Construction and Building Materials 253 (2020) 119029

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Construction and Building Materials

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

Influence of graphite nano/micro platelets on the residual performance

of high strength concrete exposed to elevated temperature
Hafiz Waheed Iqbal a, Rao Arsalan Khushnood a,b,⇑, Waqas Latif Baloch c, Adnan Nawaz d, Rana Faisal Tufail d
a
NUST Institute of Civil Engineering (NICE), School of Civil and Environmental Engineering (SCEE), National University of Sciences and Technology (NUST), Sector H-12,
Islamabad 44000, Pakistan
b
Department of Structural, Geotechnical and Building Engineering, Politecnico di Torino, Corso Duca degli Abruzzi, 24, 10129 Turin, Italy
c
Civil Engineering Department, Ryerson University, Toronto, Ontario M5B 2K3, Canada
d
Department of Civil Engineering, COMSATS University Islamabad, Wah Campus, Pakistan

h i g h l i g h t s

High temperature mechanical, durability and fracture properties of GNMPs reinforced concrete are presented.

Properties of the modified matrices show promise.

Microstructural study showed adequate dispersion of GNMPs in cement paste matrix.

Energy absorption capacity of modified matrices improved manifolds, which helps mitigate spalling.

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

Article history: An experimental program was designed to investigate the residual properties of high strength concrete
Received 25 October 2019 (HSC) modified with different percentages of graphite nano/micro platelets (GNMPs) after exposure to
Received in revised form 25 March 2020 elevated temperature. Mechanical properties such as compressive and tensile strength, stress–strain
Accepted 5 April 2020
response, elastic modulus and mass loss have been studied at elevated temperature in 23–800 °C range.
Non-destructive testing technique such as ultrasonic pulse velocity (UPV) was used to investigate the
quality of concrete in the post fire exposure. Further, the energy dissipation characteristics have also been
Keywords:
observed in detail. Scanning electron microscopy (SEM) was used for the study of morphological changes
High strength concrete
Elevated temperature nano/micro modified
such as crack formation, microstructural damage and the dispersions of GNMPs. Results showed better
concrete retention of mechanical and physical properties of high strength concretes containing GNMPs. Data
Graphite nano/micro platelets obtained was utilized to formulate mathematical relationships for expressing mechanical, durability
Post fire resilience and energy related properties of HSC modified with different percentages of GNMPs as a function of
Compressive strength temperature.
Compressive toughness Ó 2020 Elsevier Ltd. All rights reserved.
Microstructure
Spalling

1. Introduction Modernized infrastructures pose more challenges to concrete tech-

nology, which further contribute towards favorable circumstances
Concrete is regarded as one of the most broadly used construc- for analysis and improvement of advanced and useful concrete sys-
tion materials in the world because of the fact that it has a large tems. There is a growing need for the advancement of materials
number of resources, high adaptability and matured processes having improved features to satisfy advanced needs.
for production. With an appropriate combination of ingredients, In the past few decades, supplementary cementitious materials
different types of concrete are produced for various purposes. (SCMs) such as ground granulated blast furnace slag (GGBFS), silica
However, with the expansion of modernized concrete structures, fume (SF) and fly ash (FA) have been extensively studied to develop
conventional concrete technology is not enough to comply with hybrid concrete systems. These materials improve interfacial tran-
the needs of infrastructures with multidimensional roles. sition zones (ITZ) between mortar and aggregates and help attain
dense microstructures, which is reflected by enhanced mechanical
⇑ Corresponding author. properties. However, these densely packed matrices behave con-
E-mail addresses: [email protected], [email protected]. trarily and spall if exposed to elevated temperatures [1]. Spalling
pk (R.A. Khushnood). occurs due to the sudden cracking in matrix owing to the lack of

https://doi.org/10.1016/j.conbuildmat.2020.119029
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

