Diamond & Related Materials 124 (2022) 108883

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Diamond & Related Materials

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

Experimental study on the properties improvement of hybrid graphene

oxide fiber-reinforced composite concrete
Osama Zaid a, *, Syed Roshan Zamir Hashmi a, Fahid Aslam b, Zain Ul Abedin c, Asmat Ullah d
a
Department of Structure Engineering, Military College of Engineering, Risalpur, National University of Sciences and Technology, 44000 Islamabad, Pakistan
b
Department of Civil Engineering, Prince Sattam Bin Abdulaziz University, Al-Kharj 11942, Saudi Arabia
c
Department of Mechanical Engineering, Cherat Cement Factory, Nowshera 24100, Pakistan
d
Department of Civil Engineering, University of Engineering and Technology, Taxila 47080, Pakistan

A R T I C L E I N F O A B S T R A C T

Keywords: Graphene oxide can have a massive influence on industries related to concrete and construction in the coming
Graphene oxide years. Due to the oxygenated capabilities connected to the aromatic structure, it has an improved ability to
Concrete performance disperse in mixes in comparison to the other graphene-based materials. Very few researchers have given their
Steel fibers
idea about the influence of graphene oxide plus fibers on the durability and mechanical behavior of cement-
Nanomaterial
Hybrid concrete
based composites. Five different mixes were developed with utilization of graphene oxide (0%, 0.03%, 0.06%,
0.09% and 0.12% by cement weight) and 2% of steel fibers was added by binder weight. Experimental tests were
performed related to mechanical and water permeation characteristics. The concrete mix with 0.12% of graphene
oxide has displayed a significant result in terms of mechanical properties and other durability testing in contrast
to the other sample mixtures. The permeability and sorptivity of the fiber-strengthened concrete samples in the
utilization of graphene oxide were noted to have decreased with increment of graphene oxide content in the
mixes in comparison to the reference sample. The synthesized graphene oxide was structurally categorized with
the help of FT-IR, EDX, and XRD tests. Microstructural behavior was assessed with the help of XRD spectra on
sample cured at 90 days, and the concrete quality was assessed with an ultrasonic pulse velocity test. The study
showed that M5 mix (0.12% GO and 2% steel fibers) enhanced compressive and split tensile strength up to 56%
and 37%, M5 mix also showed highest average velocity for UPV test and lower values for sorptivity test which
indicates improved mechanical properties, durability and reduced porosity. Thus, concrete with GO and steel
fibers can be confidently used in building application as sustainable and economic construction material.

1. Introduction
Cement is the fundamental ingredient utilized in concrete as a
binder. The requirement for concrete with high compressive strength is
expanding very fast [1]. But concrete with high compressive strength
requires high amount of cement [2]. Utilizing more cement for pro­
duction of cement leads to high cost and also adds risks to the envi­
ronment [3]. Supplementary cementitious materials (SCMs) can be used
as a cement substitute to reduce these environmental risks and also
improve compressive strength of concrete [4]. But the major disadvan­
tage of concrete is its brittleness and having low strength in tension.
With time this deficiency of concrete is taken care of by utilizing rebars
and fibers in concrete [5,6]. To overcome this brittle nature of concrete
different fibers have been used for example steel fibers, synthetic fibers,
macro fibers, carbon fibers into cement matrix as a reinforcement. Steel
fiber is one of the highly used fiber which is used in the concrete to
enhance its fracture toughness, ductility, tensile strength, resistance
against chemicals and averting cracks [7,8]. Researchers have noted
that concrete with steel fibers can lead to high water absorption and
lower workability of mix [5]. It was also observed that 1.5% steel fibers
enhanced splitting tensile and flexural strength by 59% and 45% [9].
Recently glass fibers, basalt fibers and carbon fibers are also being highly
used in cementitious composites. These fibers assist in against carbon­
ation depth and chemicals, improve permeability and durability
[10–12]. Such concrete having fibers are called fiber reinforced com­
posite concrete (FRCC). The characteristics of FRCC considerably rely on
the interface amid binder matrix and fibers. To safeguard the efficiency
of transfer of load amid fiber and binder matrix, strong interfacial

* Corresponding author.
E-mail address: osamazaidmarwat@gmail.com (O. Zaid).

