Materials Today: Proceedings 60 (2022) 526–533

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Materials Today: Proceedings

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Durability assessment of high-performance concretes containing

graphene oxide
Boddu Prasuna ⇑, Durga Prasad Ravella
Dept of Civil Engg, VNR Vignana Jyothi Institute of Engineering and Technology, Hyderabad 500090, India

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

Article history: The emphasis to reduce the cement utilization in construction has facilitated the use of mineral admix-
Available online 9 February 2022 ture resulting in an end product with enhanced performance characteristics in environments of severe
exposures. The utilization of ternary and quaternary blends in construction industry been gaining promi-
Keywords: nence due to enhanced performance obtained because of the synergistic effects of various mineral admix-
High performance concrete tures. The work at present is focused on evaluating compressive strength and durability properties
Nano-graphene oxide studies of high-performance concrete incorporating ash (FA), silica fume (SF) and graphene oxide (GO).
Durability studies
The performance characteristics of various combinations of GO-FA, GO-SF and FA-SF-GO are assessed
by formulating a suitable experimental programme. The experimental formulation was designed to eval-
uate the performance characteristics of concretes in marine environment where chloride and sulphate
attack are highly prominent. Parameters were evaluated through various tests like Compressive
Strength, Acid Attack test, Rapid Chloride Penetration test and Cyclic Wetting- Drying test. A relative
comparison of results has been presented, shows that both the ternary and quaternary blended cement
concrete containing combinations of GO-FA, GO-SF and FA-SF-GO have shown better results than the
conventional concrete, mix proportions C8F2G4, C9S1G4, C7F2S1G4 containing 0.04% of GO are showing
higher compressive strength values of 85, 74, 86 MPa for 365 days of fresh water curing, The highest
resistivity values of 103, 109, 94 KO-cm are obtained for the quaternary blended cement mixes,
Lowest RCPT values were achieved by mixes C7F2S1G2, C7F2S1G4, C7F2S1G8 corresponding to quater-
nary blends, The results of cyclic wet dry test have indicated the resistance to chloride permeability in
concretes containing GO is very high in comparison to conventional concretes.
Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the Sustainable Materials
and Practices for Built Environment.

1. Introduction through enhanced pore structure with reduced permeability. There

The production process of cement has been a major contributor
to the greenhouse gases [1], and this has laid emphasis on the engi-
neers to research on alternative binding materials. The primary
requirement to reduce the utilization of cement was successfully
implemented through, partial replacement of cement with various
mineral admixtures like silica fume, metakaolin, rice husk ash, fly
ash, and zeolites etc. These mineral admixtures are either used
individually or as a combination to utilize the synergistic effects
to obtain enhanced performance characteristics. However, recent
studies have revealed that small amounts of Nano additions in con-
crete help in achieving superior performance characteristics
⇑ Corresponding author.
E-mail address: bprasuna.15@gmail.com (B. Prasuna).
have been various attempts to understand the properties of Nano-
titanium Oxide, Nano aluminium Oxide, Nano-silica, carbon nan-
otubes and graphene oxide of various proportions in cement con-
cretes [2–7].
Graphene oxide utilization in cement has been a significant
breakthrough in the field of concrete technology, as the incorpora-
tion of GO in cement composites have resulted in manufacture of
concretes with enhanced strength, toughness, and durability [8].
There is an increment in compressive strength and flexural
strength by incorporation of graphene oxide in cementations sys-
tem. The participation of GO in the process of hydration of cement
has resulted in producing dense pore structure, thereby, reducing
the permeability of concrete which resists the ingress of various
aggressive agents like water, carbon-di-oxide, chlorides, and sul-
phates which cause deterioration [9,10].

