Innovative Infrastructure Solutions (2021) 6:5

https://doi.org/10.1007/s41062-020-00378-9

TECHNICAL PAPER

Effect of graphene oxide on high‑strength concrete induced with rice

husk ash: mechanical and durability performance
T. Shanmuga Priya1 · Ashna Mehra1 · Samyak Jain1 · Kunal Kakria1

Received: 10 August 2020 / Accepted: 19 September 2020

© Springer Nature Switzerland AG 2020

Abstract
The global shift to usage of eco-friendly materials has driven a movement for the utilization of many additives in construction
practices. Moreover, the application of nanomaterials has also been increased for enhancing the performance of concrete.
This paper primarily focuses on the reinforcing effects of graphene oxide (GO) on high-strength concrete (HSC) made with
and without rice husk ash (RHA). Cement was replaced with 10% RHA by weight. GO was added in different proportions
of 0.025, 0.050, 0.075 and 0.1% by weight of cement. Performance of engineered mixes was evaluated as mechanical (com-
pressive, flexural and splitting tensile strength), durability (water absorption, sorptivity, rapid chloride penetration and acid
resistance) and microstructural (SEM and EDAX). The results depicted that mechanical and durability properties of HSC
increased significantly on the incorporation of GO and further increased with partial replacement of cement with 10% RHA.
The optimum performance in terms of mechanical and durability properties was achieved by a combination of 10% RHA and
0.075% GO. Increasing the percentage of GO beyond 0.075% results in drop-in strength and durability properties. Further-
more, the microstructural studies indicated that the mixes containing both RHA and GO exhibited a denser microstructure,
by consuming calcium hydroxide and producing additional C–S–H gel in the matrix, concluding the practicability for use
of GO and RHA in HSC.

Keywords  Graphene oxide · Calcium silicate hydrate · Rice husk ash · Scanning electron microscopy · High-strength
concrete

Introduction crack formation and lower resistance to fracture [2]. Recent

researchers argued that fibres play a considerable role in con-
The usage of concrete in the construction industry has trolling the cracks which develop when cementitious materi-
been going for over a hundred years in buildings, roads als are mixed with different combinations [3]. Several prob-
and bridges. Concrete possesses high compressive strength lems such as bleeding, early cracking and segregation arise
and lower flexural properties than most other construction due to concrete’s viscosity and heterogeneous consistency
materials [1]. However, traditional concrete does not have [4, 5]. Incorrect proportioning of concrete at the time of mix-
the requisite properties or strength to meet the require- ing leads to fallible concrete viscosity. To overcome such dif-
ments of modern infrastructure because of its high risk of ficulties, nanomaterials such as graphene oxide (GO), nano-
TiO2, nano-SiO2 have recently gained importance in the
* T. Shanmuga Priya construction industry due to its distinctive properties such
shanmugapriya.t@vit.ac.in as ultra-fine size and its impact on strength and rheological
Ashna Mehra characteristics of cement paste [6, 7]. The usage of nanoma-
ashna.mehra2016@vitstudent.ac.in terials in the cement paste results in the improvement of the
Samyak Jain cementitious properties due to the pore-filling effect of the
samyak.jain2016d@vitstudent.ac.in materials and the pozzolanic reaction which occurs in the
Kunal Kakria cement paste [7]. In comparison with conventional construc-
kunal.kakria2017@vitstudent.ac.in tion materials, some distinctive characteristics of nanoma-
terials are its higher tensile strength, specific surface area
1
School of Civil Engineering, Vellore Institute of Technology, and elastic modulus [8–10]. Amongst all the reinforcement
Vellore, India