https://doi.org/10.1016/j.diamond.2022.108883
Received 21 October 2021; Received in revised form 18 January 2022; Accepted 31 January 2022
Available online 4 February 2022
0925-9635/© 2022 Elsevier B.V. All rights reserved.
O. Zaid et al.
property is very important, which can ultimately enhance the complete
properties of fiber reinforced composite concrete [13,14].
Utilization of nanomaterials [15] in concrete composites has also
improved the concrete behavior, for example, flexural, durability,
toughness, and tension characteristics by enhancing the concrete at the
nano-scale. Nanotechnology has shown that cement-based composites
could be enhanced or improved by adding a minor dose of nanomaterials
[16]. Graphene-derived, carbon nanotubes CNT, nano-silica, carbon
nano-fibers (CNF) [17], are well-known among entire nanomaterials.
Nano-composites have shown their capability to improve the charac­
teristics of the parent material. The utilization of nanomaterials in the
construction industry has [18] developed the latest practice as it has a
lot of qualities from the improvement of mechanical performance to fill
the concrete voids at the Nano-level. The characteristics of nano­
materials and cement, for example, graphene-based nanomaterials,
carbon nanotubes, graphene oxide, and graphene are known to enhance
[19] the thermal, mechanical, optical, and electrical features of the
concrete composites. Some of the authors have [20] researched on
durability and mechanical characteristics of nano-reinforced concrete
mixtures, and it showed improved outcomes in comparison to reference
concrete mixtures [21,22]. Graphene oxide is known as a nano-material
that is carbon-based. Benjamin C Brodie was the original person who
developed it in 1859 [23]. The aromatic structure of the graphene oxide
is like some other graphene-based inferred material [24], but because of
the chemical reaction that is happened, few of the electron pair bonding
were split down and functional groups for example phenol, carbonyl,
were connected on the sp2 aromatic one-layered structure [25,26]. GO
has its qualities when it is utilized in concrete composites. Specific
surface area of graphene oxide is high. Commonly, nanomaterials have
one drawback [27] which is their ability to disperse uniformly, but the
graphene oxide does not have this disadvantage due to the oxidative
nature which lets it scatter effortlessly in the water. Recently graphene
oxide has become widely used material [24] in structural application
due to its impressive mechanical behavior, high rate of dispersion in
water, high hydrophilicity and large availability due to its
manufacturing. The introduction of the graphene oxide in cement con­
crete has a negative influence on the workability [28] of concrete
because of the higher specific surface area of GO that leans to engross
additional particles of water to become bulky and wet with more volume
for retaining of water formed because of the cluster of graphene oxide
nano-sheets [29,30]. Irrespective of the above-called drawback of gra­
phene oxide, the inclusion of a small amount of graphene oxide of almost
0.1% of cement weight has improved the flexural strength by 39–60%
and compressive strength by 18–35% [22,31]. The researchers have
revealed that with the addition of 0.07% graphene oxide to the paste of
cement, the compressive strength was enhanced by 14.9% in compari­
son to the paste of cement without the addition of GO [32]. The flexural
and compressive strength was improved by 39% with the inclusion of
0.02% graphene oxide by cement weight at the curing of 28 days [33].
The author in another study has revealed that the incorporation of
graphene oxide led to improvement of penetration of chloride and
sorptivity of water while it also decreases the pore size of graphene oxide
strengthened binder paste demonstrating the enhancement of resistance
against chemical attack [34]. Few authors have mentioned that the
addition of graphene oxide quickens the hydration heat. The sheets of
graphene oxide with oxygenated capabilities form further amicable
particles of cement hence letting the nanosheets behave as a nucleus for
the stages of cement accelerating the reaction of water with cement
[34]. In another study, the author revealed that the microstructure of
graphene oxide strengthened cement-based composites have huge