https://doi.org/10.1016/j.matpr.2022.01.427
2214-7853/Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the Sustainable Materials and Practices for Built Environment.
B. Prasuna and Durga Prasad Ravella
Most of the researchers have incorporated the GO additions
varying from 0.01% to 0.05% of the cement content. Incorporation
of low amounts of Nano particles poses a problem of achieving uni-
form dispersion in cement concretes, and it has been a major con-
cern to various researchers. However, this was addressed through
the process of sonification where GO is mixed with partial amount
of mixing water and treated with ultrasonic waves using a sonica-
tor to achieve a solution of uniform dispersion, which was mixed in
fresh concrete during the process of manufacturing of concrete
[11]. Thereby, avoiding agglomerates of nanoparticles in cement
concretes. Apart from the improvement in crack resistance through
enhanced compressive and flexural strengths, the variation in
electrical.
Resistance property of composites due to the addition of GO has
made it a potential material in structural health monitoring appli-
cations [13–17].
Most of the works in cement composites containing GO have
been extensively carried out on either cement pastes or cement
mortars or in Ultra High-Performance Concretes (UHPC) and stud-
ies pertaining to conventional cement concretes are very minimal.
Hence the current study was focused to determine the mechanical
and durability characteristics of concretes containing ternary
blended and quaternary blended cements with combinations of
GO-FA, GO-SF and FA-SF-GO respectively [18–25]. The durability
properties were determined by curing the specimens in fresh
water at the end of 90 and 365 days, in order to eliminate the
effects of any delay in hydration due to addition of mineral admix-
tures like FA. All the concretes were exposed to extreme exposure
conditions to evaluate deterioration characteristics.
2. Materials and methods
2.1. Materials
OPC cement of grade 53 procured from Penna Cements was
chosen for this investigation and the characteristics were con-
firmed to the requirements specified by IS: 12269 [30] for OPC
53 grade respectively. Class-F Fly ash and Silica fume were
obtained from Rama Gundam Power Plant and Elkem industries
respectively. A Poly-carboxylic ether based super plasticizer was
used to achieve the required workability. Graphene Oxide with
99.5% purity was procured from Nano-Research lab, New Delhi.
River sand and crushed aggregates (20 mm and 10 mm) were used
as fine and coarse aggregate respectively [26,27].
The chemical composition of cement consists of Cao which con-
trols the strength and soundness of the cement, SiO2 gives strength
and excess of it causes cement to set at lower rate, Al2O3 causes
cement to set at quicker rate and excess of it can reduce the
strength, Fe2O3 is responsible for the colour, MgO colour and hard-
ness. The chemical composition of the Class-F Fly is SiO2 48.91%,
Al2O3 31.92%, CaO 5.23%, Fe2O3 7.89%, MgO 0.32%, So3-
1.81%, Na2O- 0.36%. the specific gravity of the cement, fly ash, silica
fume is 2.97, 2.01, and 2.19.
2.2. Mix proportions
The enhancement in performance of cement concretes due to
the utilization of ternary and quaternary blended cements have
been well established [12]. The primary motivation of the work
was to study the effect of nano-GO additions on durability proper-
ties of cement concrete containing blended cements, here the GO is
the additive which is added by the % weight of the cement. To start
with conventional cement concrete was designed to achieve
strength of 60 MPa at the end of curing for 28 days as per the
guidelines in IS-10262: 2019[28], which was further verified