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materials available for concrete, GO has received consid-
erable attention because it has several advantages over
other materials. Previous studies have revealed that GO is
a rare monomolecular nanomaterial obtained from graph-
ite with different arrangements of oxygen functionalities
[11]. According to studies [12, 13], excellent mechanical
behaviour of GO–cement composites is usually because of
the nucleation sites formed due to substantial surface area
and excellent interfacial bond of GO with the cement paste.
Studies of Li et al. [14] discussed the usage of GO in con-
crete which further enhances the flexural strength because of
its unique morphology characteristics. According to Ghazi-
zadeh et al. [15], GO caused the acceleration in hydration
of Portland cement due to its plating profile. Shang et al. [4]
studied the influence of GO on the cement mortar properties
such as workability, segregation and bleeding and concluded
that GO resulted in the betterment of aforementioned prop-
erties. According to Long et al. [16], addition of different
percentages of GO with construction wastes and its applica-
tions as an additive have several advantages, as it leads to an
overall improvement in the properties of concrete. Previous
studies reported that on reinforcing the cement paste with
GO helps in formation of calcium silicate hydrate (C–S–H)
gel, and hence improving the concrete’s overall performance
[17, 18]. To transform concrete into a more economical and
sustainable material, many admixtures are partially added to
cement-like fly ash, GGBS, etc., amongst which rice husk
ash (RHA) is known to have the highest amount of silica
(87–97%) which is beneficial for pozzolanic reaction in
cement along with increasing the binding and strength of
interfacial transition zones [19–21]. The similarity between
the properties of RHA and cement makes RHA a very com-
pliant replacement material for ordinary Portland cement
(OPC) [22]. India is a leading producer of rice, contributing
around 20 million tonnes of RHA to the world, which has
the potential to be used as an eco-friendly and economical
supplementary cementitious material to enhance the proper-
ties of the cement [23]. The properties of concrete enhanced
by the addition of RHA include setting time, internal pore
structure and mechanical performance [24]. According to
De Sensale [25], the mechanical strength of the cement paste
was improved when RHA was incorporated in the concrete
mixes. He concluded that the partial substitution of cement
paste with RHA resulted in improvements at the microstruc-
tural level due to the enhancement of pozzolanic reaction.
According to Nguyen [26], the usage of RHA in cement
paste leads to the development of a denser C–S–H matrix.
The microstructural development of RHA concrete starts
after 1 h of mixing RHA with cement before which hydra-
tion products are formed on the top of the RHA. Forma-
tion of a hexagonal plate-like structure is developed on the
surface of RHA, because of the reaction between RHA and
Ca(OH)2 due to cement hydration, densifying the matrix
13
Innovative Infrastructure Solutions (2021) 6:5
[27]. According to Kang et al. [28], the inclusion of RHA
enhances the mechanical strength of the concrete because
of its action as a reactive filler in between cement parti-
cles. Moreover, experimental data depicted that the concrete
gained maximum compressive strength after 91 days with
a limiting value of 200 MPa under favourable conditions.
According to Malhotra and Mehta [29], the substitution
of cement with fine rice husk ash resulted in a mix with
enhanced mechanical properties and lowered water absorp-
tion due to increased particle packing.
According to Habeeb and Mahmud [30], 10% substitu-
tion of cement with RHA was optimal because on further
incrementing the percentage of RHA, the densification of
the matrix was found to reduce. This reduction in densifi-
cation was because of the lesser amount of C–H released,
thus being insufficient for completely reacting with all the
available silica, which acts as a dormant material. According
to Ahsan and Hossain [22], on increasing the RHA con-
tent to more than 10% of cementitious material, a decrease
in strength was observed. Moreover, densification of the
microstructure was observed when 10% RHA was used, as
it strengthened the interfacial transition zone (ITZ) due to
the silica content present in RHA. Antiohos et al. [31] stud-
ied the concrete samples by adding RHA (0–30%) to the
specimens and concluded that those samples in which RHA
of 7000 cm2/g was added gave extraordinary results in terms
of the development of strength, 10% replacement being opti-
mum. Moreover, the water absorption tests concluded that
the concrete which contained RHA had much lower water
absorption capacity in comparison with the conventional
concrete. On partial substitution of RHA, rapid chloride pen-
etration test (RCPT) results showed a decrease in the charge
transfer because of the densification of the matrix [32]. How-
ever, due to cement’s nature of consuming a large amount of
energy, it is responsible for over 7% of the world-wide ­CO2
emissions [33]. One possible alternative to minimize these
environmental issues is to use a greener, economical and a
more sustainable RHA incorporated concrete [34, 35]. The
addition of rice husk ash in cement pastes has reduced C ­ O2
footprint significantly and has also solved the issues related
to landfilling [36].
Research objective
Incorporation of GO in our study was because it could be
synthesized in large amounts from reasonable graphite pow-
der. Usage of eco-friendly and economical materials such
as GO and RHA together was expected to complement each
other and improve the cementitious properties of the final
concrete mix by producing an optimal mix in terms of den-
sification of the compound microstructure. Many research-
ers have used RHA in concrete as one of the pozzolanic
Innovative Infrastructure Solutions (2021) 6:5 Page 3 of 16  5

Table 1  Chemical properties of OPC and RHA Table 2  Fine and coarse aggregate properties
Compound Proportion (%) Property Fine aggregate Coarse aggregate
OPC RHA Fineness modulus 2.37 6.72
SiO2 18.91 86.9 Bulk density (kg/m3) 1670 1526
Al2O3 4.51 0.24 Water absorption (%) 1.2 0.8
MgO 0.87 0.34
Fe2O3 4.94 0.10
K2O 0.43 2.11

Cumulative Passing Percentage

100
CaO 66.67 1.03
Na2O 0.12 0.11
80
SO3 2.5 0.14
Loss due to ignition 1.05 1.53 60

40
materials, but a minimal investigation has been carried out
on the usage of RHA and GO together for the production of 20
concrete. Although there were a few studies on the addition
of GO in cement composites, the impact of different percent- 0
ages of GO in high-strength concrete is unexplored. The 0.1 1 10 100
Sieve size (mm)
present study investigates the use of different percentages of FA CA
GO (0.025%, 0.050%, 0.075% and 0.1%) with and without
partial replacement of cement by RHA (10% by weight) in
Fig. 1  Cumulative passing percentage of coarse aggregate (CA) and
concrete. Moreover, applications of GO and RHA together fine aggregate (FA)
mark originality in concrete and is expected to enhance the
mechanical strength and durability characteristics of the
engineered mix. Furthermore, the samples were analysed for Table 3  Properties of GO [39]
mechanical and durability properties and cross-referenced at Parameters Description
the microstructural level using SEM–EDAX analysis.
Colour Greyish liquid
Fineness <5 µm
Surface tension 35 dyne/cm
Experimental investigation Density 1.1 g/cm3
Viscosity 15 Pa. S at 25 °C
Materials Boiling point 100 °C
Dispensability Water, ethanol,
In this study, OPC of Grade 53 (Zuari Cement Ltd.) was IPA- (polar
solvents)
used. The specific gravity and surface area of OPC were
3.14 and 344 m2/kg, respectively. RHA is considered to be
a highly reactive pozzolan, which was obtained by calci-
nation of rice husks below temperatures of 780 ͦ C. RHA Graphene was obtained from Ad-Nanotechnologies,
was collected from Sri MKS Distributor, Vellore, Tamil Bengaluru, Karnataka (India) and was added as nanofillers
Nadu, India. The specific surface area and specific grav- without any further processing. GO used in this study was
ity of RHA are 364 m2/kg and 2.32, respectively. Table 1 extracted from graphite and was prepared to a powdered
shows the chemical properties of OPC and RHA as observed form, accordance with modified Hummer method [38]. Dis-
from X-ray fluorescent (XRF). In this research, 4.75-mm- tilled water was used to disperse GO and make a solution of
sized river sand was used as a fine aggregate. The specific 0.89 mg/ml [39]. The characteristics of GO are mentioned
gravity of the fine aggregates used was 2.65 and it complies in Table 3 [39].
with zone II of IS 383:2016 [37]. The 12.5-mm-sized coarse
aggregates having a specific gravity of 2.81 were used in Mixture proportions
this study. The properties of the aggregates used are men-
tioned in Table 2. The cumulative passing percentage curve In this research, the effects of addition of GO in high-
of coarse and fine aggregate is shown in Fig. 1. strength concrete with and without 10% RHA were