crystal structure cover indicating leaching of Ca(OH)2 through the
phases of hydration have been enhanced at curing of 28 days [35]. From
the above literature, it is concluded that combining graphene oxide and
fibers to develop concrete composites will have a promising result in
terms of performance of concrete for the construction industry. Research
on the hybrid GO fibers-reinforced concrete is still in the early stages
2
Diamond & Related Materials 124 (2022) 108883
[36]. Insufficient considerations are given to study the mechanical
performance and interface of hybrid fibers-GO reinforced concrete [37].
More notably, significant issue regarding the method for making and
mix design of hybrid fibers-GO reinforced concrete needs to be
addressed as well [38]. This research is planned to develop budget and
eco-friendly GO hybrid fiber reinforced composite concrete.
1.1. Research significance
The inclusion of graphene oxide in cement matrix is in trend due to
its exceptional properties. As graphene oxide is very cheap in compar­
ison to the highly costly single-walled and multi-walled carbon nano-
tubes and carbon Nano-fibers [39], interest in graphene oxide has
arisen worldwide. Hence graphene oxide is the suitable option for the
present study. This study was performed to make a fiber-reinforced
cement composite with the inclusion of graphene oxide of different
proportions by cement weight. According to the authors reliable infor­
mation very few research has been performed on utilization of graphene
oxide and steel fibers in concrete composites with natural fine and
coarse aggregates considering compressive strength, workability, sorp­
tivity, workability, flexural strength, ultrasonic pulse velocity test
(UPV), water permeation, XRD spectra, and the analysis of cost-benefit
to determine if the current study will be appropriate to be imple­
mented in the construction industry for practical applications.
2. Experimental plan
2.1. Materials
Following modified Hummer's method, raw graphene oxide was
produced [40,41], 5 g of sodium nitrate Na2NO3 and 10 g of graphite
powder were permitted to react with concentrated 230 ml of sulfuric
acid H2SO4 at a temperature of 25 ◦ C on a heater stirrer for 30 min and
then we slowly added 30 g of (KMnO4) potassium permanganate. The
resulted mix was heated for over 30 min at a temperature of 35 ◦ C and
then gradually diluted with 325 ml of water. The subsequent mixes were
heated for over 15 min at a temperature of 98 ◦ C and then 4% (H2O2)
hydrogen peroxide was introduced to finish the chemical reaction after
380 ml de-ionized water and then permitted to settle. Lastly, the dilute
solution of graphene oxide was washed with 1:10 HCl and 3 l of de-
ionized water till the filtrate pH came to 8. The filtered paste was
placed in an oven at 70 ◦ C for 24 h to acquire the needed powder of
graphene oxide as shown in Fig. 1. The acquired graphene oxide was
structurally characterized utilizing an Energy-dispersive X-ray, Fourier
transom infrared spectroscopy (FTIR), and X-ray diffraction procedures
to determine the near-surface composition, crystalline configuration and
recognize the present functional classes. Size of graphene oxide was
0.33 nm and it was single layered sp2 bonded carbon atoms arranged in
a hexagonal or honeycomb lattice. 53 grade type-I Portland cement was
utilized for the current research. Its chemical and physical properties are
presented in Table 1. Conventional river sand was utilized as a fine
aggregate and crushed granite stone was acquired as a coarse aggregate
with a maximum size of 25 mm. Only 2% of Steel fibers as shown in
Fig. 2 were added in GO modified concrete samples. Properties of steel
fibers are provided in Table 2.
2.2. Mix proportioning and casting of samples
Five different mixes were developed in total and lab experiments
were conducted on freshly mixed concrete and hard concrete at the
curing of different days. The quantity of cement, fine aggregates, and
coarse aggregates remained the same at 390 kg/m3 of cement, 720 kg/
m3 of fine aggregates, and 1120 kg/m3 of coarse aggregates with a w/c
ratio of 0.41. Graphene oxide was included in different proportions by
cement weight from 0% to 0.12% with an interval of 0.03%. Complete
materials' content for all samples is provided in Table 3. To ensure the
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