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Materials Today: Proceedings 60 (2022) 526–533
through the laboratory trial mixes. The Table 1 shows the concrete
mixes set for the formulated experimental evaluations. The mixes
were formulated specifically in three sets with combinations of FA-
GO, SF-GO and FA-SF-GO. The set of mixes in FA-GO combination
consisted of 20% FA as partial replacement of cement with 0.02%,
0.04% and 0.06% of GO additions respectively titled as C8F2G2,
C8F2G4 & C8F2G6 respectively. Mixes in SF-GO combinations were
titled as C9S1G2, C9S1G4 & C9S1G6, which had 10% of cement
replaced with silica fume with 0.02%, 0.04% and 0.06% of GO
respectively. Final set of quaternary blended mixes in FA-SF-GO
system consisted of 20% FA and 10% SF as partial replacement of
cement with 0.02%, 0.04% and 0.06% of GO, which were designated
as C7F2S1G2, C7F2S1G4 and C7F2S1G6 respectively. The percent-
age of FA and SF were fixed based on results available in literature
to obtain optimized performance characteristics [11]. The GO was
dispersed uniformly in the concrete mixture after preparing a solu-
tion through the process of sonification by utilizing an ultrasonic
sonicator (see Fig. 1).
2.3. Experimental investigations
In accordance with IS: 516-2019[29] compressive strengths
were determined at the end of 7, 28, 90 and 365 days for all the
concrete specimens. The 100 mm concrete cube specimens cured
in water for a period of 365 days were also exposed to acidic envi-
ronment by immersing them in 3 N Sulphuric Acid, loss in weight
and loss in strength were determined at the end of 45 and 90 days
of immersion respectively. The concentration of acid was evaluated
periodically to maintain it as a constant throughout the period of
immersion. Using a two-probe technique at the end of 28 and
90 days of curing in fresh water in accordance with CEB-FIP 1989
[32] the variation in electrical resistivity was measured, as shown
in Fig. 2 on cube of 100 mm size.
The samples of 100 mm dia and 50 mm height were used for
test of resistance to chloride penetration through Rapid Chloride
Penetration Test (RCPT) at the end of 90 days and 365 days of
freshwater curing. The RCPT test was conducted in according to
ASTM 1202 [31] as shown in Fig. 3.
A set of reinforced and unreinforced specimens were tested for
chloride ingress and its effect on corrosion of reinforcement
through cyclic wetting and drying process. Each cycle consisted
of 7 h of heating at 105 °C, followed by 1 h of exposure to room
temperature followed by 16 h of immersion in 3% Sodium Chloride
solution. The unreinforced specimens subjected to cyclic wet dry
process were cubes of 100 mm size, which were painted on 5 sides
with an epoxy-based paint and one side was left open to facilitate a
unidirectional ingress of chloride into the concrete. The ultrasonic
pulse velocity was also measured for all the cubes subjected to cyc-
lic wet-dry process to evaluate if there are any micro structural
changes occurring which can be identified through the change in
velocity. The reinforced specimens consisted of a cylinder of
100 mm diameter and 200 mm height reinforced with a 12 mm
Fe550 steel bar which was embedded to a depth of 180 mm at
the center of the cylinder. The corrosion of embedded steel was
measured through Half-Cell potential using a cu/cuso4Electrode
as shown in Fig. 4.
3. Results & discussions
3.1. Compressive strength
Concretes containing SF-GO and FA-SF-GO achieved strengths
lower than the conventional concrete at 28 days of freshwater cur-
ing. The concrete containing FA-GO achieved strengths slightly
higher than conventional concrete at the end of 28 days of fresh-
B. Prasuna and Durga Prasad Ravella Materials Today: Proceedings 60 (2022) 526–533