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 5  Page 4 of 16 Innovative Infrastructure Solutions (2021) 6:5

evaluated, expecting strength developments, better durabil-
ity and microstructural properties. Ten batches of modified
concrete samples were cast and the description for mixes
is given in Table 4. M-40 grade concrete was prepared in
accordance with IS 10262: 2009 [40] for this study and
the mix proportions in kg/m3 are presented in Table 5. The
water–cement ratio used for the mixes was considered as
0.45.
The specimens were cast into two sets, (a) incorpora-
tion of GO in steps of 0.025%, 0.05%, 0.075% and 0.1%
of cement; (b) partial substitution of cement by 10% RHA
and incorporation of GO varying from 0 to 0.1% by weight
of cementitious materials (cement + RHA). Moreover, two
controlled samples were also cast as mentioned in Table 4.
Testing procedures
All the materials were kept at room temperature
(27 °C ± 2 °C) to maintain a uniform mixing temperature.
A pan mixer was used to mix all the materials. The mixing
of materials was done for 7 min to ensure a standardized
mix. After mixing the materials, the concrete was compacted
in three layers using the vibration table apparatus. The
specimens were cured using tap water at a temperature of
27 °C ± 2 °C.
Mechanical strength
The compressive strength test was performed according to
IS 516:1959 [41], using 100 mm × 100 mm × 100 mm sized
cubes. For every mix, nine cubes were cast and the strength
was determined after 3, 7 and 28 days of curing. AIMIL
compression testing machine was used to perform the test
with a uniform load rate of 2.5 kN on the cubes. A prism of
size 100 mm × 100 mm × 500 mm was used to conduct the
flexural test, and the test was performed in accordance with
IS 516:1959 [41]. A total of six beams was cast to test the
flexural strength after a period of 7 and 28 days. A cylinder
of size 100 mm (diameter) and 200 mm (height) was cast for
different concrete mixes for performing the splitting tensile
strength test. For each mix, three specimens were cast to
perform the splitting tensile strength test for a period of 7
and 28 days. The test was performed in accordance with IS
5816: 1999 [42] under a uniform load rate of 2.5 kN.

Water absorption and sorptivity

Table 4  Details of mix IDs
Mix ID Description The water absorption test was performed using
100  mm × 100  mm × 100  mm sized cube specimens in
RHA0 GO-0 Controlled concrete mix without GO and RHA
accordance with ASTM C 642:1997 [43]. The test was per-
RHA0 GO-1 Concrete mix with 0.025% GO
formed by immersing the specimens in water for a period of
RHA0 GO-2 Concrete mix with 0.05% GO
28 and 90 days, and then oven drying them for 24 h at a tem-
RHA0 GO-3 Concrete mix with 0.075% GO
perature of 105 °C ± 10 °C. After the specimen was oven-
RHA0 GO-4 Concrete mix with 0.1% GO
dried for over 24 h, the weight of the sample was recorded
RHA10 GO-0 Concrete mix with 10% RHA
as the specimen’s dry weight. The specimen’s wet weight
RHA10 GO-1 Concrete mix with 10% RHA and 0.025% GO
was determined after immersing the specimen in water for
RHA10 GO-2 Concrete mix with 10% RHA and 0.05% GO
48 h. Recently, sorptivity has gained a lot of importance in
RHA10 GO-3 Concrete mix with 10% RHA and 0.075% GO
checking the concrete’s durability, in terms of measuring
RHA10 GO-4 Concrete mix with 10% RHA and 0.1% GO
the amount of water absorbed in the unsaturated concrete

Table 5  Details of mix design Mix IDs Cement (kg/m3) RHA (kg/m3) GO (kg/m3) Fine aggre- Coarse Water (kg/m3)
gate (kg/ aggregate
m3) (kg/m3)

RHA0GO-0 420 0 0 826 1190 168

RHA0 GO-1 420 0 0.105 826 1190 168
RHA0 GO-2 420 0 0.210 826 1190 168
RHA0 GO-3 420 0 0.315 826 1190 168
RHA0 GO-4 420 0 0.420 826 1190 168
RHA10 GO-0 378 42 0 826 1190 168
RHA10 GO-1 378 42 0.105 826 1190 168
RHA10 GO-2 378 42 0.210 826 1190 168
RHA10 GO-3 378 42 0.315 826 1190 168
RHA10 GO-4 378 42 0.420 826 1190 168