Fig. 1. Graphene oxide.

Fig. 2. Steel fibers.

Table 1
Physical and chemical properties of Portland cement. Table 2
Physical properties OPC Chemical Concentration Physical properties of steel fibers.
composition (%) Property Value
Specific gravity 3.16 SiO2 22.10 Shape Straight
Standard consistency (%) 33 CaO 58.90 Appearance Light grey color
Specific surface area (m2/kg) 300 Al2O3 6.05 Length (mm) 50
Initial setting time (minutes) 59 Fe2O3 3.07 Diameter (mm) 0.75
Final setting time (minutes) 265 SO3 2.63 Elastic modulus (GPa) 190
Compressive strength (MPa) MgO 2.75 Aspect ratio 66
3 days compressive strength 24.5 K2 O 0.50 Tensile strength (MPa) 1200
(MPa)
7 days compressive strength 33.4
(MPa)
mix with 0.03% graphene oxide and steel fibers. The nomenclature also
28 days compressive strength 46.3
(MPa) follows for other mixes as well.
Loss of ignition (%) 2.05 Loss 4.00
3. Test procedure

uniform dispersion of graphene oxide in water, GO was permitted to 3.1. Slump

spread utilizing a 600-Watt high power ultrasonic processor [42] in a
solution comprising 0.06% admixture kept the same for the whole
samples in a sonicator with ultrasonic energy of almost 2150 J/min at
20 s cycles (to circumvent overheating) functioned at 60% continuous
amplitude for 25 min. Moreover, the solution was mixed in a volume of
2150 ml mixer. To improve the dispersion of GO, polycarboxylic based
admixture was utilized as a main dispersant dissolved in water. The 15%
and 25% of whole water of the blend were utilized in the exfoliating
procedure utilizing a mixer and sonicator. The mix was introduced with
various percentages of graphene oxide (0.03%, 0.06%, 0.09%, 0.12%).
A standardized mix was made from fine aggregate, cement, water,
fibers and coarse aggregate. These concrete ingredients were then
introduced to a mechanical mixer having a capacity of 40 l, the mixture
was in the mixer for 4 min at 25 revs/min. The freshly mixed concrete
was filled into steel molds, subsequently 24 h the samples were detached
from the casts and then placed in a water tank with a temperature of
25 ◦ C for curing at 7, 28, 56, and 90 days. The nomenclature for mixes
was planned as follows. M1-0%-GO-PC means that it is M1 mix with 0%
graphene oxide plain concrete. M2-0.03%-GO-SFRC means that it is M2
Concrete workability is known as the comfort with which the con­
crete can be mixed, placed, consolidated, and finished with minimal loss
in the homogeneity of concrete mixes, such as bleeding or segregation.
Slump test was performed per ASTM C143 [43] using the slump cone
which had an upper diameter of 100 mm, bottom diameter of 200 mm,
and the height of 300 mm, concrete was poured in 3 layers and each
layer was compacted by tamping 25 times, and the obtained slump value
for reference sample (sample with 0% of graphene oxide) was 100 mm.
3.2. Compressive and split tensile test
Compressive strength and split tensile strength of concrete was
determined following the procedure defined in ASTM C39 [44] and
ASTM C496 [45] respectively. 100 mm cubes were used for both tests,
the cubes were first cured in water for 7, 28, 56, and 90 days and then
they were tested using a compressive testing machine which had the
capacity of 150 ton. The load was applied on the concrete cubes at the
rate of 4 N/mm2/min and the load was gradually increased until the