Table 1
Mix proportions formulated for experimental investigations.

MIX Designation Cement Fly ash Silica Fume Water Fine aggregate Coarse aggregate Graphene oxide (gm/m3) % SP by cement weight
(Kilogram per cubic meter)
NC 500 - - 190.0 770.0 940.0 - 0.45
C8F2G2 400 100 – 190.0 770.0 940.0 100.0 0.4
C8F2G4 400 100 – 190.0 770.0 940.0 200.0 0.4
C8F2G6 400 100 – 190.0 770.0 940.0 300.0 0.4
C9S1G2 450 – 50 190.0 770.0 940.0 100.0 0.5
C9S1G4 450 – 50 190.0 770.0 940.0 200.0 0.5
C9S1G6 450 – 50 190.0 770.0 940.0 300.0 0.5
C7F2S1G2 350 100 50 190.0 770.0 940.0 100.0 0.45
C7F2S1G4 350 100 50 190.0 770.0 940.0 200.0 0.45
C7F2S1G6 350 100 50 190.0 770.0 940.0 300.0 0.45

Fig. 1. Sonification procedure adopted to achieve uniform dispersion Of GO in

Fig. 3. Evaluation of resistance to chloride ingress using RCPT Test.
Water.

Fig. 2. Test Setup to measure resistivity of concrete cubes. Fig. 4. Evaluation of Half-cell Potential using Cu/CuSO4 electrode.

water curing. However, at the end of 90 days and 365 days
strengths achieved by all the concrete mixes were superior to con-
ventional concrete. The concrete mixes C8F2G4, C9S1G4 and
C7F2S1G6 achieved a highest strength of 73 MPa, 73 MPa and
82 MPa at 90 days fresh water curing. After 365 days of fresh water
curing the strengths attained by concretes C8F2G6, C9S1G6,
C7F2S1G4 were 86, 76, 86 MPa respectively. However, in each
set the strengths obtained by concrete containing 0.04% and
0.06% of GO had marginal difference in strength. The values of
compressive strengths achieved at 28, 90 and 365 days have been
tabulated in Table 2.
The concretes containing SF-GO and FA-SF-GO achieved lower
strength at the end of 28 days in comparison to conventional con-
crete due to the presence of excessive fines with increased in the
528
specific surface area demanding high water content. But the end
of the 90 and 365 days the strength achieved for the ternary and
quaternary blended concrete mixes are due to the secondary poz-
zolanic reaction and filler ability of the admixtures added (see
Figs. 5a-c).
3.2. Resistivity
Determination of electrical resistivity is to evaluate the likely
rate of corrosion of steel in concrete which is highly significant
in concrete used in marine environment.
Table 2 shows the values of resistivity measured at 28 and
90 days of freshwater curing. The concretes containing mineral
admixtures and Nano additions have achieved values higher than
B. Prasuna and Durga Prasad Ravella Materials Today: Proceedings 60 (2022) 526–533

Table 2
Results of Compressive strength, Resistivity and RCPT values.

MIX Designation Compressive strength (MPa) Resistivity (KO-cm) RCPT values (coulomb)
7D 28 D 90 D 365 D 28 D 90 D 90 D 365 D
NC 57.00 60.00 66.00 69.00 10.00 20.00 971.00 727.38
C8F2G2 45.00 61.00 69.00 75.00 68.00 85.00 382.00 95.00
C8F2G4 47.00 62.00 73.00 85.00 78.00 94.00 293.00 140.00
C8F2G6 42.00 62.00 72.00 86.00 70.00 84.00 382.00 170.00
C9S1G2 46.00 48.00 64.00 74.00 27.00 31.00 952.00 591.00
C9S1G4 45.00 55.00 73.00 74.00 26.00 30.00 1046.00 566.00
C9S1G6 51.38 56.00 72.00 76.00 17.00 22.00 1461.00 817.00
C7F2S1G2 39.00 53.00 73.00 82.00 72.00 103.80 314.00 125.00
C7F2S1G4 34.00 52.00 80.00 86.00 94.00 109.00 249.00 146.00
C7F2S1G6 41.00 56.00 82.00 85.00 78.00 94.00 283.00 188.00

Fig. 5a. Variation of Compressive Strength of the mixes containing Fly ash and NC Fig. 5c. Compressive Strength with age of concrete mixes containing fly ash, silica
with the age. fume and NC with the age.

3.3. Acid attack test

Acid attack test was carried out to evaluate the deterioration

characteristics of the proposed concrete mixes, as to simulate the
effect of sulphate attack on structures used in the vicinity of chem-
ical industries and in coastal areas. Cube specimens of size 100 mm

Fig. 5b. variation of Compressive Strength of the mixes containing silica fume and
NC with the age.

conventional concrete at all the ages which could be attributed to

its superior ability to resist corrosion. Due to enhanced pore struc-
ture with reduced permeability. The mixes containing SF, FA and
GO which are quaternary blended cements exhibited highest resis-
tivity values of 104, 109 and 94 KO-cm respectively. However, all
the concretes achieved higher resistivity at the end of 90 days in
comparison to values achieved at the end of 28 days, due to the
reduction in porosity with occurrence of secondary pozzolanic Fig. 6. Variation of percentage loss in weight in samples exposed to Acidic
reaction. environment.