dissipation of pore pressure [2], development of thermal inertia [3] of nano-particles. GNPs increase the thermal conductivity of
or concentration of thermal stresses [2]. Behnood and Masoud [4] cement matrix as reported by Xia Cui et al. [14]. The researchers
studied the use of polypropylene fibers (PP) to mitigate spalling. PP used 0%, 1% and 5% by volume of GNPs in cementitious composites
fibers being thermally unstable, fuse at around 200 °C and provide and results indicated that the incorporation of GNPs increases the
pockets of space for vapor pressure to dissipate. However, the pres- thermal characteristics of cementitious mixtures with a maximum
ence of these pores in turn causes durability issues [5]. Use of fibers rise of 75%. Similar intuition has been developed by Kalaitzidou
such as steel [6] and basalt [7] to reduce cracking have also been et al. [22], as the researcher studied the effect of GNPs inclusion
explored. These fibers bridge across the cracks by providing on reinforced polymer composites containing GNPs and concluded
anchorage and help to retain the effective load bearing area. How- that composites exhibited higher thermal conductivities.
ever, issues arise with the proper bonding of these fibers in cement There is little research available on the investigations of carbon-
matrix [8] and the overall cost [9]. The cementitious materials are based media integrated into the concrete exposed to fire and its
usually quasi-brittle, thus are sensitive to cracking and contain no only limited till 1-d elements [10]. There isn’t any published data
functional characteristics. Nanotechnology is being introduced in on performance evaluation of such 2-d nano-carbon elements
the cementitious materials to resolve the aforementioned issues. added into concrete matrices at elevated temperatures which are
The carbonaceous nano materials (NCMs) such as carbon nano tubes believed to develop better interfacial contact with the host matrix.
(CNTs), carbon nano-fibers (CNFs), and graphite nano-platelets Therefore, to bridge in this research gap an effort has been made to
(GNPs) have shown the capacity to improve the mechanical, func- explore fire endurance of concrete reinforced with 2-d plates of
tional and durability properties of the cementitious materials at graphite.
ambient conditions [10,11]. Waqas et al. [10,12] have reported This strong interfacial locking adds into energy absorbing
the use of multiwalled carbon nanotubes (MWCNTs) to develop capacity of the nano-modified samples which characterizes their
fire enduring concrete. The authors suggested that the use of these ability to resist fracture and sustain inelastic deformations without
nano-scale reinforcements not only catered for thermal cracking substantial decrease in the load carrying capacity at elevated tem-
but also reduced the thermal inertia. The reduction of thermal peratures. This improvement can be of much advantage in extenu-
inertia and uniform scattering of thermal stresses was because of ating the fire induced spalling in reinforced concrete members that
the highly thermal conductive nature of the nanotubes. Though a are highly susceptible to fire such as columns and shear walls. The
lot of research is available on CNTs and CNFs and the fire behavior recent research is an effort to explore the said research gap.
of the cementing matrices containing these nano-materials. How- The aforementioned studies indicate that GNPs not only
ever, the study on graphite nano-platelets (GNPs) in conjunction improve the mechanical properties but also add in the thermal
with cement matrices exposed to elevated temperature is scarce conductivity aspect. This increment in thermal conductivity can
in technical literature. help to scatter the thermal stresses and can also help to reduce
GNPs are tiny sacks consisting of graphene layers having the thermal inertia which is found to have detrimental effects on
thickness of commonly between 0.34 and 100 nano-meters [13]. concrete structures subjected to fire [14]. Insightfully, the use of
Graphene comprises of hexagonal plane made up of single car- GNPs can improve fire endurance. However, till date, no safe statis-
bon–carbon layer and is usually named as a ‘‘sub structure unit” tics are available about the properties of such modified cementi-
[14]. Thus, the structures of GNPs consist of a structure resembling tious matrices under fire exposure. To predict the elevated
a net, which is made up of multilayer carbon–carbon hexagonal temperature properties, an elaborated experimental data and ana-
plane and graphene is a specialized illustration of GNPs that lytical design has been established. This study provides mechani-
contains only a single layer of carbon atoms. As a result, the char- cal, durability, physical and microstructural properties of high
acteristics of GNPs are regarded as nearly close to graphene. strength concrete modified with various proportions of graphite
Mechanical, durability, electrical and thermal properties of nano/micro platelets (GNMPs) to the target temperatures of
GNPs have been studied in detail and many researchers have con- 800 °C, reflected in literature as ambient to replicate the fire
cluded that GNPs helped to develop multifunctional matrix having [23,24]. Residual behavior has been studied, which is quite often
excellent structural performances, serviceability, reliability and used in fire testing and majority of elevated temperature testing
high durability [15,16]. Like other carbonaceous nano materials, data is based on this approach [12].
GNPs contain high thermal and electrical conductivities with
improved mechanical properties [17,18]. However, compared to
2. Experimental investigation
CNTs (8$/gram), GNPs (2$/kg) have lower unit cost [9]. Studies
have shown improved interfacial bonding of GNPs with cement
2.1. Materials
mixture [19]. Blocking and diversion of cracks at micro and nano
level due to the plated structure, and delaying of cracks initiation
Ordinary Portland cement (OPC) Type-I in compliance with
due to their bridging capability have also been reported [19,20].
ASTM C150 was used in the preparation of investigated concrete
Compared to other nano-particles, GNPs are easy to disperse in
cement matrix which improves the properties of incumbent matrix
manifolds, such insights were shared by Bansal et al. [21]. They Table 1
used 5% wt. of GNPs and concluded that GNPs increased not only Chemical and physical properties of OPC.
the mechanical properties but also reduced the porosity. At 1.5% Chemical configuration Content Physical properties Content
wt. of GNPs, the flexure strength and flexural modulus increased (oxides) (%)
by 27% and 68%, respectively, as compared to the controlled mix Calcium Oxide 64.83 Insoluble residue 0.46
owing to adequate dispersion of GNPs [17]. Thus, GNPs are an (% mass)
excellent alternative to other nano-materials that are not only Silicon Dioxide 19.81 Specific gravity (g/cm3) 3.15
expensive but are difficult to disperse in cement. Aluminum Oxide 5.96 Specific surface area 8400
(cm2/g)
A study by Weina and Kamal [19] concluded the impact of GNPs Ferric Oxide 4.45 Particle size (d50) (um) 16.59
on ultrahigh strength concrete and stated that 56% increase in flex- Magnesium Oxide 1.95 Loss on ignition 1.76
ural strength and 187% energy absorption increase was attained (% mass)
compared with the controlled samples. Both studies concluded Sulphur Trioxide 1.31
Na2O + K2O 1.2
that the improvement was due to crack blocking and filler effect
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 3

formulations [25]. Table 1 represents the physical and chemical Table 3

properties of OPC. The summarized oxide composition in Table 1 Physical and chemical properties of silica fume.

is experimentally attained via X-Ray Fluorescence (XRF) technique. Properties Value