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Innovative Infrastructure Solutions (2021) 6:5 Page 5 of 16  5
samples. The sorptivity test was performed on 100-mm cube
specimens, by immersing the samples in water for 28 days in
accordance with ASTM C 1585: 2013 [44]. After curing, the
specimens were oven-dried and the weight of the specimen
was noted. The second weight was noted after submerging
the specimen in a certain water level, which was less than
5 mm above the base of the sample. The flow from the sides
of the specimen was restricted by the usage of the non-absor-
bent coating. The tests were performed after 28 and 90 days.
Rapid chloride penetration test
Ingress of chloride ions is one of the most common causes
for corrosion of reinforcement steel. This phenomenon
leads to a severe decrease in the load-bearing capacity of
concrete structures. Hence, to minimize the potential dam-
age of concrete due to chloride-induced corrosion, a proper
assessment of chloride permeability is necessary. RCPT was
conducted based on ASTM C 1202: 2009 [45] for a period
of 28 and 90 days. The test was performed with 60 volt-
age DC and maintained throughout the sample. The charge
which passed through the specimen was noted and a quali-
tative rating was then estimated, based on the permeability
of the concrete. The quantity of current passing through the
specimens (50 mm thickness and 100 mm diameter) for 6 h
was monitored. The test was conducted by immersing the
specimen into two different sample cells containing 3% salt
solution and 0.3 N solution of sodium hydroxide. Depend-
ing upon the charge that travelled through the specimen,
a qualitative rating was estimated based on the concrete’s
chloride permeability.
Acid resistance test
Acid resistance test was performed on cubes of 100-mm-
sized specimens for 28 days by submerging the concrete
samples in an acid solution. The specimens were wiped with
a soft brush before performing the test. The specimen’s ini-
tial weight was noted and then submerged in diluted water
with 3% H ­ 2SO4 by weight, for a period of 28 and 90 days
[46]. A constant pH of 4 was maintained throughout the
testing period. After the test was conducted, the weight of
the sample was noted again. Thereafter, the percentage loss
in weight and compressive strength was estimated.
SEM and EDAX
SEM is a highly advanced and accurate analytical system
which makes use of beams of electrons to produce enlarged
surface images of the required area. The raster scan image
which is generated can target a resolution higher than 1 nm.
Before being considered for SEM analysis, the sample
was broken down into smaller sections by grinding, after
undergoing the compressive strength test. Thereafter, the
specimens were thoroughly cleaned and oven-dried at
96 °C. To experiment, the specimens were converted to a
powdered form, which passed through a 75-micron sieve.
Furthermore, the uncoated sieved samples were then kept
securely on top of a glass plate (Canada balsam coated). A
25.4 cm × 6.35 cm glass plate was used for the experiment.
Subsequently, the samples are then analysed through LEICA
microscope and visualized using QWIN software. This ana-
lytical technique is used to scrutinize the surface texture of
the sample. EDAX is an analytical technique, which finds
its application in pin-pointing the elemental composites of
different materials. EDAX technique depends on the interac-
tion between a source of X-ray excitation and the concrete
specimen.
Results and discussion
Compressive strength
The concrete specimens were evaluated for their compres-
sive strength after a curing period of 3, 7 and 28 days in two
sets: first being with varying proportions of GO (GO-1 to
GO-4) and the second set including 10% RHA with vary-
ing proportions of GO (RHA10 GO-1 to RHA10 GO-4)
as shown in Fig. 2. Maximum compressive strength was
observed on the addition of 0.075% GO for both sets of
samples as shown in Table 6. Compressive strength values
were seen to have a drop on further addition of GO after
0.075%, i.e. beyond GO-3. An 49.38% and 122.45% increase
in the strength was observed on increasing the curing period
from 3 to 7 and 28 days, respectively, for mix RHA0 GO-3,
whereas an increase of 13.3% was seen for a mix without
RHA (RHA0 GO-3). The increase in strength was found
due to the accelerated hydration process observed due to
the addition of GO. GO has oxygen-containing functional
groups that help in accelerating the hydration process [47].
With respect to the 3-day strength of RHA0 GO-3, the 7-
and 28-days strength was found to be increased by 49.38%
and 122.45%, respectively. Further, on adding only 0.075%
of GO in absence of RHA (RHA0 GO-3), an increase of
13.3% in compressive strength was observed at the end of
28 days for controlled mix.
Considering the particle size of GO being less than 3 µm,
it fits into the microscopic interstitial voids and between the
ITZ, further promoting compactness and increasing density.
A reaction of GO with Ca(OH)2 (released during hydration
of cement) was observed promoting the auxiliary formation
of C–S–H gel. GO provides a large surface area for chemi-
cal reactions to occur and acts as centres of nucleation [48].
With 10% replacement of cement with RHA in absence
of GO (RHA10 GO-0), a 4.4% increase in strength was
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 5  Page 6 of 16 Innovative Infrastructure Solutions (2021) 6:5

Fig. 2  Compressive strength of 70
the mixes at 3, 7 and 28 days 3 Days
65 7 Days
60 28 Days

55

Compressive Strength (N/mm2)

50
45
40
35
30
25
20
15
10
5
0
O -0 -1 -2 -3 4 -0 -1 -2 -3 -4
GO 0 GO 0 GO 0 GO- 10 GO 10 GO 10 GO 10 GO 10 GO
A0G H A 0 A A A A A A A A
RH R RH RH R H R H R H R H R H R H

