Cement & Concrete Composites 48 (2014) 26–34

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Cement & Concrete Composites

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

Effects of elevated temperatures on the interface properties of carbon

textile-reinforced concrete
Flávio de Andrade Silva a,⇑, Marko Butler b, Simone Hempel b, Romildo Dias Toledo Filho a,
Viktor Mechtcherine b
a
Department of Civil Engineering, COPPE, Universidade Federal do Rio de Janeiro, P.O. Box 68506, CEP 21941-972 Rio de Janeiro, RJ, Brazil
b
Institute of Construction Materials, TU Dresden, 01062 Dresden, Germany

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

Article history: This work reports on an experimental investigation of the influence of elevated temperatures on the
Received 2 May 2013 interface between carbon yarns and a Portland cement based matrix. Polymer-coated and uncoated car-
Received in revised form 8 January 2014 bon yarns were tested at temperatures of 20 °C under a double-sided pullout test configuration after
Accepted 9 January 2014
being subjected to a heating regime at temperatures of 100, 150, 200, 400 and 600 °C. The degradation
Available online 24 January 2014
mechanisms of the cementitious matrix were investigated by X-ray diffraction and thermal analysis.
Using an environmental scanning electron microscope, micro-structural analysis was performed to eval-
Keywords:
uate the degradation of the carbon yarn and of its interface with the matrix. After preheating up to 150 °C,
Carbon fibre
Interface
samples with coated fibres showed significant increases in maximum pullout load and, correspondingly,
Textile reinforced concrete work to pullout. On a micro-scale this is related to a polymer interlocking mechanism in the yarn–matrix
Pullout interface, which is generated during the heating and cooling of the polymer yarn coating. Above 400 °C no
Temperature further typical fibre pullout behaviour was observed; the reinforcing yarn failed suddenly after the crack-
ing of the matrix. For uncoated yarn preheating up to 200 °C had no significant impact on the maximum
pullout load. At 600 °C the matrix and fibres showed major signs of deterioration; no further typical fibre
pullout behaviour other than failure of the reinforcing yarn could be observed.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction dimensional fabrics can also be tested under a pullout-loading con-

The correct understanding of the bonding behaviour of textiles
with cement-based matrices is an important step in comprehend-
ing the degrading mechanisms which a composite can suffer when
subjected to elevated temperatures. Different to conventional
reinforcement systems, the textiles are composed of yarns fabri-
cated using a large number of filaments. In the yarns themselves
the outer filaments in direct contact with the matrix show better
bond performance, while neighbouring inner yarns are activated
by friction [1]. When a coating is used, the filaments are stressed
more equally, resulting in more filaments taking part in the load-
bearing function [2].
To characterise fibre–matrix interface pullout, experimental
tests on yarns and filaments were performed in single [3–5] and
two-sided [6–8] configurations. Although two-sided pullout tests
are more complicated and time-consuming in their designing and
carrying out, they can predict material behaviour in a more
realistic way since the fibres bridge cracks during the test. Two-
⇑ Corresponding author. Tel.: +55 (21)2562 8493x48; fax: +55 (21)2562 8484.
E-mail address: fsilva@coc.ufrj.br (F. de Andrade Silva).
figuration [9,10]. Such tests take into account the fabric geometry
and also the intersection of warp and weft yarns; which give rise to
a further mechanical bond component.
Bonding properties of carbon-fibres at room temperatures have
already been investigated in the past. Katz et al. [11] performed
single-sided pullout tests in carbon filaments with two different
diameters: 10 and 46 lm. For the smaller fibre the bond strength
varied from 0.52 MPa, for a water-to-binder ratio of 0.50, to
1.29 MPa for a matrix with silica fume addition and w/b ratio of
0.35. Badanouiu and Holmgren [12] performed tests using carbon
yarns. The authors tried to improve bond by treating the surface
of the yarn with silane and also designing a matrix with polymer
and silica fume additions. The results showed an improvement of
the bonding properties of carbon fibres in matrices containing sil-
ica fume and high amounts of polymer. The silane treatment of the
fibres led to an increase in the average bond strength of 368% for
samples cured in air and by 140% for samples cured first in a fog
room. Scheffler et al. [13] showed that tailoring sizings and com-
patible coatings provide a basis to achieve highest carbon roving
performance in the concrete composite. In addition, a modification
of coatings by nanoclay enables to tailor the morphology of the