Sand was used as fine aggregate. The natural crushed aggre- Specific gravity 2.1
gates of maximum size of 12.5 mm were used as coarse aggregate. Mean grain size (nm) 140
Table 2 summarizes the physical properties of fine and coarse Specific surface area cm2 /gm 150000–300000
aggregates. Color Light to Dark Grey
Silicon dioxide (SiO2 %) 84
Silica fume was used for improving the properties of concrete Aluminium oxide (Al2O3 %) 1.14
and to attain high strength as per ACI 363R-10. Table 3 shows Calcium oxide (CaO %) 0.18–0.78
the physical and chemical properties of Silica Fume. The physical Sodium oxide (Na2O %) 0.6–1.1
characterization was done using BET Analyzer and Laser Granu- Magnesium oxide (MgO %) 0.18–0.78
Iron oxide (Fe2O3 %) 1.45
lometry while the oxides were measured via X-Ray Florescence
Potassium oxide (K2O) 0.6–1.1
technique. Graphite nano/micro platelets (GNMPs) were commer-
cially procured. Physical and morphological investigations were
performed using particle size analysis (PSA) and field emission
scanning electron microscopy (FESEM) techniques, respectively.
PSA shown in Fig. 1(a) indicates GNMPs size ranging from
2.3. Mixture proportions and specimen preparation
0.29 mm to 22.79 mm with a median size (D50) of 5.5 mm. Fig. 1(b)
indicates predominantly irregular shaped GNMPs particles. Fig. 1
A control high strength concrete (HSC) formulation and three
(c) shows the particle size distribution of silica fume. Fig. 1(d) indi-
modified formulations of high strength concrete containing GNMPs
cates rounded shaped silica fume particles. Table 4 shows the
of 0.1% (0.1GNMPs), 0.3% (0.3GNMPs) and 0.5% (0.5GNMPs) were
physical properties of raw graphite and acacia gum. The chemical
prepared using water to cement ratio of 0.27. The quantity of water
composition of GNMPs shown in Table 5 is experimentally attained
absorbed by GNMPs was compensated in the formulated mix pro-
via X-Ray Fluorescence (XRF) technique. The results shown in
portions. Third generation super-plasticizer (Sika viscocrete-3110)
Table 5 evident the heavy carbon concentration of around
1% by weight of cement was used to adjust the workability of con-
90.18%. Acacia gum was used as surfactant to disperse GNMPs as
crete mixes to 100 mm. Cylindrical specimens (100x200mm) were
it has been reported much effective for the purpose [12]. The ele-
prepared and de-molded after 24 h of casting. For curing, speci-
mental composition of Acacia gum is also shown in Table 6 as
mens were placed in controlled conditions as specified in ASTM
attained via EDX spectra.
C192 (23 °C ± 2 °C, 95% humidity) [27]. Table 7 shows the mix
design detail and the strength development of analyzed
2.2. Dispersion and characterization of GNMPs
formulations.
Various researchers have used different percentages of
GNMPs in composites such as cement paste and ultra-high- 2.4. Test equipment and procedure
performance concretes [14,16]. From previous research, it is con-
cluded that for mechanical enhancement, optimum dosage of An electric furnace, having temperature simulation capacity up
GNPs is 0.5% as that of binder. Nano/micro platelets consisting to 1100 °C, was used to expose the specimens to extreme high tem-
of graphite get closely packed, and resist dispersion into the peratures. Electric furnace was assembled with temperature con-
cementitious matrix because of Van der Waals forces. Thus, for troller for adjustment of heat rate and hold time. After exposure,
homogeneous dispersion of GNMPs, a chemical or mineral sur- specimens were tested in conformance with the ASTM C39 [28]
factant aided with mechanical sonication is usually adopted to obtain compressive strength values using a load controlled uni-
[19,26]. In this study, Acacia gum (AG) was used as the surfac- versal testing machine of 1000 kN capacity. Controlled compres-
tant. It weakens the Van der Waals forces and helps to disperse sive load of 0.2 MPa/second was applied to record the
nano-particles, as indicated by Waqas et al. [10]. GNMPs were mechanical response in compression. ASTM C469 testing proce-
diffused by using the surfactant-ultrasonic technique. Prior to dure [29] was adopted to compute modulus of elasticity from
the use of sonication, ultraviolet–visible (UV–Vis) spectroscopy stress-strain curves. For splitting tensile strength, the samples
was employed to identify the absorbance values of prepared were diametrically tested according to ASTM C496 procedure
aqueous suspensions at 500 nm (nm) wavelength, which [30]. The targeted temperatures for investigations were selected
remains least affected at the ambient settings [10]. Optimum as 100, 200, 400, 600 and 800 °C including the ambient one of
surfactant to GNMPs ratio was explored via successive disper- 23 °C. RILEM test procedures were adopted for hold time and heat-
sions of GNMPs to GA suspensions varying from 0.2 to 1 at ing rate [31]. Lower thermal conductivity of concrete requires at
the constant interval. Results revealed that the surfactant to least a hold time of 2 h to reach thermal steady state conditions
GNMPs ratio of 0.6:1 is optimum to attain homogeneous suspen- [10,32]. Thus, for all the selected temperatures, a hold time of
sions aided with mechanical sonication of 45 min, as given in 2 h and 30 min was practiced. An average heating rate of 5 °C/min-
Fig. 2. ute was adopted to achieve the set targeted temperatures
[10,32,33]. The specimens were allowed to cool down to ambient
temperature after provision of hold time. The weight of the speci-
men was measured before and after heat exposure to determine
Table 2
Physical properties of fine and coarse aggregates.
relative mass loss during the fire phase. Ultrasonic pulse velocity
(UPV) test was also performed before and after the heat treatment
Aggregate type Coarse aggregates Fine aggregates
to qualitatively assess the internal structure damage.
Maximum size (mm) 12.5 –
Specific gravity (g/cm3) 2.58 2.64
Water absorption (%) 1 1.59 3. Results and discussion
Bulk density (kg/m3) 1564 1550
Crushing value 21 – Results of mechanical and durability tests such as compressive
Fineness modulus 2.76 2.18
and tensile strength, stress–strain response, compressive
4 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

Fig. 1. a) PSA of Graphite, b) FESEM of Graphite, c) Particle size distribution of Silica Fume, d) FESEM of Silica Fume.