3
O. Zaid et al.
Table 3
Mixture proportion of all specimens (kg/m3).
Mix ID Mix description OPC (kg/m3) Graphene oxide (GO) (grams)
M1 0%-GO-PC 390 0 0
M2 0.03%-GO-SFRC 390 11.7
M3 0.06%-GO-SFRC 390 23.4
M4 0.09%-GO-SFRC 390 35.1
M5 0.12%-GO-SFRC 390 46.8
concrete cube failed under the load. For the split tensile test, the sample
was placed in a way that longitudinal axis is perpendicular to the applied
load. Two strips of plywood between the upper and lower sides of the
samples, and the load was 5.5 N/mm2/min and the applied load was
slightly increased until the sample failed.
3.3. Water permeation of concrete
3.3.1. Initial surface absorption
The objective of this test is to examine the water flow into the surface
of concrete per unit area at the stated level. 150 mm cubes were used to
perform the concrete test for initial surface absorption as per BS 1881
Part 208 [46]. The samples were oven-dried at 103 ◦ C, the test setup was
developed in such a manner that a cap of 80 mm diameter was clamped
to the surface of the cube which provided water area contact with the
surface to be examined of at least 4500 mm2. The water was permitted to
stream over the reservoir bay which had a diameter of 100 mm and that
was attached with a tap to an exit channel connected with a gauge. The
height of water was kept in the range of 170 mm and 210 mm for this
trial. The tap was unlocked and values were recorded for 2 min at a
break of 20 min, 40 min, and 60 min from the beginning of the test. The
flow rate was calculated in mL/m2s. This test was conducted on samples
that were cured in water for 28, 56, and 90 days.
3.3.2. Sorptivity
100 × 50 mm discs were used for this test by cutting 100 mm × 200
mm cylinders, these discs were then oven-dried at 103 ◦ C, this test was
conducted following ASTM C1585 [47]. The circumference area of the
sample was covered with epoxy paint and both the top and circumfer­
ential surfaces were firmly wrapped by utilizing plastic sheets for
blocking evaporation. The disc weight was noted at 0, 5, 15, 35, 45 and
60 min for each 60 min interval up to 7 h since the beginning. This test
was performed on concrete samples having graphene oxide of 0%,
0.03%, 0.06%, 0.09%, and 0.12% and placed in water for 28, 56, and 90
days.
3.4. Ultrasonic pulse velocity test (UPV)
An electro-acoustical transducer was used to generate ultrasonic
pulse velocity (UPV). UPV was conducted following ASTM C597 [48].
Transducer disseminated on one side of concrete sample and getting a
frequency of 49 kilo-Hertz, the identical by an alike transducer in
interaction with another end of the concrete surface. A coupling gel in a
thin layer was used to assist in receiving higher signals. When the con­
crete quality, in terms of uniformity, density and homogeneity is good,
then high velocity is obtained. If the concrete quality is low, then lower
velocity is attained. All the ranges of ultrasonic pulse velocity (UPV)
tests are provided in ASTM C597 [48]. This test was conducted on
concrete cubes that were placed in water for 28, 56, and 90 days.
4. Interpretation of results
4.1. Structural classification of synthesized graphene oxide
The structural classification of synthesized graphene oxide in
powdered form was performed utilizing energy dispersive x-ray (EDX),
Diamond & Related Materials 124 (2022) 108883
Steel fibers (kg/m3) Water (kg/m3) Coarse aggregate (kg/m3) Fine aggregate (kg/m3)
160 1120 720
7.8 160 1120 720
7.8 160 1120 720
7.8 160 1120 720
7.8 160 1120 720
to acquire the elemental composition. Fig. 3(a) represents the EDX
analysis of synthesized graphene oxide displaying the crumpled shape
with the elemental configuration of near-surface, in Table 4 the chem­
ical percentage of GO is presented in which was noticed to that the
carbon and oxygen have maximum percentages, which specifies the
affinity of oxidative functional groups. The high surface area of nano-
sheets of graphene oxide interlocked with a weak attractive forces
bond which below the microscope seems to be wrinkled. X-ray diffrac­
tion (XRD) test was conducted on graphene oxide to analyze its crys­
talline structure to reveal the true chemical composition of graphene
oxide, from Fig. 3(b) it can be observed that the XRD spectra measured
in a scope of 2-theta from 4◦ to 60◦ that shows diffraction peak at 2-
theta = 7.11 and 2-theta = 2.13 signifying the distance between the
layers of graphene. Fourier transform infrared spectroscopy (FTIR) was
performed on the graphene oxide, as FTIR is a time saving, non-
destructive method gives information about on molecular vibrations
which is used to detect a variety of functional groups that is existing in a
molecule. Fourier Transform Infrared Spectroscopy (FTIR) identifies
chemical bonds in a molecule by producing an infrared absorption
spectrum. The peak value for FTIR was 2360 and 1515 was the lowest
peak transmittance percentage. From XRD and FTIR spectroscopy as
presented in Fig. 3(b) and (c), it was confirmed the existence of oxidative
functionalities on the nanosheets of graphene oxide. The results of the
above observations are confirmed by the present study [49,50].
4.2. Workability
The concrete sample (M5, 0.12% of graphene oxide + 2% SF) had the
lowest slump value followed by (M4, 0.09% graphene oxide + 2% SF),
(M3, 0.06% graphene oxide + 2% SF) and (M2, 0.03% graphene oxide +
2% SF) in comparison to the reference sample (M1 with 0% graphene
oxide + 0% SF). Fig. 4 represents the slump values of the control sample
along with fiber-reinforced concrete composites, Fig. 4 indicates that as
we increase the amount of graphene oxide and add steel fibers, the
slump reduces, which decreases the workability of mixes. Similar test
outcomes were observed on the increase in viscosity and decrease of
flowability when the amount of graphene oxide was increased [19,29].
Graphene oxide specific surface area is very high (theoretical value is
2610 m2/g), which absorbs water from freshly mixed fiber concrete to
wet the nanosheets of graphene oxide [30]. Similarly, the hydrophilic
oxygenated functionalities are connected to the nano-sheets of graphene
oxide, which absorbs the molecule of water and stand entrapped because
of the development [51] of the agglomeration and flocculation led by
electrostatic interaction between particles of cement and graphene oxide
[32,33,52]. Thus, with more GO and steel fibers in the specimens, the
workability of samples will reduce linearly.
4.3. Mechanical properties
4.3.1. Compressive strength
The compressive strength and split tensile strength were measured
using universal testing machine (UTM) as shown in Fig. 5 on samples
that were cured in water for 7, 28, 56, and 90 days. The samples with
graphene oxide had improved splitting tensile and compressive strength
in comparison to the reference sample, M1. The concrete sample with
(0.12% of graphene oxide + 2% SF) had the maximum enhancement in
4
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

3
C
2.5

Counts
1.5 O

1 H
S
0.5

0
3100 2900 2700 2500 2300 2100 1900 1700 1500
Energy KeV

(a)

2000 D = 7.119 Ao

1750

1500
Lin (Counts)

1250

1000 D = 2.13 Ao

750

500

250

0
20 25 30 35 40 45 50 55 60
2θ Scale

(b)

50

45

40

35
Transmiance (%)

30

25

20 1515
15
2360
10

0
3000 2800 2600 2400 2200 2000 1800 1600 1400 1200 1000
Wavenumber (cm-1)

(c)

Fig. 3. (a) EDX, (b) XRD, (c) FT-IR of graphene oxide.