http://dx.doi.org/10.1016/j.cemconcomp.2014.01.007
0958-9465/Ó 2014 Elsevier Ltd. All rights reserved.
 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34
interfase and contributes to reduce crack widths at maximum force
by development of hydration products and thus enhancing the
interface stiffness of the composite.
The effect of high temperature on the ultimate tensile strength
(UTS) of pitch-based carbon fibres under a nitrogen atmosphere
seems not to be affected up to 1300 °C. Tanabe et al. [14] showed
that in a nitrogen atmosphere the carbon fibre UTS even increases
slightly from 1000 to 1300 °C. Sauder et al. [15] showed that for
PAN and rayon-based carbon fibres UTS increases slightly when
the temperature increases to 1600 °C. This phenomenon was re-
lated to a possible reduction in flaw severity associated with inter-
nal stress relaxation. When exposed to oxygen atmosphere the
carbon undergoes an oxidisation process and burning which starts
from 300 to 400 °C for uncoated carbon yarns and from 200 to
250 °C for polymer-coated yarns [16].
When exposed to high temperatures Portland-cement-based
concrete materials exhibit a loss in strength. Chen et al. [17]
showed that the residual compressive strength of high strength
concrete starts to decrease above 200 °C, yielding only 10% of its
original strength at 800 °C. This can be traced back to the calcium
hydroxide decomposition, which takes place between 370 and
470 °C, and of calcium carbonate and of other carbonates, occur-
ring between 600 and 730 °C. Drchalová et al. [18] performed
mechanical tests in PAN-carbon fibre reinforced cement based
composites after preheating the samples to temperatures up to
1000 °C. For the material with Portland-cement matrix a drop in
tensile strength from 4.86 to 3 MPa at 600 °C was noticed, which
was governed by the carbon fibre pullout from the cement matrix.
At higher temperatures this behaviour is dominated by the matrix.
Çavdar [19] demonstrated that carbon fibres as well as PP, glass,
and PVA are active in cement-based matrices under bending and
compressive loads only up to 450 °C.
In the present work the bond of polymer-coated and uncoated
PAN-based carbon yarns with a Portland-cement matrix was inves-
tigated for temperatures ranging from 20 to 600 °C. Double-sided
pullout tests were performed on the pre-heated and reference
specimens at room temperature (20 °C). Micro-structural analysis
using an environmental scanning electron microscope was carried
out to evaluate the degradation of the carbon fibre and of its inter-
face with the matrix. X-ray diffraction and thermal analysis were
used to quantify the degradation of the matrix when exposed to
the different temperatures.
2. Materials and processing
2.1. Carbon fibres
The carbon fibre was obtained from TohoTenax Europe GmbH.
The fibre used in the present study is the TohoTenax HTA (High
Tenacity Fibre) with a nominal fineness of 800 tex and density of
1.79 g/cm3. Table 1 presents the properties of coated and uncoated
carbon yarn and filament. The basic material used in the
Table 1
Fibre filament and yarn: physical and mechanical properties.
Properties Uncoated
Filament Yarn
*
Fineness (tex ) 0.067 803
Diameter (lm) 6.96 – –
Number of filaments – 12,000
Tensile strength (MPa) 3245 1032
Strain to failure (%) 1.46 0.58
Young’s modulus (GPa) 213.5 222.9
* Water
Mass in g of 1 km yarn or filament, respectively; (tex = g/km).
27
production of the carbon fibre was Acrylonitrile. In a first step,
using a catalytic process together with co-monomers and solvents,
a Polyacrylonitrile (PAN) fibre is spun to obtain the so-called chem-
ical precursor. In the second step the precursor is oxidised at tem-
peratures ranging from 250 °C to 300 °C in air, and subsequently
carbonated in nitrogen atmosphere at temperatures ranging from
1000 °C to 1500 °C to drive off non-carbon atoms. During this ther-
mal treatment the fibres are stretched in order to align the polymer
molecules, thus enhancing the mechanical parameters, i.e., tensile
strength and Young’s modulus. Before winding onto bobbins sev-
eral surface treatments are performed to improve the handling
quality and the chemical properties of the fibre surface. Because
the carbon fibre under investigation was not produced for use in
cementitious matrices, a subsequent polymer coating was applied.
This coating is an aqueous dispersion based on self-crosslinking
polymers. The polymer coating was applied as a suspension with a
polymer content of 30% by weight by means of two counter-rotat-
ing rollers with a contact pressure of 1.7 bar between the rollers.
The fresh polymer was dried and cross-linked by infra-red heating
at 160 °C for 1 min. The polymer film remained stable at tempera-
tures up to 200 °C. At temperatures in excess of this, the polymer
was decomposed stepwise up to 500 °C. The carbon fibre resisted
oxidation up to temperatures in the range of 550–600 °C.
2.2. Matrix and specimen preparation
In mixing the specimens for the pullout tests, a finely grained
matrix was used, which consisted of cement, fly ash, microsilica,
and quartz sand [20]. Table 2 summarises the matrix composition.
A superplasticizer with a basis of naphthalene-sulphonate was
added in order to achieve sufficient flowability. The average slump
flow value measured with a small cone (bottom diameter 100 mm,
top diameter 60 mm, height 70 mm) was 200 mm.