Table 6
Table 4 Elemental detail of acacia gum.
Physical properties of raw graphite and Acacia gum.
Element Acacia Gum
Property Raw graphite Acacia gum Weight% Atomic%
Density 2.23 g/cm3 1.4 g/cm3 C 66.81 73.70
Specific gravity 1.9 1.35 O 31.01 25.69
Surface area 24 m2/g – Na 0.24 0.14
Color Steel grey to black – K 0.20 0.07
Luster Metallic – Ca 0.84 0.28
Si – –
Mo 0.90 0.12
Total 100 100

Table 5
Chemical composition detail of raw
graphite. 3.1. Visual assessment and spalling of concrete after exposure to high
Chemical configuration Weight% temperature
C 90.18
O 5.84 Visual assessment is the first tool to access the serviceability
Ca 1.5 and condition of a fire damaged structure. Cracking and spalling
Fe 1.64 can be observed by visual inspection of the specimens. Visual
Mg 0.41 assessments of heated specimens were performed to examine
Si 0.23
any changes of color, crazing, or cracking patterns for assessing
Al 0.2
Total 100 the serviceability of concrete after being exposed to fire, as shown
in Fig. 3. The color of a fire damaged concrete sample serves for the
comprehensive concept regarding temperature to which it has
been exposed. Loss of water, dehydration of paste and microstruc-
ture disintegration at high temperature are the major causes of
toughness, elastic modulus, mass loss and ultrasonic pulse velocity crazing and thermal cracking in concrete [32].
test under residual conditions have been analyzed for high The visual analysis of reference HSC samples revealed no con-
strength concrete with and without nano/micro modifiers. siderable change in color till 400 °C. Although, above 600 °C,
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 5

homogeneous distribution, adequate quantity and high thermal

conductivity [14,15,26].

3.2. Compressive strength

Fig. 4 shows the values of absolute and relative compressive

strengths. It was analyzed that each type of concrete lost its stabil-
ity when the exposed temperature was increased from 23 °C to
800 °C. The indicated reduction in compressive strength is due to
the change in physical and chemical compositions upon heating.
At 200 °C, the loss of free and absorbed water causes hydrothermal
changes and leads to the strength reduction due to internal micro-
cracking [33,35]. Thermal expansion of aggregates at 300 °C leads
to microcracking and internal stresses [36–38]. Above 400 °C, cal-
cium hydroxide (CH) which forms a major portion in the hydrated
products of concrete starts to disintegrate [39–42]. At 600 °C,
calcium silicate hydrate (CSH) gel decomposes which results in
significant strength reduction accompanied with loss of stiffness
[39–41,43]. Above 600 °C, major cause of strength degradation is
Fig. 2. UV–Vis Spectroscopy of Acacia Gum with Graphite nano/micro platelets. the instability of aggregates. As de-carbonation of calcium carbon-
ate (CaCO3) occurs in the ranges of 600–800 °C, resulting in the
dissociation of limestone and subsequent loss in strength [23,35].
change of color from greyish to light grey color was observed. From Fig. 4, it could be found that compressive strength of mod-
However, GNMPs showed a peculiar color behavior. 0.1GNMPs ified mixes increased by 20%, 28% and 24% by adding 0.1%, 0.3% and
showed dark grey color at 23 °C. At 400 °C, the color was trans- 0.5% GNMPs, respectively, compared with HSC mix at ambient
formed to grey, while it turned to light grey at 600 °C. 0.3GNMPs temperature. This increment of the compressive strength could
color was greyish black at 23 °C. At 400 °C, the color transformed be due to the filler effect of these particles, that refines the
to grey and then to light grey after exposure to 600 °C. 0.5GNMPs microstructure, and tend to increase the degree of cement hydra-
color was light-black in ambient, later turned into greyish black at tion as well [16,19]. It was observed from the data of performed
200 °C and then turned into grey at 600 °C. tests that concrete having graphite nano/micro platelets exhibited
In all the concrete types, no significant cracking and crazing was comparatively lower reduction of the compressive strength
observed till 200 °C. At 400 °C, surface cracks were developed in all throughout the heating phase of 100–800 °C. At 100 °C, relative
the investigated formulations, but these cracks were relatively compressive strength loss for all samples followed the same trend.
wider in HSC as compared to GNMPs mix. After exposure to However, the strength loss above 200 °C becomes more noticeable.
600 °C, intensive cracking of surface and crazing was noticed in ref- 0.3GNMPs concrete performed better as compared to HSC and
erence as well as in the GNMPs reinforced concrete formulations. other modified formulations. The strength loss in 0.3GNMPs con-
Fire induced explosive spalling was observed in HSC concrete sam- crete at 100, 200, 400 and 600 °C was 6%, 13%, 36% and 57%, respec-
ples when temperature reached around 650 °C, while the spalling tively, while in HSC the strength loss was 10%, 26%, 54% and 74%,
was observed in 0.5GNMPs after hold time of around 30 min, when respectively. The observed trend of results are relatable to the past
heated to 800 °C. Fire induced spalling in HSC is mostly attributed research on HSC by Sofren and Takashi [5] and Khaliq and Taimur
to the accumulation of thermal stresses, which is due to the lower [23]. High temperature induces concentrated heat pockets with
thermal conductivity [34]. The lack of thermal conductive media in high thermal stresses. However, due to higher thermal conductiv-
control samples led to the occurrence of concentrated heat pock- ity [14] and uniform dispersion of GNMPs, these thermal stresses
ets. Hence, a pattern of concentrated cracks was observed in HSC are well scattered and dispersed in the modified matrices.
samples. High thermal conductivity of modified samples dispersed Moreover, these GNMPs promote the growth of CSH gel on their
the thermal stresses, because of which cracks were well scattered surface and consequently improve the mechanical properties [16].
and in turn improved the thermal stability of modified samples. Fig. 5 shows the microstructure of 0.3GNMPs mix at 400 °C. It can
0.3GNMPs formulation showed better thermal endurance and did be seen that the GNMPs are well dispersed in the cement phase.
not spall off on experiencing the temperature of 800 °C like the Growth of CSH gel can also be witnessed on the surfaces of GNMPs
reference and 0.5GNMPs modified formulation. The modified in Fig. 5, which establishes it being a nucleation site to some
response of 0.3GNMPs mix may be attributed to their extent.