Table 6  Compressive strength Mix ID Compressive strength in N/mm2 Percentage increase in strength

of mixes
3 Days 7 Days 28 Days 3 Days 7 Days 28 Days

RHA0 GO-0 21.2 31.6 48.1 – – –

RHA0 GO-1 22.8 34.5 49.5 7.55 9.18 2.91
RHA0 GO-2 23.6 35.3 52.3 11.32 11.71 8.73
RHA0 GO-3 24.5 36.6 54.5 15.57 15.82 13.31
RHA0 GO-4 23.1 35 51.6 8.96 10.76 7.28
RHA10 GO-0 22.8 32.8 50.2 7.55 3.80 4.37
RHA10 GO-1 24.2 35.7 52.3 14.15 12.97 8.73
RHA10 GO-2 25.8 36.4 54.6 21.70 15.19 13.51
RHA10 GO-3 26.1 37.6 56.6 23.11 18.99 17.67
RHA10 GO-4 23.1 35.5 51.8 8.96 12.34 7.69

observed at the end of 28 days. A reaction undertakes the Flexural strength

conversion of the poor cementitious silica-rich material to
calcium silicate, which has good cementitious properties,
hence, increasing the strength. Large specific area and reac-
tive silica present in RHA lead to an increase in the strength
[49]. An increase in the compressive strength was found
on addition of GO and RHA till 0.075% of GO (RHA10
GO-1 to RHA10 GO-3) after which it was found to drop
with the increase in GO percentage. This decrease was pos-
sibly related to the agglomeration of the GO particles, which
further resulted in non-uniform distribution of these parti-
cles in the concrete mix [39]. RHA GO-3 was found to be
optimum in terms of compressive strength being 56 N/mm2.
Overall, the strength on 28 days for mix RHA10 G0-3 was
increased by 17.7% from the reference mix (RHA0 GO-0).
This increase was due to the effect of pozzolanic reaction
of concrete, filler effect and hydrophilic properties of the
GO–RHA mix.
Table 7 and Fig. 3 show the flexural strength of two sample
sets with varying content of GO for 7 and 28 days of curing.
From Table 7, it was observed that all the mixes exhibited
greater flexural strength than the conventional mix (RHA0
GO-0) for both 7 and 28 days. Maximum flexural strength
was obtained on addition of 0.075% of GO for both sample
sets being (RHA10 GO-3) and (RHA0 GO-3). The flexural
strength increased by 26.81% at the end of 28 days, on add-
ing 0.075% of GO (RHA0 GO-3). The increase in the flex-
ural strength attributes to the control on the micro-cracks at
the nanoscale level due to the crack-binding effect of GO.
The results also outlined that the flexural strength
increased by 10.46% for the mix of 10% RHA by weight
of cement without any addition of GO (RHA10 GO-0) at
28 days. The increased flexural strength was because of the
high specific area of RHA, which acts as centre of nucleation

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Innovative Infrastructure Solutions (2021) 6:5 Page 7 of 16  5

Table 7  Flexural strength of mixes consequently blocking the entry of water to the un-hydrated
Mix ID Flexural strength in N/ Percentage increase
cement, preventing further reaction [50].
mm2 in strength
Splitting tensile strength
7 days 28 days 7 days 28 days

RHA0 GO-0 3.15 5.26 – – Table 8 and Fig. 4 highlight the change in splitting tensile
RHA0 GO-1 3.85 5.51 22.22 4.75 strength for various test specimens, revealing the highest
RHA0 GO-2 4.14 6.32 31.43 20.15 split tensile strength obtained on addition of 0.075% of GO
RHA0 GO-3 4.32 6.67 37.14 26.81 for both sample sets RHA0 GO-3 and RHA10 GO-3 com-
RHA0 GO-4 3.85 5.52 22.22 4.94 pared to the controlled mix (RHA GO-0).
RHA10 GO-0 3.45 5.81 9.52 10.46 From Fig. 4, there was a 47.5% increase in the splitting
RHA10 GO-1 4.12 6.06 30.79 15.21 tensile strength for RHA0 GO-3 after a curing period of
RHA10 GO-2 4.25 6.44 34.79 22.43 ­28th day as compared with 7-day curing. The increase in
RHA10 GO-3 4.68 6.82 48.57 29.66 GO percentage was beneficial for the strength gain and was
RHA10 GO-4 3.52 5.82 11.75 10.65 displayed by both the sample sets, however, after 0.075%
of GO, the trend was found to decrease. The decrement in
the strength after 0.075% of GO could be attributed to the
[49]. Taking into account the mix with both GO and RHA agglomeration of GO. The splitting tensile strength with GO
(RHA10 GO-3), the strength increased by 48.57% after increased because of the ultra-fine sized particles and high
7 days and 26.8% after the age of 28 days. Amongst all the specific surface area of GO, which further accelerated the
mixes, RHA10 GO-3 showed the highest flexural strength, hydration process. The 28-days strength was increased by
at the end of both 7 and 28 days. The test procedure high- 32.9% for the mix RHA10 GO-3 with respect to the con-
lighted the reduction in the strength with the further increase trolled mix at 7 days. Under absence of GO and 10% replace-
in GO beyond 0.075%. This can be explained as, due to the ment of cement with RHA (RHA10 GO-0), the strength was
consolidated hydration products formed by the pozzolanic found to increase by 7.89%, on other hand, the strength was
reaction between GO and Ca(OH)2 which resulted in the increased by 21.05% when 0.075% GO was added in the
coating of the un-hydrated cement, henceforth, reducing absence of RHA and by 34.21% when 0.075% of GO was
the rate of hydration. Moreover, these hydration products added with 10% replacement of cement with RHA (RHA
also tend to occupy the pores between the cement particles, GO-3).