Doubly symmetrical, narrowed prisms with a notch depth of
1 mm were used as specimens (cf. Fig. 1). In the vicinity of the
notch each specimen was 5 mm thick, and at the ends the thick-
ness increased to 10 mm. The width of the samples was 50 mm.
Each specimen was reinforced with one multi-filament yarn ex-
tended over the entire length of the sample. Prior to concreting,
the reinforcing yarn was fixed on a stretching frame in order to
imbed it properly into the fine-grained concrete. After casting the
samples were demoulded at an age of two days and stored in water
(20 °C) until one day before testing. Afterwards the samples dried
for one day at a controlled lab temperature (20 °C). Steel plates
were then glued to the loading areas of the specimens and fixed
between the clamping jaws of the testing machine. In this way a
nearly unconstrained mounting of the specimens was possible.
3. Experimental testing procedure
The double-sided pullout tests were performed using coated
and uncoated multifilament yarns embedded in the fine-grained
matrix. Before testing, the specimens were heated up to 100,
150, 200, 400, and 600 °C and subsequently cooled to room tem-
perature (20 °C). Additional experiments on specimens stored at
Coated
Table 2
Yarn
Matrix composition [19].
903
Mix ingredients (kg/m3)
12,000 CEM I 32.5 R 557
2723 Fly ash 251
1.51 Microsilica suspension (50% powder by mass, 50% water by mass) 56
204.4 Sand 0–1 mm 1114
251
28 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34
Fig. 1. Dimensions of specimen and arrangements of load adapters and crack width
sensors for double-sided pullout test.
room temperature were carried out. The heating regime was
applied to the specimens at an age of 28 days subject to a heating
rate of 2 °C/min through the above-mentioned temperature
sequence. The temperature level was kept constant for 120 min,
followed by a natural cooling process.
The mechanical testing was conducted under a displacement-
control regime in a servo-hydraulic universal testing machine.
The displacement rate was set to 0.05 mm/min until the fine-
grained concrete matrix cracked at the notched cross-section.
The test displacement rate was then increased to 1 mm/min and
stopped when a crack opening of 2.5 mm had been reached. The
values of load, crack width, and displacement of the crosshead of
the testing machine were then measured and recorded. The mea-
surement of crack width was accomplished by means of precision
gauges fixed in the vicinity of the crack. Fig. 2 shows the test
arrangement.
After testing, the fibre and fibre–matrix interface were investi-
gated in an environmental scanning electron microscope (ESEM)
model XL30 (FEI Philips Company, Netherlands). For this purpose
the double sided pullout specimens were sectioned along the line
of the multi-filament yarn in samples of 10 mm length. The ESEM
was operated under a low vacuum. All the micrographs were taken
under the gaseous secondary electron (GSE) detector mode at
accelerating voltages of 20 and 30 kV and chamber pressure of
0.6–0.7 mBar. No coating with carbon or gold, as is usually done
for high vacuum SEM, was required.
Using X-ray diffraction (XRD) and thermo-gravimetrical
analysis (TGA), the matrix was investigated after having being sub-
jected to all temperatures under study. The XRD device used was a
Fig. 2. Clamped specimen instrumented with extensometers.
Theta-Theta powder diffractometer model XRD 3003 TT (Seifert
Company, Germany). For sample preparation the matrix material
was pulverised to particle sizes of less than 20 lm in a micro-mill,
which enables powder preparation without collapse of crystalline
structure of micro-grains. Hence the content of amorphous mate-
rial is practically capped in the pulverisation process. During
pulverisation the matrix material was immersed in isopropanol.
In order to enable a quantitative analysis of XRD data by means
of the Rietveld method, ZnO was added to the matrix material as
an internal standard, essential for quantification of amorphous
phases. Before deposition on the sample holder the isopropanol
was removed from the matrix-powder-isopropanol-suspension
by drying in air. The XRD measurement was performed in the 2
(theta) range from 20 to 70 °C.
For TGA analyses a STA409 (Netzsch Company, Germany) was
used. The sample mass of 60 mg was taken from the same powder
as prepared for XRD analysis. The sample was deposited on the
TGA crucible and heated from 20 to 1000 °C at a heating rate of
10 C°/min. During the heating process the loss in mass was noted
for both processes, i.e., dehydration, the collapse of the ettringite,
gypsum, CH, C–S–H, and deacidification, the collapse of the cal-
cium carbonate. The samples were subjected to testing conditions
in an Al2O3 crucible using 60 ml/min of helium as the purge gas.
4. Results and discussion
Fig. 3 presents schematically a complete load-deformation
curve as measured in the double-sided pullout tests. Three regions
of the graph can be distinguished according to the degree of spec-
imen deformation according to the theoretical background pre-
sented in [21]. Region 1 represents the straining of the uncracked
samples. It ends with the formation of a macro-crack in the
notched area of the specimen. In region 2 a sudden drop in force
from Fu to Fs occurs. Caused by the specimen’s under-critical fibre
content, the reinforcement cannot bear the imposed, relatively