Table 7
Detail of mixture proportions and strength progression.

Mix Cement GNMPs Silica Water (w/c = 0.27) Fine aggregate Coarse aggregate
kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 kg/m3
HSC 713 0 71 192 802 820
0.1GNMPs 713 0.713 71 192 802 820
0.3GNMPs 713 2.14 71 192 802 820
0.5GNMPs 713 3.56 71 192 802 820
Compressive Strength (MPa)
HSC 0.1GNMPs 0.3GNMPs 0.5GNMPs
3 days 19.10 23.21 24.68 23.51
7 days 31.67 36.20 40.65 39.35
14 days 37.40 46.41 49.20 48.10
28 days 47.98 57.95 61.46 59.62
6 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

Fig. 3. Color change, cracking and spalling visuals of reference and modified HSC with nano/micro graphite platelets modified HSC at ambient and elevated temperature
conditions.

Furthermore, these highly dispersed GNMPs particles act as configuration of these GNMPs, which are well dispersed as in the
heat carrier and ensure its uniform distribution, thereby reduce mixtures of 0.1 and 0.3GNMPs, allow to hinder and alter micro
the quantum of induced thermal stresses. GNMPs possess the ‘‘sur- and nano level cracks and hence better retain the compressive
face effect”, contributing to provide excess interface area, to estab- strength [16,19]. Higher strength loss in 0.5GNMPs as compared
lish firm binding with the cement grains [44]. The platted to 0.1GNMPs and 0.3GNMPs might be associated with unnecessary
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 7

Fig. 4. Variation in compressive strength of HSC and nano/micro graphite platelets modified HSC at ambient and elevated temperatures (a) absolute compressive strength (b)
relative compressive strength.

Fig. 5. Micrograph of 0.3GNMPs concrete after being exposed to elevated temperature of 400 °C.

flocculation of stiff platelets forming the weak zones [17,26,45]. indicates that the graphite nano/micro platelets have successfully
The micrographs shown in Fig. 6 evidencing the flocculation and acted as nucleation sites and promoted the growth of hydrates.
cracking patterns. Square EDX spectra of the flocculation point in
Fig. 6c shows the high concentration of carbon indicating it to be 3.3. Tensile strength
GNMPs.
Fig. 7 shows the XRD of HSC and 0.3GNMPs to study any chem- ASTM C496 [30] was followed for the computation of splitting
ical change due to formation of new hydration products. No addi- tensile strength. It may be observed in Fig. 8 that the tensile
tional products are found, which upholds the statement that strength of modified mixes improved by 16.3%, 30% and 19% by
incorporation of these nano inert does not influence the host adding 0.1%, 0.3% and 0.5% GNMPs respectively, compared to the
matrix chemistry. However, the increase in Si peaks at 50(2Ho) HSC mix having no GNMPs. There was an increment in the tensile
8 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

Fig. 6. SEM images for 0.5GNMP concrete at X5000 shows flocculation and cracking pattern a) Unheated b) Post heated c) Square EDX spectra.

HSC showed higher strength loss of 28%, 38%, 60% and 84% at
100, 200, 400 and 600 °C, respectively, while the strength loss in
0.3GNMPs were 11%, 23%, 42% and 70%, respectively, at the afore-
mentioned targeted temperatures. This reduction in the tensile
strength of HSC conforms to prior studies by Suhaendi and Khaliq
[5,33]. Load carrying area of the concrete mix reduces due to the
inception and progression of cracks [4]. Furthermore, because of
lower thermal conductivity of concrete, concentrated thermal
stresses are generated at elevated temperatures, which produce
thermal cracks and effect the mechanical properties [46]. GNMPs
possess high thermal conductivity which can help to scatter the
thermal stresses uniformly and resist their concentration. Further,
due to the crack blunting and bridging effect of GNMPs, the process
of initiation and opening up of the cracks can be delayed. Improve-
ment in the interfacial bonding of such composites has also been
reported [16,19] which can also help to better retain the strength.
Thus, the GNMPs concrete samples showed better performance at
elevated temperature as compared to the control samples.
Fig. 7. XRD comparison of HSC and 0.3GNMPs.

3.4. Stress–strain response

strength of mixes having GNMPs constituents but at 0.5% GNMPs
concentration, concrete showed lesser increment in the tensile Along with the compression tests, stress–strain response was
strength that might be attributed to inadequate dispersion of stiff obtained at each targeted temperature for all high strength con-
platelets, leading towards agglomerate formations [21,26,45]. The crete types. Load and displacement data were obtained by a load
physiochemical degradation of concrete mix exposed to elevated cell and a linear variable displacement transducer (LVDT) attached
temperature resulted in reduction of tensile strength. to the universal testing machine. A data logger was used to store
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 9

Fig. 8. Variation in tensile strength of HSC and nano/micro graphite platelets modified HSC at ambient and elevated temperatures (a) absolute tensile strength (b) relative
tensile strength.