Fig. 3  Flexural strength of the 9

mixes at 7 and 28 days 7 Days
28 Days
8

7
Flexural Strength (N/mm2)

0
-0 1 2 3 -4 -0 -1 -2 -3 -4
O- O- O- GO GO GO GO
0GO A0 G A0 G A0 G 0 GO 0 0 0 GO
1 0 0
A A A1 A 1 A1 A A 1
RH RH RH RH RH RH RH RH RH RH

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Table 8  Splitting tensile strength of mixes performed to lay a linear equation (Eqs. 1 and 2) using the
Mix ID Split tensile strength in Percentage increase test result values.
N/mm2 in strength
y = 0.18x1 − 3.48 (1)
7 days 28 days 7 days 28 days

RHA0 GO-0 2.32 3.82 – – y = 0.1386x2 − 2.803 (2)

RHA0 GO-1 2.41 4.14 3.88 8.38
where y = compressive strength, x1 = flexural strength and
RHA0 GO-2 2.45 4.36 5.60 14.14
x2 = split tensile strength.
RHA0 GO-3 3.14 4.63 35.34 21.20
The equation enables to predict the value of flexural or
RHA0 GO-4 2.82 4.57 21.55 19.63
split tensile strength for a particular mix using its compres-
RHA10 GO-0 2.46 4.12 6.03 7.85
sive strength. R-squared values were found to be compel-
RHA10 GO-1 2.81 4.46 21.12 16.75
ling to unity and estimated values with a reliability of 93%
RHA10 GO-2 3.16 4.75 36.21 24.35
and 92% for flexural and split tensile strength, respectively,
RHA10 GO-3 3.86 5.13 66.38 34.29
evincing the accuracy of the results.
RHA10 GO-4 3.43 4.28 47.84 12.04

Water absorption and sorptivity

Relationship between strengths The water absorption and sorptivity results for engineered
sample sets were below than the controlled mix (RHA0
The variation in compressive, flexural and splitting tensile
GO-0), for both 28 and 90 days as shown in Figs. 7 and 8.
strength for 28 days is presented in Fig. 5. The strengths
The addition of GO in different percentages revealed that the
were produced in a radial chart to identify the variance of
lowest water absorption was obtained at 0.075% of GO for
strengths in different mix designs. The radial chart shows the
both replaced and non-replaced RHA mix.
split tensile, flexural and compressive strength all together,
The percentage decrease in water absorption of differ-
and a similar pattern in strength variation is observed.
ent mixes was with respect to the controlled mix (RHA0
In the above graph, a radial pattern was used for the ease
GO-0). The decrement in the water absorption capac-
of comparison. It was observed that both the flexural and
ity was around 25.4% for the mix with 0.075% of GO in
the splitting tensile strength of the sample has more or less
absence of RHA (RHA0 GO-3), for the age of 28 days,
followed the similar trend to compressive strength. However,
which is primarily as less water could be adsorbed due
the variation between strengths remained less.
to the pores being filled by GO, thereby reducing the
To predict the values and form a correlation amongst
water absorption and densifying the pore structure of the
all the strengths, a linear regression analysis (Fig. 6) was
concrete. Furthermore, the high pozzolanic effect of GO

Fig. 4  Splitting tensile strength

of mixes at 7 and 28 days

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Innovative Infrastructure Solutions (2021) 6:5 Page 9 of 16  5

Fig. 5  Radial variation of com- Flexural Strength

pressive, flexural and splitting Split-Tensile Strength
tensile strength for mixes RHA0GO-0
Compressive Strength
60
RHA10 GO-4 RHA0 GO-1
60
60 45
45
45
30
30
30 60
RHA10 GO-3 RHA0 GO-2
60 45
15 15
45 30
15
30 15
15
15
15 30
15 45
30
15 15 60
45
RHA10 GO-2 60 30 RHA0 GO-3
30
30
45
45
45 60
60
RHA10 GO-1 RHA0 GO-4
60

RHA10 GO-0

Fig. 6  Regression model to 7.5

estimate compressive strength Flexural Strength
using flexural and split tensile 7 Split Tensile strength
strength
6.5
y = 0.18x1 - 3.48
R1² = 0.93
Strength in N/mm2

5.5

4.5 y = 0.1386x2 - 2.803

R2² = 0.9203
4

3.5

3
46 48 50 52 54 56 58 60
Compressive Strength in N/mm2

helped to make the concrete more compact hence reduc-
ing water absorption [18]. With a further increase in the
amount of GO beyond 0.075%, the water absorption was
found to increase due to the agglomeration of GO, result-
ing in a non-uniform dispersion and thereby, leaving the
pores vacant. For the age of 28 days, when 10% of cement
by weight was partially replaced with RHA (RHA10
GO-0), the water absorption lowered by 14.5%. The reason
for this significant decrease in water absorption percent-
age was the filler effect and pozzolanic reaction of RHA.
Similar densified pore structure was also seen in under
the SEM as further explained in Sect. 4.8. The optimum
results were obtained when the mix containing optimum
quantities of GO and RHA (RHA10 GO-3) were used, for
both 28 and 90 days. There was a decrease of 41.7% in
water absorption in mix RHA10 GO-3 after 28 days as the

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 5  Page 10 of 16 Innovative Infrastructure Solutions (2021) 6:5

Fig. 7  Percentage of water 3.5

absorption at 28 and 90 days 28 Days
90 Days
3.0

2.5

Water Absorption (%)

2.0

1.5

1.0

0.5

0.0
0 1 2 3 4 -0 -1 -2 -3 -4
GO- GO- GO- GO- GO- GO GO GO GO GO
A0 A0 A0 A0 A0 A1
0
A1
0
A1
0
A1
0
A1
0
RH RH RH RH RH RH RH RH RH RH

Fig. 8  Sorptivity at 28 and
90 days

pozzolanic reaction resulted in the formation of C–S–H gel
which hindered the absorption characteristics of the mix.
It can be concluded that all the mixes displayed lower
sorptivity than the reference mix (RHA0 GO-0), for both
28 and 90  days. The lowest sorptivity was obtained at
0.075% of GO for both RHA replaced and non-replaced
cubes. The percentage decrease in sorptivity of all the
mixes was with respect to the controlled mix (RHA0
GO-0).
In the concrete mix with 0.075% of GO without any
cement replacement with RHA (RHA0 GO-3), the sorptiv-
ity decreased by 22%, after 28-days curing. This decrease
in capillary sorption of concrete was because the pores were
filled by GO, thus reducing the capillary pores. Therefore,
because of GO’s packed and refined microstructure, the addi-
tion of GO was favourable in terms of gain in mechanical
strength and reduction in sorptivity of the concrete. With the
further addition of GO, the sorptivity increased, displaying