high load Fu after matrix cracking. In region 2 the crack-bridging
mechanisms of the matrix, e.g., aggregate locking and crack
branching, occurs as well as the failure of sleeve yarn filaments
intensively bonded to the matrix.
In region 3 finally the typical pullout of crack-bridging, multifil-
ament yarn takes place. The single filaments are stretched in differ-
ent manners during crack opening, according to their bond
 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34
Fig. 3. Schematic view of a typical pullout curve [20].
characteristics within the yarn or to the matrix. The filaments fail
successively with increasing crack opening. Thus, at first, a rising of
pullout force up to Fmax can be noticed, followed by a softening and
leading to complete failure of the crack-bridging multifilament
yarn.
In Fig. 4 the representative pullout force vs. crack opening
curves for the uncoated yarn (Fig. 4a) as well as for the coated yarn
(Fig. 4b) are presented instead of the complete load-deformation
diagrams. Regions 1 and 2 of these curves are not displayed in or-
der to simplify their graphic representation. Only when region 2
could not be distinguished from region 3 due to the continuous
drop of the curve, e.g., in the case of the preheating up to 600 °C,
the graph was plotted starting with region 2. Each curve was se-
lected from a collection of up to 10 individual curves as that repre-
senting typical behaviour as accurately as possible.
To enable quantification and easy comparison from among the
test series, three distinct parameters were defined to characterise
the pullout curves, as is shown in Fig. 4: maximum fibre pullout
force Fmax and the work to fibre pullout, W0.3 and W0.6 at crack
widths of 0.3 and 0.6 mm, respectively (cf. Fig. 3). Whereas in
Fig. 4 only characteristic curves are represented, the parameters
Fmax, W0.3 and W0.6 are given for each measured curve so that the
scatter of the values obtained can be observed as well. The speci-
fied crack widths were chosen as they can be correlated with the
average Fmax. In Fig. 5 in the bottom graphs the maximum pullout
load of each individual curve is plotted vs. the maximum temper-
ature of preheating. In the top graphs for each individual test the
Fig. 4. Influence of temperature on the pullout resistance of carbon yarns from a cementitious matrix: (a) uncoated and (b) coated fibres; selected, representative curves are
shown.
29
pullout work to a crack opening of 0.3 mm as well as up to a crack
opening of 0.6 mm were indicated over the preheating tempera-
ture, respectively. The data for uncoated yarns were represented
in Fig. 5a and the data for coated yarns in Fig. 5b. In addition,
Table 3 gives the average values and the associated standard
deviations.
For uncoated yarn preheating up to 200 °C has no significant
impact on the maximum pullout load. The slightly higher pullout
load of the curve of the reference specimen (20 °C) as presented
in Fig. 4a is within the scattering of results (cf. Fig. 5a). However,
the stiffness of yarn pullout (ascending branch of curve, cf.
Fig. 4a) increases when the preheating temperature is increased
to 100 °C, but no further changes in stiffness can be observed when
the preheating temperature is increased from 100 °C to 200 °C.
While at larger crack openings the descending branches of the pull-
out curves become shallower with increasing temperature of the
preheating, the work to pullout W0.3 and W0.6 (at relatively low
crack openings) stays largely constant for the range of preheating
temperatures between 100 °C and 200 °C.
The first sign of deterioration in material behaviour in the
experiments with uncoated yarns could be observed at a preheat-
ing temperature of 400 °C. The inclination of the rising branch of
the pullout curve and the maximum pullout load were reduced.
On the other hand, the descending branch of pullout curve became
much shallower (cf. Fig. 4a). Again, due to the fact that the work to
pullout was calculated only for relatively small crack openings, this
phenomenon does not significantly affect the results of work to
pullout, W0.3 and W0.6, as represented in Fig. 5a. It must be noted,
however, that there is a tendency to drops in these values when
compared to samples subjected to preheating temperatures of
200 °C or less.
When preheating to 600 °C no further typical fibre pullout
behaviour could be recorded. After exceeding the tensile strength
of the concrete matrix, the samples failed catastrophically. The
minor crack-bridging action of the fibres could be neglected as
compared to the results at the other preheating temperatures.
After the pullout test was finished the half-parts of the speci-
mens were separated completely by fast moving-down the
hydraulic jaw of the testing machine so that the typical pullout
length could be measured with the help of a caliper. The pullout
length of the carbon multifilament yarn (Table 4) for preheating
up to 200 °C was found to be 100 mm. Preheating up to 400 °C re-
duced the pullout length to 42 mm due to yarn failure. After pre-
heating up to 600 °C only a characteristic length of 15 mm was left.
The degradation in the matrix due to exposure to elevated tem-
peratures was investigated by XRD and TGA. The results are shown
in Figs. 6 and 7, respectively. The XRD analysis shows that at
30 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34