Fig. 9. Stress-strain response at ambient and elevated targeted temperatures of analyzed formulation (a) HSC (b) 0.1GNMPs (c) 0.3GNMPs (d) 0.5GNMPs.

the input of LVDT and load cell to an attached computer. Modulus each target temperature. This can be due to the alteration in
of elasticity was calculated from stress-strain curves. microstructures that involves cracking of mortar, disintegration
Fig. 9 shows a common trend in the stress–strain response that of bond as a result of paste-aggregate thermal incompatibility,
by increase in temperature, the ultimate peak stress decreases and CH decomposition, de-carbonation and above all CSH gel disinte-
corresponding strains increase for all the analyzed formulations, at gration [32,47]. The peak strain values for HSC were 22%, 48.2%,
10 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

126% and 225% higher after exposure to 100, 200, 400 and 600 °C was quantified by determining the area under the stress–strain
temperatures respectively, as compared to the ambient tempera- curve. Area up to the ultimate strains was taken under considera-
ture strain. Similarly, increase in strains with the increase in tem- tion for all the concrete mixtures, in accordance with prior study
peratures was observed for nano/micro modified formulations. For by Marar et al. [49].
0.3GNMPs the peak strains were 160% and 295% higher after expo- Fig. 10(a) shows the energy absorption capacity of all the ana-
sure to 400 and 600 °C, respectively, as compared to the ambient lyzed concrete mixtures. For effective interpretation of increase
temperature strain. Peak strains of 0.3GNMPs were higher as com- in fracture energy, toughness indices (TI) were also evaluated using
pared to HSC strain values. The peak strain values were higher for Eq. (1) with the trend plotted in Fig. 10 (b).

Compressive toughness of modified sample at an exposure temperature

TI ¼ ð1Þ
Compressive toughness of control sample at that certain exposure temperature

0.3GNMPs due to adequate quantity and uniform distribution of

GNMPs, as shown in the scanning electron micrograph included The increase in toughness of mixtures containing GNMPs was
in Fig. 5. Expulsion of water at high temperature causes the dehy- compared to the control HSC mixture with the help of a baseline
dration of matrix and subsequent development of cracking [48]. (control HSC). The toughness of GNMPs mixtures was greater than
Similarly, the concentration of thermal stresses can cause cracking that of the controlled HSC samples. Increase in toughness was
in the matrix resulting in deterioration of effective load bearing achieved (123–300%) with maximum value recorded for 0.3GNMPs
area [4]. GNMPs mitigate the thermal stresses by maintaining the on subjection to 600 °C temperature. The greater energy absorbing
temperature uniformity in the concrete matrix due to their higher capacity of these nano/micro modified matrices indicate towards
thermal conductivity [14,44]. Moreover, higher aspect ratio plated the improvement of their fracture characteristic alongside the abil-
structure of GNMPs enables them to block and divert the micro- ity to sustain inelastic deformations without substantial compro-
cracks, resulting in slowing down crack progression and the subse- mise on the load carrying capabilities. The increased energy
quent formation of crack network, which is reflected in their higher absorption of nano/micro modified mixtures is attributed to the
strain taking capability [44]. presence of GNMPs that effectively resist the initiation and pro-
gression of induced cracks.
3.5. Compressive toughness
3.6. Modulus of elasticity
Stress–strain results showed that mixtures having GNMPs owe
relatively higher peak stresses and alongside the higher values of Elastic modulus for all concrete types was calculated as per the
peak and rupture strains. Thus, the energy dissipation ability for procedure given in ASTM C469/C469M-14 [29]. For all the ana-
all the analyzed formulations was computed for fracture phase. lyzed mixtures, elastic modulus was evaluated at strains corre-
Compressive toughness (Tc) is the energy absorption capacity of sponding to the 40% of the values of stress at each of the
a material to resist the loading in the fracture initiation and pro- targeted temperature. The results are demonstrated in the form
gression phase. Tc was calculated for the increase in fracture of absolute (ET) and relative (ET/E) loss of elastic modulus in
energy of the GNMPs modified mixes. Compressive toughness Fig. 11. GNMPs concrete showed higher elastic modulus than that

Fig. 10. Compressive toughness of HSC and nano/micro graphite platelets modified HSC at ambient and elevated temperatures (a) absolute compressive toughness (b)
toughness indices.
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 11

Fig. 11. Variation in modulus of elasticity of HSC and nano/micro graphite platelets modified HSC at ambient and elevated temperatures (a) absolute elastic modulus (b)
relative elastic modulus.