5
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

Table 4 showed the minimum improvement in strength with only 6%, in samples
Chemical composition of graphene oxide. cured at 90 days. Different studies on the [59] influence of adding
Element Weight (%) graphene oxide in concrete composites have determined that graphene
oxide speeds hydration reaction, enhances flexural and split tensile
C 57.1
O 38.8 strength, improving the mechanical intertwining at the interface of GO
H 1.2 reinforced binder matrix [19,33,55,60,61]. Microstructure densification
S 2.7 might have produced because of the filler effect and high aspect ratio of
Mn 0.2 graphene oxide at nano-scale which results in enhanced strength of GO
Total 100%
composites.
Table 5 illustrates the strengthening influence of graphene oxide in
strength followed by the M4 (0.09% Graphene oxide + 2% SF), M3
(0.06% Graphene oxide + 2% SF), and M2 (0.03% Graphene oxide + 2%
SF). Fig. 6(a) displays the compressive strength of concrete and Fig. 6(b)
improvement in concrete compressive strength in terms of percentages
at various curing days. It may be noticed that steady improvement in
strength with increment in the content of graphene oxide in the samples
at various hydration rates. The sample with 0.09% of graphene oxide
shows the highest compressive strength after curing of 90 days with
39.4% enhancement in comparison to the reference sample. The con­
crete sample M2 with 0.03% graphene oxide had the minimum
improvement in compressive strength with only 22%. Past researches
have stated that the addition of low amount nanosheets of GO in con­
crete samples has improved the compressive strength at a higher level
[22,32,33,53–56].
Authors in another study [57] established that graphene oxide be­
haves as a catalyst and assists in hastening hydration of cement without
producing any variations in the oxygenated functional groups connected
to graphene oxide nanosheets [58]. This functional class behaves as
active sites that entice binder particles. The graphene oxide nanosheet's
high ratio of surface area to mass helps the nucleation for the develop­
ment of hydrates of cement and produces firm covalent bonds at the
interface of graphene oxide and binder matrix. Hence, the addition of
graphene oxide reinforces the composites of concrete at the nano-level,
which leads to improvement of compressive strength of graphene oxide
nano-strengthened cement-based composites in comparison to the
reference sample.

4.3.2. Tensile strength

Fig. 7 shows the effect of GO on the splitting tensile strength of fiber-
strengthened cement-based composite. It could be noted that the sample
which had 0.12% of graphene oxide exhibits the highest tensile strength
with 40% improvement and the sample with 0.03% of graphene oxide Fig. 5. Universal Testing Machine (UTM).

100
100

95
95
92

90 88
Slump Value (mm)

85
85

80

75

70

65
0%-GO-PC 0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

Fig. 4. Slump value of all concrete samples.

6
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

70

Compressive Strength (MPa)

60

50

40

30

20

10

0
7 Days 28 Days 56 Days 90 Days

M1 (Control Sample) M2 (0.03%-GO-SFRC) M3 (0.06%-GO-SFRC)

M4 (0.09%-GO-SFRC) M5 (0.12%-GO-SFRC)

(a)

40
Percentage (%) Increase in Compressive strength

35

30

25

20

15

10

0
7 Days 28 Days 56 Days 90 Days
0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

(b)

Fig. 6. (a) Compressive strength of concrete (MPa), (b) percentage increase in compressive strength at various curing days.

the mechanical strength of the present study in comparison to the past
researches on the utilization of graphene oxide in composites of cement
mortar and cement paste. It is noted that adding 0.03% and 0.06%
graphene oxide in a paste of cement has increased the strength by
39–71% and 14–32% correspondingly, at various days of curing.
Moreover, utilization of graphene oxide in cement mortar with different
percentages from 0.02% to 0.06%, 0.02%–0.025% up to 0.15% can be
used to improve the compressive strength by 13–60%, 27–59%, and
62–87% respectively at various curing days. Likewise, in the present
research, adding of 0.03–0.12% with the interval of 0.03% of graphene
oxide in sample have increased the compression strength by 22–56%,
which could be ascribed to the firm interfacial bond amid matrix
ascending from the 2-D wrinkled shape with huge surface area of gra­
phene oxide [62]. The strengthening impact of graphene oxide on
concrete strength brands graphene oxide as a capable strengthening
material in concrete composites.
4.3.3. Water permeability property
4.3.3.1. Initial surface absorption test. This test is performed on all 5
combinations of sample mixtures on cubes of 150 mm × 150 mm, that
were cured in water for 28, 56, and 90 days. The rate of absorption was
acquired by measuring the penetration of water onto the concrete sur­
face. The outcomes of this experiment are presented in Fig. 8. It was
revealed that the absorption was more for all the samples at the curing
period of 28 days, in comparison to the samples cured at 56 days. The
lower and higher rate of absorption was noted to be attained by sample
made with inclusion 0.03% and 0.12% of graphene oxide in concrete
composites that was noted to decrease the rate of absorption as
compared to the reference sample by 7.0% and 35% respectively, at
curing age of 90 days. A steady decrease in surface absorption of the
nano-strengthened samples was noted for 28 and 56 days of cured
samples. Previous studies have revealed that adding graphene oxide in
concrete composites produces by congregating sheets of graphene oxide
because of the weaker van der Waals bond with binder matrix [63,64].