Fig. 5. Influence of temperature on the maximum pullout force and on the pullout work of (a) uncoated and (b) coated carbon yarns.

Table 3
Summary of pullout test results performed on coated and uncoated carbon fibres (mean values); standard deviations in parentheses.

Temperature (°C) Uncoated fibres Coated fibres

Fmax (kN) W0.3 (J) W0.6 (J) Fmax (kN) W0.3 (J) W0.6 (J)
20 0.690 0.262 0.529 0.566 0.171 0.388
(0.109) (0.032) (0.083) (0.116) (0.021) (0.067)
100 0.675 0.268 0.511 0.726 0.196 0.445
(0.061) (0.024) (0.039) (0.195) (0.018) (0.055)
150 0.639 0.249 0.496 0.729 0.181 0.434
(0.155) (0.052) (0.106) (0.300) (0.039) (0.101)
200 0.640 0.245 0.496 0.534 0.154 0.363
(0.074) (0.021) (0.057) (0.110) (0.018) (0.050)
400 0.521 0.181 0.402 0.101 0.040 0.084
(0.069) (0.015) (0.039) (0.024) (0.012) (0.026)
600 0.028 0.023 0.028 0.050 0.036 0.042
(0.025) (0.006) (0.007) (0.022) (0.007) (0.010)

Table 4
Filament pullout lengths after yarn pullout test.