of the HSC mix. The enhancement in strength and modulus could

be associated with the greater strength and greater aspect ratio
of the graphite platelets, along with the homogeneous dispersion
and favorable interfacial bonding between the matrix and added
platelets [16,19]. Aforementioned characteristics add valuable load
transfer from the matrix to the platelets [17]. It can also be seen
that the modulus of elasticity continued to decrease by increasing
the temperature accompanying the deficit of only 12% at 100 °C for
0.3GNMPs and almost 23% at 200 °C. The loss in modulus at 400 °C
for HSC, 0.1GNMPs, 0.3GNMPs and 0.5GNMPs was recorded as 61%,
49%, 45% and 53%, respectively. While the loss in modulus at 600 °C
for HSC, 0.1GNMPs, 0.3GNMPs and 0.5GNMPs was 91%, 77%, 66%
and 79%, respectively, as compared to that at room temperature.
The loss in modulus of HSC was 61% and 91%, while in 0.3GNMPs
the loss was 45% and 66% at 400 and 600 °C, respectively, which
showed relatively better performance of modified samples. Smaller
size particles enable GNMPs to serve as nuclei that can improve the
homogeneity and compactness of cement matrix [44]. The loss of
modulus in 0.3GNMPs was 45% and 66% at 400 and 600 °C, respec-
tively, while 0.5GNMPs showed loss of 53% and 79%, respectively.
Similarly, 0.3GNMPs showed relatively better performance than Fig. 12. Variation in UPV of HSC and nano/micro graphite platelets modified HSC at
0.1GNMPs and loss in modulus was 82% at 800 °C, as compared ambient and elevated temperatures.
to the loss of 90% for 0.1GNMPs. Due to uniform dispersion and
adequate quantity of GNMPs in 0.3GNMPs, thermal stresses were
quite well scattered [14]. Therefore, 0.3GNMPs showed better per-
formance to retain the loss in elastic modulus at elevated temper- attributed to the development of relatively lesser cracks. Because
atures in comparison to remaining formulations. of lower thermal conductivity of concrete, thermal stresses are
not very well scattered that contributes in the formation of con-
centrated stress pockets [14]. 0.3GNMPs exhibited the highest val-
3.7. Ultrasonic pulse velocity test ues of UPV due to optimum amount and uniform distribution of
graphite nano/micro platelets, which are deemed useful as per
In order to determine the extent of fire damage and the service- the mechanical tests. These platelets act as an effective heat carrier
ability of the analyzed specimens, ultrasonic pulse velocity (UPV) and uniformly distribute the heat in the matrix due to higher ther-
test was conducted on concrete specimens before and after expo- mal conductivity and reduce the thermal cracking by scattering the
sure to targeted temperature as per ASTM C597 procedure [50]. thermal stresses. 0.1% GNMPs mix was insufficient to cater for the
UPV test is a qualitative technique and is sensitive to the phenom- mitigation of micro-cracking and hence the value of pulse velocity
ena of quality degradation which includes internal cracking and was lower as compared to 0.3% GNMPs mix. 0.5 GNMPs mix per-
some other deteriorations because of the thermal exposure. A formed better than HSC. However, due to the agglomeration of
higher severity of damage is associated with smaller value of highly stiffed platelets, concentrated cracks were developed and
UPV. Fig. 12 shows that the GNMPs concretes owe higher values hence the UPV value of 0.5GNMPs was relatively lower in compar-
of UPV compared with the reference HSC mix that may be ison to the 0.3GNMPs mix.
12 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

and results in a loss of overall concrete mass. Fig. 13 shows the rel-
ative mass loss of the analyzed formulations. The average mass loss
at 200 °C and 400 °C was almost 2% and 5%, respectively for all the
concrete mixtures. The observed mass loss in 0.1GNMPs at 800 °C
was 11%, while the loss was 10% in 0.3GNMPs. Mass loss of HSC
was 6% and 8.3%, while in 0.3GNMPs the mass loss was 4.3% and
7% at 400 °C and 600 °C, respectively. The observed pattern of
results conforms to the previous study on high performance con-
crete by Huzeyfa and Nilufer [52]. Mass loss in HSC was more than
the mass loss in GNMPs modified mix which may be associated to
the refined pore structure of GNMPs formulations at ambient con-
ditions [53]. Nano size effect enables GNMPs to serve as nuclei that
accelerate the hydration reaction of cementitious composites and
reduce the porosity of concrete [19]. Due to large surface area,
more hydrates are formed on the surface of GNMPs and higher
density CSH gel is produced. This high-density gel increases the
temperature exposure range of evaporable liquid, making difficult
for the water to expel from the matrix and hence lower mass loss
occurs in the GNMPs concrete as compared to reference HSC mix.

3.9. Mathematical relationships

Fig. 13. Relative decrease in mass of HSC and nano/micro graphite platelets
modified HSC at ambient and elevated temperatures.
Mathematical equations have been developed with the accu-
mulated data over complete range of temperature between 23
and 800 °C. These mathematical equations might help to estimate
3.8. Mass loss the post fire residual capacity of damaged structural member. The
mentioned relationships are established employing linear regres-
All concrete samples lost some mass when exposed to elevated sion, using a commercial software Minitab [54]. Each analytical
temperatures. Concrete as a hydrated bonding matrix holds a bal- design was achieved by using material property as the response
ance between the mass loss and concrete strength due to the dis- variable and temperature as the predictor. The coefficient of deter-
turbances in the associated moisture. Since the mixing of water mination (R2) determines the efficiency of an analytical model. The
with concrete plays an important role in hydrating cement and coefficients for the present study lie in the range of 0.85 and 0.99,
strength development, this forced moisture loss degrades strength hence corresponding to a fair comparison of the properties of HSC
due to the loss of water from concrete mix. The expulsion of water and GNMPs concrete recipes.
at elevated temperature accompanies cracking due to developed The alteration of the material properties such as compressive
water pressure as well [51]. Thus, the loss of mass at higher tem- strength (f’c,T), splitting tensile strength (f’t,T), ultrasonic pulse
peratures is associated to the loss of moisture and hence bears a velocity (UPV), elastic modulus (ET) and mass loss (MT) corre-
direct relation with the concrete strength. Dehydration of hydrated sponding to temperature can be associated by a coefficient bT.
chemical compounds (like calcium hydroxide and C-S-H gel) in the The coefficient bT correlates the value of investigated parameters
concrete also takes place at the temperatures higher than 400 °C (f’c,T, f’t,T,UPVT, ET, and MT) at targeted high temperature with

Table 8
High temperature material property relations for HSC and nano/micro graphite modified high strength concrete mixtures.