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B. Prasuna and Durga Prasad Ravella Materials Today: Proceedings 60 (2022) 526–533

sizes were immersed in 3 N sulphuric acid solution to evaluate the

percentage loss in weight and strength.
The results are presented in Fig. 6 and Fig. 7 respectively. These
specimens were exposed to acidic environment after 365 days of
freshwater curing. The Percentage loss in weight was minimum
in the mix C8F2G4 at the end of 45 days of immersion and the
mix C8F2G6 exhibited the lowest value in terms of loss in weight
at the end of 90 days of immersion. However, concretes containing
quaternary blended cements exhibited the least values of percent-
age loss in strength at 45 and 90 days of immersion exhibiting
superior performance characteristics due to reduced ingress of sul-
phate because densified pore structure formation due to superior
packing density. The set of mixes containing GO-SF exhibited
higher loss in strength in comparison to conventional concrete
and other two sets of concrete containing GO-FA and FA-SF-GO.

3.4. Rapid chloride penetration test Fig. 8. RCPT values of specimens tested at the end of 90 days and 365 days of
curing.
All the concrete specimens tested for its resistance to chloride
ingress through Rapid Chloride Penetration Test in accordance
with ASTM 1202 as this provides data with regard to chloride
ingress into the concretes exposed to marine environment.
The results of RCPT values obtained at the end of 90 days and
365 days curing of samples in fresh water have been shown in
Table 2 and Fig. 8. The RCPT values attained at the 365 days of cur-
ing were less than those obtained at 90 days which can be attrib-
uted to the change in the microstructure due to hydration at
later ages due to the presence of mineral admixtures. The least
value of RCPT was exhibited by the mix C8F2G2 with negligible
chloride permeability. However, all the concretes exhibited very
low chloride permeability with values less than 1000 Coulombs.
At 90 and 365 days the mixes C9S1G2, C9S1G4 and C9S1G6 shown
relatively higher values when compared to other concretes.
The correlation of 90 and 365 days RCPT values with 28 days
and 90 days of resistivity have been presented in Fig. All the three
sets exhibited a linear variation and the RCPT values reduced with
an increase in Resistivity value. Respective equations have been
presented in the graphs with correlation coefficient in Fig. 9.
The correlation studies of resistivity of concrete with RCPT val-
ues was done as both the tests depend on the electrical resistance
of concrete. The R2 values determined with 365 days RCPT test
Fig. 9a. Correlation of 90 day RCPT values with Resistivity values of 28 days.
were more coherent with values of 0.90 and 0.92 in comparison

to 0.87 and 0.89 obtained by plotting resistivity against 90 days

RCPT value.
This phenomenon of increased R2 values can be attributed to
the densification of concrete pore structure after 365 days of curing
in fresh water in comparison to those cured till 90 days.
The linear equation was chosen as resistivity of concrete is a
qualitative assessment with values varying from 5KO-cm, as pro-
posed in with CEB-FIP 1989 corresponding to very high and negli-
gible rate of corrosion.

3.5. Cyclic wetting-drying test

The cyclic wetting-drying test was done to study the ingress of

chloride into the concrete through an accelerated technique. This
process of simulation is normally used to simulate the splash zone
in structures like jetty’s submerged in ocean.
As mentioned above a set of unreinforced and reinforced spec-
imens were subjected to cyclic wetting and drying process. The
ultrasonic pulse velocity of cube specimens was evaluated and
Fig. 7. Variation of percentage loss in strength in samples exposed to acidic the results corresponding to the variation of UPV with No. of cycles
environment. have been presented in Fig. 10. The ultrasonic pulse velocity of NC
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B. Prasuna and Durga Prasad Ravella Materials Today: Proceedings 60 (2022) 526–533

Fig. 9d. Correlation of 365 days RCPT values with Resistivity values of 28 days.
Fig. 9b. Correlation of 90 day RCPT values with Resistivity values of 28 days.

Fig. 10. Variation of UPV with No. of Cycles.

Fig. 9c. Correlation of 365 days RCPT values with Resistivity values of 28 days.

witnessed a higher rate of reduction in comparison to the other

concretes containing blended cements. Depicting a relatively
higher rate of deterioration but all other concretes with superior
performance characteristics showed a relatively lower rate of dete-
rioration. The cube specimens were broken by conducting a split
tensile test and the depth of chloride penetration was evaluated
by spraying 0.1 N Silver Nitrate solution. The formation of Gray col-
our indicated the depth of chloride penetration as shown in Fig. 11.
The results corresponding to depth of penetration have been pre-
sented in Table 3. The depths of penetration of chloride in con-
cretes containing quaternary blends were found to be least with
values of 5 mm 3 mm and 0 mm respectively. Due to dense pore
structure and reduced permeability. Fig. 11. Evaluation of chlorin penetration depth using silver nitrate.