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O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

Split Tensile Strength of Concrete (MPa)

4.5

3.5

2.5

1.5

0.5

0
M1 (Control M2 (0.03%-GO- M3 (0.06%-GO- M4 (0.09%-GO- M5 (0.12%-GO-
Sample) SFRC) SFRC) SFRC) SFRC)

7 Days 28 Days 56 Days 90 Days

(a)

30
Percentage (%) Increase in Split Tensile Strength

25

20

15

10

0
7 Days 28 Days 56 Days 90 Days

0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

Fig. 7. (a) Split tensile strength of concrete (MPa), (b) percentage rise in splitting tensile strength at various curing days.

Hence, the samples made with graphene oxide have exhibited minimum
Table 5
surface absorption for different age of curing in comparison to the
Assessment of compressive strength of binder-based fiber-composites strength­
reference sample, which could be because of the graphene oxide acting
ened with graphene oxide.
as a filler, which densifies the matrix at nano-degree and it does not let
Mixture Proportion of Water to Percentage rise in Reference more water molecule absorption at a respective time interval.
description graphene oxide binder compressive
by cement ratio strength at curing of
weight various days 4.3.3.2. Sorptivity. Sorptivity test is performed to oversee the water
Paste 0.02% 0.45 39–65% [33]
absorption rate by measuring the increase in the absorption of water (on
Paste 0.05% 0.45 16–31% [22] one side of the specimen) w.r.t to time. It is noted that sorptivity for the
Mortar 0.01–0.04% 0.40 13–60% [56] samples with the inclusion of graphene oxide as presented in Fig. 9, has a
Mortar 0.1% 0.40 62–85% [54] lower value as compared to the reference sample. The decrease in the
Mortar 0.01–0.030 0.40 27–55% [39]
percentage of rate of absorption was highest for sample made with
Concrete 0.03–0.12% 0.41 22–39% Current
Study 0.12% of graphene oxide at the curing of 90 days which was noted to
45% and the lowest decrease was observed to be 17 of a sample made
with 0.03% of graphene oxide in comparison to reference sample. The
Likewise, nanosheet of graphene oxide when intertwined with further author of the study stated that the insertion of graphene oxide affects the
sheets of graphene oxide becomes placed that acts as a shielding cloak, transport characteristics in the binder matrix improves the gel pores and
that leads to improving the ability against penetration of chemicals. strengthened the microstructure [33,34]. It can be noted that with rise in

8
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

0.045

Inial Surface absorpon (ml/m2sec)

0.035

0.025

0.015
28 Days 56 Days 90 Days

Control Sample 0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

Fig. 8. Initial surface absorption of graphene oxide nano-reinforced concrete.

0.025

0.02
Sorpvity (mm/s1/2)

0.015

0.01

0.005

0
Control Sample 0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

28 Days 56 Days 90 Days

Fig. 9. Sorptivity of concrete samples.