Temperature (°C) Uncoated fibres Coated fibres

Lmax (mm) Lmax (mm)
20 100 100
100 100 100
150 100 100
200 100 99
400 42 93
600 15 28

temperatures over 100 °C there were no traces of ettringite and

that for temperatures of 500 °C and 600 °C Portlandite was absent
from the matrix (Fig. 6). From TG analysis the results can be better
visualised in the TG derivative (DTG) by the peaks, which corre-
spond to the several steps of mass loss. It can be seen that between
35 and 200 °C the DTG peaks indicate a loss of combined water,
which comes initially from the calcium silicate hydrate (C–S–H)
and ettringite, cf. Fig. 7. At higher temperatures the dehydroxyla- Fig. 6. X-ray diffractogram of the cementitious matrix after being exposed to the
tion of the calcium hydroxide (CH) can be observed, which occurs various elevated temperatures.

between 370 and 470 °C, and finally between 600 and 730 °C, the
decomposition of calcium carbonate and other carbonates present
in the initial cement composition occurs due to the loss of CO2. It
can be seen that the amounts of ettringite and C–S–H gradually de-
crease with increasing temperatures up to 200 °C, and for temper-
atures of 500 °C and 600 °C the calcium hydroxide is degraded
from the matrix.
Based on the available data for the uncoated yarn pullout tests
and for the matrix decomposition with increasing temperature the
following conclusions can be drawn:
Up to the preheating temperature of 200 °C the bond behaviour
between carbon filaments and matrix is for all practical purposes
 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34
Fig. 7. Thermal analysis of the cement based matrix after exposure to the various
elevated temperatures.
unaffected by thermal processing. The collapse of the hydration
products at temperatures below 200 °C has no impact on the inter-
face performance.
Moreover, the mechanical properties of carbon-fibre are not
influenced. This is evidenced on the one hand by the mechanical
behaviour of the carbon yarn [14] and on the other hand by the fact
that the pullout length of filaments stays constant, while the pull-
out curves do not change their shape significantly.
As discussed, the further increase of preheating temperature to
400 °C leads to changes in pullout behaviour. At about 370 °C the
calcium hydroxide begins to collapse and is transformed to calcium
oxide (CaO). As well, the dehydration of C–S–H and ettringite
phases is intense at 400 °C, cf. Figs. 6 and 7. The impact of the
decomposition of these compounds on the morphology of the ma-
trix leads to a loosening of the interface and consequently to a
reduction of bond intensity between yarn and matrix.
In addition, a slight reduction in yarn strength [14] can be noted
as compared to its initial values. Furthermore, the reduction of
yarn strength becomes obvious through the reduction in pullout
lengths, cf. Table 4: due to the lower filament strength the proba-
bility of filament failure at lower stress levels increases, thus lead-
ing to the shorter pullout lengths.
After preheating up to 600 °C the calcium hydroxide collapse is
complete. Also a large portion of the C–S–H phases are dehydrated.
Therefore, the interface is essentially altered, becoming insufficient
for effective bonding to the yarn, and the loss of yarn strength is
very pronounced due to the oxidation of the carbon’s structure
[14]. The loss of filament strength is also demonstrated by the min-
imal pullout length of filaments (Table 4), which can be traced back
to the failure of filaments already at very low load levels. Finally, in
case of uncoated multifilament yarn both mechanisms, i.e., the in-
tense matrix dehydration and the degeneration of multifilament
yarn filaments above 400 °C govern the decay of the pullout
properties.
The samples with coated yarn showed different fibre–matrix
interface mechanisms. Here the preheating up to 150 °C led to a
significant increase in the maximum pullout load and correspond-
ing crack opening (Figs. 4b and 5b). Due to the smaller amount of
stiffening in the rising branches of pullout vs. crack opening curves,
the work to pullout W0.3 and W0.6 for preheating up to 100 or
150 °C rises only slightly. It must be emphasised that the work to
pullout for larger crack openings, those above 0.6 mm, is consider-
31
ably higher for the specimens subjected to temperatures up to
150 °C.
At preheating up to 200 °C a clear drop of pullout performance
back to the same observed in the reference specimen (20 °C) can be
seen. Only at larger crack openings, above 0.6 mm, can a higher
crack-bridging load transfer by means of the yarn be noticed. Thus,
the maximum pullout force, Fmax, as well as the work to pullout
W0.3 and W0.6 decrease to the reference level (Fig. 5b).
Preheating to 400 °C leads to a nearly complete loss of crack
bridging ability in the multifilament yarn. The pullout curve shows
only a slight rise up to a mean pullout load of approximately 100 N
(cf. Fig. 4b, Table 3); afterwards steady yarn pullout at low load lev-
els takes place (Fig. 4b). After the preheating up to 600 °C specimen
behaviour is the same as in the case of uncoated yarn, i.e., after
exceeding the tensile strength of concrete matrix the samples fail
suddenly.
The observed pullout length of the carbon multifilament yarn
when pre-heated up to 200 °C (see Table 4) was 100 mm. Only a
slight reduction of the mean value of the pullout length could be
noticed after preheating up to 400 °C. Preheating to 600 °C causes
a pronounced failure of the yarn leading to an average pullout
length of 28 mm.
In contrast to the samples reinforced with uncoated yarns, here
chiefly the coating of yarn governs the bonding behaviour between
yarn and matrix. For the range of preheating temperatures of
100 °C and 150 °C the pronounced increase in the maximum pull-
out force and corresponding crack opening and therefore the total
pullout energy might be related to the mechanisms described as
follows:
At a temperature of approximately 100 °C the glass transition
temperature of the yarn coating made of the copolymer styrol–
butadiene is reached. At this temperature the mechanical behav-
iour of the coating transforms from visco-elastic to plastic. At the
same time a thermally induced volume expansion of the copoly-
mer takes place. The volume expansion of copolymer generates a
hydrostatic pressure on the plasticized polymer, thus pushing it
into small pores of the surrounding cementitious matrix. When
cooling the sample to the room temperature, the copolymer be-
comes stiffer and visco-elastic again. This volume reduction now
generates tensile stresses inside the polymer. But a complete
retraction of copolymer from the small pores is not possible due
to the adhesive forces between the polymer and the hydration
product surfaces in the matrix. Hence, the re-stiffened polymer be-
comes stretched and some of the newly generated polymer inter-
locks may fail. However, the predominant portion most likely
remains intact, in this fashion forming effective cross links be-
tween the matrix and the coated multifilament yarn.
These mechanisms of matrix–polymer interlocking enable a
high-performing bond between filaments and matrix and conse-
quently cause the high pullout maximum loads and energy
absorptions.
The slight steepening of the rising branch of the fibre pullout
curves can be attributed to the same mechanisms. Since there is
no change in the visco-elastic material properties of re-cooled
coating copolymer, only the improved mechanical interlocking
can be the reason for these changes.
Regarding yarn strength, preheating up to 150 °C had no impact
on coated yarn. The pullout lengths corresponded to the embedded
yarn length. Thus, yarn strength was sufficiently high to bear the
crack bridging forces imposed by the improved matrix–filament
bond.
Due to the preheating up to 200 °C the first thermo-chemical
degradation was observable in the copolymer. During heating the
same processes of softening and expansion of coating occur, but
when exceeding a temperature of 150 °C, some degradation in
the polymer begins.
32 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34