Specimens with embedded reinforcement have been tested for

its corrosion through variation of half-cell potential with No. of
C8F2G6 exhibited cracks at the end of 21 and 20 cycles respec-
cycles. The variation of half-cell potential measured with cu/cuso4
tively. However, all the concretes containing SF exhibited cracks
electrode has been presented in Fig. 12. The conventional concrete
almost after 30 cycles. The half-cell potential value at the time of
exhibited cracking at the end of 21 cycles however the other con-
cracking has been presented in Table 3. These results are well in
cretes exhibited cracking at later. The concrete mixes C8F2G4 and
coherence with results obtained in all the pervious tests.

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B. Prasuna and Durga Prasad Ravella
Table 3
Results corresponding to cyclic wetting–drying test.
MIX Designation Cycle No at which initial
crack was observed
NC 21
C8F2G2 29
C8F2G4 21
C8F2G6 20
C9S1G2 30
C9S1G4 32
C9S1G6 33
C7F2S1G2 31
C7F2S1G4 30
C7F2S1G6 33
Fig. 12. Variation of Half-cell Potential with No. of Cycles.
4. Conclusions
An experimental program was formulated with various combi-
nations of ternary and quaternary blends with combinations of FA-
GO, FA-SF and FA-SF-GO. A relative comparison of results corre-
sponding to mechanical and durability characteristics have been
evaluated and presented.
 The mechanical characteristics of combinations containing sup-
plementary cementitious materials exhibited higher values at
90 and 365 days respectively in comparison to normal concrete.
Most of the concretes achieved lower strengths at the end of 7
and 28 days when compared with NC. But at later ages the
strength increase was higher in concretes containing mineral
admixtures due to the secondary pozzolanic reaction. The high-
est strength was achieved by C7F2S1G4with a value of 86 MPa.
 The mix proportions C8F2G4, C9S1G4, C7F2S1G4 containing
0.04% of GO are showing higher strength values of 85, 74,
86 MPa.
 The resistivity values depicting the corrosion characteristics of
concrete were found to be highest at 365 days in concretes con-
taining quaternary blends. Where a value of 103, 109, 94 KO-cm
are obtained for the quaternary blended cement mixes and the
value of the ternary blended mixes of FA-GO are showing higher
resistivity values of 85, 94, 84 KO-cm when compared to the SF-
GO mixes. However, all the concretes have shown higher resis-
tivity in comparison to conventional concrete at all the ages
exhibiting a superior resistance to corrosion of steel in concrete.
 Results of RCPT exhibited a trend similar to variation in resistiv-
ity values. Lowest values were achieved by mixes C7F2S1G2,
C7F2S1G4, C7F2S1G8 corresponding to quaternary blends with
Materials Today: Proceedings 60 (2022) 526–533
Half-Cell Potential (mV) of Depth of chlorine penetration (mm) for 15 cycles
cycle where initial crack is formed of cyclic wetting -drying of concrete cubes
700 45.00
706 10.00
748 11.00
738 4.00
730 5.00
835 7.00
760 10.00
680 5.00
705 3.00
757 0.00
the values of 314, 249, 283 coulombs and 125, 146, 188 cou-
lombs for 90 and 365 days, when compared to other ternary
mixes.
 The correlation between resistivity and RCPT was studied as
both are a variant of fundamental electrical resistance of the
material. At the end of 365 days R2 values increased indicating
the changes in pore structure at micro level.
 The results of cyclic wet dry test have indicated the resistance
to chloride permeability in concretes containing GO is very high
in comparison to conventional concretes. The results of UPV
measured on cubes subjected to cyclic wetting and drying indi-
cate a deterioration occurring internally which is quite evident
from the reduction of UPV values, which can be attributed to
change in microstructure.
CRediT authorship contribution statement
Boddu Prasuna: Conceptualization, Methodology, Writing –
original draft. Durga Prasad Ravella: Methodology, Supervision.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
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