to 700°C and after cooling at three different exposure
times. The following conclusions are drawn from the results:
• The irreversible process of weight loss increases with higher
temperatures. This process involves dehydration of residual
moisture at low temperatures, dehydration of chemically bound
water at medium-high temperatures, and decarbonation of cal-
cium carbonate at higher temperatures.
• The addition of fibers creates a network of channels in the ma-
trix that reduces internal pressure damage and spalling effects.
However, it also reduces material strength at room temperature
due to the increased number of pores created by the trapped air.
• As long as they are not degraded, the fibers have a bridge effect
on the crack front that stitches any eventual microcracking. This
improves the strength properties and ductility of the concrete in
both hot and cold conditions.
• Longer fibers reduce the effects of spalling and create a greater
network of channels for the evaporation of internal pressure.
Yet, they also increase the number of voids in the matrix, which
in turn reduces its mechanical properties and causes a softening
of the material.
• The cooling process generates microcracking due to the thermal
gradient that is more noticeable from medium-high tempera-
tures, where this thermal gradient is more abrupt, and the fibers
are partially melted. These harmful effects add to those sus-
tained during the heating process.
• When the thermal gradient is more gradual, the cooling process
does not cause significant damage, and the fibers help to stitch
any microcracking. This leads to higher mechanical properties.
• Exposure time has no effect when the temperature is uniformly
reached in the entire matrix. From that point, the behavior of
concrete is the same regardless of the length of time the speci-
mens are exposed to the temperature.
Acknowledgments
The authors acknowledge the financial support provided to this
study by the Spanish Ministry of Economy and Competitiveness
under project BIA2016-75431-R.
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