13
Innovative Infrastructure Solutions (2021) 6:5 Page 11 of 16  5
possible agglomeration of GO particles, thus creating voids
within the molecule. In the partially replaced concrete mix
with RHA (RHA10 GO-0), the sorptivity decreased by 4.9%.
These results depicted that the least sorptivity was obtained
for RHA10 GO-0. For this mix (RHA10 GO-3), the decrease
of 23.3% was observed and this was due to the filler effect of
both RHA and GO [50].
Rapid chloride penetration test
RCPT is used to assess the resistance of a concrete specimen
to not allow the chloride ions to penetrate. Figure 8 shows
the RCPT values of nominal mixes of GO and RHA at the
age of 28 and 90 days. The test results at 28 days depicted
that the chloride penetration was either low or very low in
all the mixes. With nominal mixes only containing GO, the
RCPT values were found to be decreasing from 1124 to
910 coulombs for an increase in GO values up to 0.075%
(RHA0 GO-0–RHA0 GO-3), at the age of 28 days. With the
increase in GO, the reduction in the charge passing through
the mixes was probably because of the interconnected layers
of GO and its ability to hold the chloride ions. Moreover,
this reduction in the penetration depth of chloride ions was
because of the formation of sponge-like structure, arising
from well packed GO particles [51]. The value increased
from 910 to 920 coulombs on further increase in GO content
from 0.075 to 0.1% (RHA10 GO-4), for the age of 28 days.
Figure  9 depicts a very low chloride ion penetration
for all the mixes, aged at 90 days. However, with a mix-
ture of RHA and GO, there was a significant decrease in
the charge passing through the concrete from 988 to 786
coulombs (RHA10 GO-0 to RHA10 GO-3), at the age of
90 days. It was also found that on increasing the GO content
Fig. 9  RCPT value for mixes at
28 and 90 days
to 0.1%, there was a hike in the charge passing through the
concrete. The test results after 90 days showed a decline in
chloride ion penetrability when the nominal mix contained
only GO. The value decreased from 998 to 867 coulombs
for the mixes RHA10 GO-0 to RHA10 GO-3 for an age
of 90 days. The pozzolanic reaction between the GO and
RHA accounted for this decrease in charge passing through
the concrete. However, for 0.1% of GO addition, the value
depicted an increase to 954 coulombs. When 10% RHA and
GO was used, the value decreased from 842 to 688 coulombs
(RHA10 GO-0–RHA10 GO-3) and then increased to 834
coulombs with the further addition of GO (RHA10 GO-4),
for an age of 90 days. The increase in chloride penetration on
further addition of GO was due to the further densification
of the pore structure [52]. It is noticed from Fig. 8 that the
charge passing through the concrete mix after 28 days was
much more than the charge passing through the concrete
mix after 90 days.
Acid resistance test
The acid resistance test results for all the mixes, including
a loss in weight and compressive strength, are shown in
Fig. 10.
Figure 10 depicts that all the mixes had higher acid resist-
ance than the reference mix (RHA 0 GO-0), for both 28 and
90 days. Furthermore, the percentage of loss in weight and
compressive strength was lower for all the mixes than the
reference mix. This enhanced resistance to acid attack was
due to the addition of GO and partial replacement cement
with RHA. The gradual percentage decrease in weight loss
and compressive strength loss was with respect to the ref-
erence mix. After the age of 28 days, with an increase in
13
 5  Page 12 of 16
Fig. 10  Acid resistance for
mixes at 28 and 90 days
GO content up to 0.075%, the decrease in weight loss was
from 10.16 to 5.73% (RHA0 GO-0 to RHA0 GO-3). This
decrease in weight loss was because of the ability of GO
particles to form a protective layer and increase its resist-
ance to chemical attack. Moreover, GO also behaves as a
filler material which compacts the voids at a microstruc-
tural level, thus improving the concrete ability to resist
acid ingress. With further increase in GO content at the age
of 28 days, the weight loss increased from 5.73 to 6.84%
(RHA0 GO-3 to RHA0 GO-4). When RHA (partial replace-
ment by weight of cement) along with GO was used, the
weight loss decreased from 8.86 to 5.13% (RHA10 GO-0
to RHA10 GO-3), and then increased to 6.11% (RHA10
GO-4) with the further addition of GO. The trend of change
in weight loss for 90 days was similar to the trend of weight
loss for 28 days. For an age of 28 days, with an increase in
GO content up to 0.075%, the loss in compressive strength
was from 25.06 to 18.43% (RHA0 GO-0–RHA0 GO-3).
With further increase in GO content (> 0.075% of GO),
the loss in compressive strength increased from 18.43 to
20.12% (RHA0 GO-3–RHA0 GO-4). Moreover, for the age
of 28 days, when both RHA and GO were used, the loss
in compressive strength decreased from 22.12 to 16.65%
(RHA10 GO-0–RHA10 GO-3). This decrease in loss of
compressive strength can be primarily attributed to RHA’s
pozzolanic reaction, which converts calcium hydroxide (eas-
ily attacked by acids) to C–S–H. Thereby, this C–S–H bond
leads to increased resistance to acid attack. Furthermore,
the enhanced acid resistance of these mixes was because
of RHA, as it leads to a drastic drop in the permeability
of the concrete [53]. With further increase in GO content,
the compressive strength loss increased to 18.14% (RHA10
13
Innovative Infrastructure Solutions (2021) 6:5
GO-4). A similar trend in compressive strength loss results
was also seen at the age of 90 days.
Microstructure study results
The results of the mechanical strength and durability proved
that the optimum results were obtained for 10% partial
replacement of cement by RHA along with 0.075% addition
of GO (RHA10 GO-3). The SEM analysis was conducted for
RHA10 GO-0 and RHA10 GO-3 and is shown in Figs. 11
and 12. Moreover, the EDAX analysis of these mixes was
also conducted and shown in Fig. 13.
The SEM images of RHA10 GO-0 in Fig. 11a depict
the presence of bundles of fibrous C–S–H gel in the central
region. However, Fig. 12a of RHA10 GO-3 shows denser
patches of C–S–H matrix than RHA10 GO-0. A hexago-
nal plate-like structure identified in both Figs. 11 and 12
was depicted to be C–H crystals. The presence of GO was
confirmed in the SEM images by the flat-surfaced flake-like
structure present in Fig. 12b. As compared with Fig. 12,
with the addition of 0.075% of GO, the hydration products
eventually became more complex-stacked structures as seen
in Fig. 11. Lu et al. [54], confirmed the reaction between
C–S–H of the cement matrix and carboxylic acid of GO,
confirming the presence of hydration products. Furthermore,
the acceleration of the hydration process was seen when GO
reacts with calcium hydroxide, thus producing C–S–H. It
helped in enhancing the mechanical properties as resulted
in a denser-more compact structure at a microscopic level
with minimum amounts of Ca(OH)2 crystals [48]. Thus, it
can be concluded that GO acts as good reinforcing mate-
rial in concrete. Figure 11 shows that RHA has an angular
Innovative Infrastructure Solutions (2021) 6:5 Page 13 of 16  5