However, the damage to the coating is not very pronounced in polymer films. If compared to the reference (cf. Fig. 9a), the poly-
this temperature range. So, a drop-back limited to the performance mer films on the fibre surfaces are morphologically modified. On
level of the reference specimens takes place. Damage to the yarn the other hand, for uncoated fibres subjected to the same regime
cannot be noted yet; see Table 4. a typical interface is observed with C–S–H and CH crystals and par-
Further preheating up to 400 °C causes the nearly complete tially hydrated fly ash, cf. Fig. 10. As a result of the preheating up to
thermal destruction of the polymer. Now the yarn lies inside its
matrix channel without effective cross links to the matrix, since
the former cross-linking coating has disappeared. Consequently,
effective load transfer is impossible. Corresponding to the findings
on uncoated yarn at this temperature level an initial, slight degen-
eration in the mechanical yarn properties could be observed. But
here its impact on the characteristic pullout length of the filaments
(cf. Table 4) can be neglected since nearly no load can be trans-
ferred from the matrix to the weakened filaments.
A micro-structural investigation using the ESEM was carried out
to confirm the mechanisms discussed above. Fig. 8 shows a strand
of coated carbon yarn in its natural condition and after exposure to
temperatures of 150 °C and 200 °C, respectively. It can be seen that
the styrol–butadiene copolymer coating starts to melt after 150 °C,
which changes interface characteristics.
The fibre–matrix interface micrographs are depicted in Fig. 9 for
the natural condition and the preheating temperatures of 150, 200
and 400 °C. In the specimens pre-heated up-to 150 °C there takes
place a polymer interlocking mechanism which can be observed
by a pronounced merging of polymer towards the matrix, cf. Fig. 10. Uncoated carbon-fibre–matrix interface after exposure to a temperature of
150 °C.
Fig. 9b. The matrix constituents seem now to be coated by thin

Fig. 8. Carbon fibre (a) in its natural condition and (b) after exposure to 150 °C and (c) 200 °C.