the content of graphene oxide in percentages, the porosity of graphene
oxide reinforced concrete samples is decreased.
4.3.4. Ultrasonic pulse velocity
The characteristics of concrete can be assessed by performing an
ultrasonic pulse velocity test on the concrete samples that were cured in
water for 28, 56, and 90 days. The concrete homogeneity was attained
from that transducer pulse velocity that passes through at a low or high
velocity. Fig. 10 displays the concrete sample quality relative to a
reference sample. The pulse velocity below 3 km/s is considered poor
quality, between 3 and 3.5 km/s is considered medium quality, 3.5–4.5
km/s is considered good quality, and more than 4.5 is considered
excellent quality. It was noted that the velocity of whole concrete
samples that were cured for 28 days was of good class concrete. Samples
cured at 56 days and with 0.12% of graphene oxide had higher velocity
in comparison to the remaining samples that were falling under the
excellent quality. Samples cured at 90 days and with 0.12% of graphene
oxide were noted to have the highest velocity followed by 0.09%,
0.06%, and 0.03% of graphene oxide which fall to excellent concrete
quality. While the velocity of the reference sample had lesser than 4.5
km/s. It could be ascribed to the nano-filler impact of graphene oxide
making the sample dense at the nano-level. Hence, enhancing the con­
crete quality and homogeneity in the concrete durability and mechani­
cal performance.
4.3.5. X-ray diffraction
X-ray diffraction was performed on the graphene oxide reinforced
sample as shown in Fig. 11, which shows the development of (C-S-H)
gels. This is due to the nucleation of calcium silicate hydrate by the
flakes of graphene oxide. It is important to indicate that calcium silicate
hydrate which is developed in hydration of cement is amorphous.
5. Cost-benefit study
The detailed rates for sample preparation are provided in Table 6.
The rate for all the different materials utilized for concrete composites

9
O. Zaid et al. Diamond & Related Materials 124 (2022) 108883

4.5

Average velocity (km/s)

4

3.5

2.5

1.5

0.5

0
Control Sample 0.03%-GO-SFRC 0.06%-GO-SFRC 0.09%-GO-SFRC 0.12%-GO-SFRC

28 Days 56 Days 90 Days

Fig. 10. Ultrasonic pulse velocity of concrete samples.

M1 Mix M2 Mix M3 Mix M4 Mix M5 Mix

12000
SiO2

10000

8000
Lin (Counts)

C-S-H
6000
C-H SiO2
C-S-H CaCO3

4000

2000

0
15 25 35 45 55 65 75 85
(2θ) Scale

Fig. 11. XRD spectra of graphene oxide reinforced concrete sample.

Table 6
Cost-benefit analysis.
Materials (kg) Cost Rs/kg Mixtures

M1 M2 M3 M4 M5

Cement 8.5 3315 3315 3315 3315 3315

Coarse aggregate 1.2 1344 1344 1344 1344 1344
Fine aggregate 1.5 1078.5 1078.5 1078.5 1078.5 1078.5
Graphene oxide 1800 0 1696.5 3393 5089.5 6786
Admixture 120 22.680 22.680 22.680 22.680 22.680
Water 5 925 925 925 925 925
Total rate (PKR) – 6685.18 8381.68 10,078.18 11,774.68 13,471.18
Compressive strength – 36.5 41.8 50.90 60.3 55
EI (strength/rate) – 0.00435 0.00498 0.00501 0.005123 0.00460

was determined by adopting the commercial price. From the mechanical comparison to the other mixes, which depicts that the M4 sample is the
and durability point of view the M5 sample showed the highest per­ ideal candidate for further usage of graphene oxide in cement-based
formance. The economy index (strength/cost) was noted to have the matrices for structural applications and other commercial uses.
highest worth at the M4 sample (with 0.09% graphene oxide) in

10
O. Zaid et al.
6. Conclusion
The present study evaluated the mechanical and durability perfor­
mance of graphene oxide in the concrete. Graphene oxide was added in
different proportions (0.03%, 0.06%, 0.09% and 0.12%) by cement
weight. Based on the different tests the following conclusions are
obtained.
• Inclusion of the graphene oxide with varying proportions by cement
weight in making concrete, has lowered the workability by a sig­
nificant margin due to high specific surface area.
• Addition of graphene oxide and steel fibers improved the mechanical
strength significantly, with compressive strength enhanced by
20–56%, split tensile strength improved by 17–37%.
• Sorptivity and initial surface absorption inclines to reduce with
increment in the amount of graphene oxide for samples cured at 28,
56 and 90 days.
• The ultrasonic pulse velocity illustrated that homogeneity of gra­
phene oxide fiber reinforced cement-based composites stay intact
with the increase in the content of graphene oxide, sample made with
0.12% of graphene oxide has the highest velocity for entirely age of
curing periods in comparison to the reference sample and the
outstanding samples.
• The economy index and the cost analysis showed that concrete
samples reinforced with M4 mix (0.09% of graphene oxide + 2%
steel fibers) are optimal blend on the base of the highest strength
obtained in samples cured at 90 days.
Availability of data
The data is accessible by demand from corresponding author.
Funding
No funding was provided during this research.
Declaration of competing interest
We wish to confirm that there are no known conflicts of interest
associated with this publication and there has been no significant
financial support for this work that could have influenced its outcome.
Acknowledgment
Not applicable.
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