Formulation Property relationship % Error**

HSC bT, compression = {1.0210–0.001312 T 23 °C  T  600 °C*} 0.92–9.8
bT, tensile = {0.9304–0.001317 T 23 °C  T  600 °C*} 0.23–14.89
bT, mass = {1.00896–0.000153 T 23 °C  T  600 °C*} 0.15–0.57
bT, UPV = {0.9938–0.001006 T 23 °C  T  600 °C*} 2.94–7.4
bT, modulus = {1.03623–0.001590 T 23 °C  T  600 °C*} 0.04–6.96
*Specimens spall off beyond 600 °C
0.1GNMPs bT, compression = {1.0178–0.001018 T 23 °C  T  800 °C} 0.92–9.9
bT, = {0.9655–0.001189 T 23 °C  T  800 °C}
tensile 2.51–6.19
bT, mass = {1.00897–0.000143 T 23 °C  T  800 °C} 0.63–9.03
bT, UPV = {1.0007–0.000935 T 23 °C  T  800 °C} 0.39–2.08
bT, modulus = {0.9918–0.001158 T 23 °C  T  800 °C} 0.02–0.49
0.3GNMPs bT, compression = {1.0495–0.001037 T 23 °C  T  800 °C}^ 0.48–7.5
bT, = {1.0063–0.001099 T 23 °C  T  800 °C}
tensile 0.58–6.1
bT, mass = {1.00889–0.000130 T 23 °C  T  800 °C} 0.99–10
bT, UPV = {0.9937–0.000895 T 23 °C  T  800 °C} 0.53–5.75
bT, modulus = {0.9956–0.001059 T 23 °C  T  800 °C} 0.11–0.65
bT, compression = {1.0411–0.001258 T 23 °C  T  600 °C*} 0.99–5.54
0.5GNMPs bT, tensile = {0.9997–0.001300 T 23 °C  T  600 °C*} 0.9–3.7
bT, mass = {1.00611–0.000127 T 23 °C  T  600 °C*} 1.03–2.08
bT, UPV = {0.9991–0.001002 T 23 °C  T  60 °C*} 2.4–7.18
bT, modulus = {1.0102–0.001344 T 23 °C  T  600 °C*} 0.09–0.3
*Specimens spall off beyond 600 °C
**% Error between predicted and experimental results
 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029 13

Table 9
Relative decrease in compressive strength of HSC and nano/micro graphite platelets modified HSC at ambient and elevated temperatures (Comparison with existing design codes).

Formulation T (°C) Experimental Eurocode ASCE Proposed

HSC 23 1 0.98 0.99 0.99
100 0.90996 0.91 0.98 0.88
200 0.73656 0.93 0.97 0.75
400 0.46415 0.74 0.89 0.49
600 0.25927 0.45 0.64 0.23
800 – 0.16 0.17 –
0.1GNMPs 23 1 0.98 0.99 0.99
100 0.88542 – – 0.91
200 0.79776 0.93 0.97 0.81
400 0.58878 0.74 0.89 0.61
600 0.36635 0.45 0.64 0.40
800 0.117 0.16 0.17 0.20
0.3GNMPs 23 1 0.98 0.99 1.02
100 0.94126 – – 0.94
200 0.87244 0.93 0.97 0.84
400 0.64367 0.74 0.89 0.63
600 0.43329 0.45 0.64 0.42
800 0.20435 0.16 0.17 0.21
0.5GNMPs 23 1 0.98 0.99 1.01
100 0.91261 – – 0.91
200 0.82506 0.93 0.97 0.78
400 0.50805 0.74 0.89 0.53
600 0.29504 0.45 0.64 0.28
800 – 0.16 0.17 –

strength for post heated HSC containing nano-carbonaceous media

with high accuracy in the temperature range of 23–800 °C. How-
ever, the same may be practiced for conventional HSC mixes with
lesser accuracy.

4. Conclusions and recommendation

The results provided in this study report new data on fire

endurance of concretes containing graphite nano/micro platelets
and were compared with well-established data of high strength
concretes (HSCs). Variable amount of GNMPs were used i.e. 0.1,
0.3 and 0.5% by weight of cement. Optimum dosage of GNMPs in
high strength concrete at elevated temperatures is conclusively
believed as 0.3%. Based on the results obtained in this study, fol-
lowing conclusions are drawn:

i. The presence of graphite nano/micro platelets improve the

compressive strength of samples pre and post-fire exposure.
Fig. 14. Relative decrease in compressive strength of HSC and nano/micro graphite GNMPs modified high strength concrete samples exhibit
platelets modified HSC at ambient and elevated temperatures (Comparison with lower strength degradation due to their thermally efficient
existing design codes).
behavior that scatters the thermal stresses in effective way.
ii. Graphite nano/micro platelets contribute in adding the split-
ting tensile strength of modified mixes as they effectively
reference to their values in ambient conditions. The relationships delay the initiation and progression phases of cracks.
are summarized in Table 8 for the analyzed functions in physical iii. The compressive strength losses alongside an increase in the
and mechanical domains limited to the defined temperature range. values of peak and rupture strains at both ambient and ele-
The reduction factor bT at various temperatures may evaluate split- vated temperatures for GNMPs modified high strength
ting tensile and compressive strength, modulus of elasticity, and concrete.
mass loss for the investigated formulations. iv. GNMPs modified samples show increase in fracture energy
The experimental values for compressive strength of post as compared to the control samples. Maximum increase by
heated HSC containing GNMPs were compared with the two 300% is attained in 0.3GNMPs formulation on being exposed
well-known design codes i.e. ASCE and Eurocode as shown in at 600 °C which is attributed to homogenized distribution of
Table 9 and Fig. 14. The design codes (ASCE and Eurocode) overes- GNMPs restraining cracks at the micro instinct.
timate the residual experimental test result values. These codes v. Graphite nano/micro platelets modified high strength con-
were developed for conventional high strength concrete (HSC) crete formulations owe better mass retention at high tem-
and are not adopted for concrete with GNMPs. The proposed perature because of the filler effect of GNMPs leading to
strength equation better predicts the residual compressive refinement of pores.
14 H.W. Iqbal et al. / Construction and Building Materials 253 (2020) 119029

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Acknowledgments
graphite nanoplatelets, Constr. Build. Mater. 47 (2013) 111–117, https://doi.
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The authors are grateful to Higher Education Commission of [21] D. Bansal, S. Pillay, U. Vaidya, Nanographite-reinforced carbon/carbon
Pakistan for the research funds awarded against an NRPU grant composites, Carbon N. Y. 55 (2013) 233–244, https://doi.org/10.1016/
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