Fig. 9. Coated carbon-fibre–matrix interface: (a) in its natural condition and (b) after exposure to temperatures of (b) 150 °C, (c) 200 °C and (d) 400 °C.
 F. de Andrade Silva et al. / Cement & Concrete Composites 48 (2014) 26–34
Fig. 11. Carbon-fibre–matrix interface after exposure to a temperature of 600 °C: (a) uncoated and (b) coated carbon yarns.
200 °C the amount of coating of fibre surface and matrix is reduced
in comparison to the specimens pre-heated up to 150 °C. In the
gaps between fibres, polymer is still present. However, on free fibre
surfaces and ‘‘elevated’’ matrix areas the polymer is largely re-
moved by pyrolysis. At 400 °C no polymer coating is present any-
more. The filaments remain without bonding particles in
excavations vacated by the polymer. Indeed the matrix seems to
be free of the polymer.
After preheating up to 600 °C the same mechanisms as for
specimens with uncoated yarn take place since the coating is
completely removed by pyrolysis. The matrix becomes damaged
due to dehydration of the CH and C–S–H, hence affecting the
chemical bond with the fibre. The yarn strength is impacted
by the heating as well, as evidenced by the pullout length
(Table 4).
Fig. 11 shows ESEM micrographs of the uncoated and coated
carbon-fibre–matrix interface after being subjected to a tempera-
ture regime of 600 °C. It can be noticed that for uncoated fibres
the interface is degenerated with no signs of calcium hydroxide
and C–S–H. Furthermore, the fibres are now oxidised. The coated
fibres appear very similar: a complete destruction of the interface,
pronounced damage to the fibres, and cracked masses of the
matrix.
5. Conclusions
The following conclusions can be drawn from the present work
on the interface properties of carbon textile reinforced concrete ex-
posed to different temperatures before testing at room
temperature:
– For uncoated yarn interfaces preheating up to 200 °C has no sig-
nificant impact on the maximum pullout load, while the
ascending branch of the force-crack opening curve after matrix
cracking at elevated temperatures up to this temperature level
is steeper in comparison to room temperature. No signs of fibre
and matrix degradation were noticed.
– The first pronounced indications of material degradation could
be observed upon heating the specimens up to a temperature
of 400 °C. At this temperature the calcium hydroxide begins to
oxidise and is transformed to calcium oxide. Also the dehydra-
tion of C–S–H and ettringite phases are already in progress. The
changes in matrix morphology lead to a loosening of the inter-
face, while during dehydration the hydrate phases change their
mechanical properties, the shape of the matrix, and the yarn–
matrix interface.
– After heating the specimens up to 600 °C and subsequently
cooling them, the matrix and fibres showed major signs of deg-
radation, and no typical fibre pullout behaviour could be
recorded due to the failure of the reinforcing yarn immediately
after the cracking of the matrix.
33
– For samples with polymer-coated yarns, the coating strongly
affects the bonding properties at certain temperatures. After
preheating up to 150 °C significant increases in the maximum
pullout load and the corresponding crack opening were
observed. This was traced back to a matrix-polymer interlock-
ing mechanism of molten and re-stiffened polymer, which
formed a high-performing bond between filaments and matrix.
– After preheating up to 200 °C a clear drop in pullout perfor-
mance back to the same level was observed for the reference
specimen (20 °C). Preheating up to 400 °C led to the polymer
coating’s thermal decomposition, which subsequently resulted
in a nearly complete loss of the crack bridging ability of the
multifilament yarn.
– After preheating up to 600 °C specimen behaviour was the same
as in the case of the specimen with the uncoated yarn: after
exceeding the tensile strength of the matrix the samples failed
suddenly due to the failure of the reinforcing yarn.
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