and porous structure, relating to its high surface area [55].

Moreover, higher silica content of RHA and densification of
the pore structure were some of the significant reasons for
the improved mechanical strength on the addition of RHA.
A presence of Si, O, Al and Ca was found through EDAX
analysis for mixes RHA10 GO-0 and RHA10 GO-3 as
shown in Fig. 13. Presence of Silicon (Si), Calcium (Ca)
and Oxygen (O) in high proportions in RHA10 GO-3 mix
confirmed the presence of GO sheets along with hydration
products. Moreover, it is evident from the EDAX report
that the silica content increases for the concrete which has
both RHA and GO (RHA10 GO-3) in comparison with the
RHA10 GO-0 mix. Furthermore, better hydration in RHA10
GO-3 mix was the reason behind the higher weight percent-
age of silica in Fig. 13b as compared with RHA10 GO-0 in
Fig. 13a. The increase in the percentage of silica in RHA10
GO-3 was also due to the large formation of C–S–H gel,
which is also a hydration product. Hence, the increase in
mechanical strength due to RHA and GO is also justified
through EDAX.

Conclusion
Fig. 11  SEM images of RHA10 GO-0 The experimental work carried out can be concluded as
follows.

• As the percentage of GO increases up to 0.075%, the

mechanical and the durability properties improve sig-
nificantly. This is possibly due to GO’s acceleration
of hydration on concrete. Moreover, it is also noticed
from the mechanical and durability tests that the optimal
results are obtained in the mix where GO along with 10%
RHA is used. This is possible because of the filler effect
and pozzolanic reaction in GO–RHA mix.
• The addition of GO in HSC is directly proportioned to
the compressive strength gain in concrete. The strength
is further increased when a combination of 10% RHA
and GO is used in concrete mixes. The mix with 10%
partial replacement of RHA and addition of 0.075% of
GO deliver the optimum results in comparison with all
other mixes. The compressive strength results also indi-
cated that beyond 0.075% addition of GO, a reduction in
strength occurred.
• The flexural and splitting tensile strength of HSC showed
similar results to compressive strength and was found
to enhance with the addition of GO and 10% RHA.
The maximum flexural and splitting tensile strength is
observed with 10% RHA and 0.075% addition of GO.
• A considerable decrease in the value of water absorp-
tion and sorptivity is observed for the mix containing
both GO and RHA, in comparison with the reference
mix (RHA10 GO-0). The water absorption and sorptivity
Fig. 12  SEM images of RHA10 GO-3

13
 5  Page 14 of 16
Fig. 13  EDAX results
values decrease due to the combined pozzolanic activity
and pore-filling effect of both GO and RHA, promising
a dense microstructure.
• RCPT results depict that the concrete with both RHA and
GO shows significantly lower chloride ion permeability
than the reference mix (RHA10 GO-0), for both 28 and
90 days. For all the mixes, the chloride ion permeability
is assessed either as “very low” or “low” for both 28 and
90 days.
• For all the mixes containing both RHA and GO, the
resistance to acid attack is higher than the controlled mix
(RHA0 GO-0). The formation of C–S–H bonds leads to
higher resistance to acid attack due to the pozzolanic
reaction of GO and RHA. The acid resistance results
depict that the mix RHA10 GO-3 is least susceptible to
acid attack, hence, indicating that it has the highest dura-
bility amongst all the mixes. Thus, this HSC is suitable
for use in acidic environments.
13
Innovative Infrastructure Solutions (2021) 6:5
• The microstructural analysis proves that the addition
of GO and RHA enhances the formation of calcium
hydroxide and calcium silicate hydrates crystals, which
led to the improvement in the strength and durability
properties. Moreover, the EDAX report shows that the
weight percentage of silica increase for the mix which
has both RHA and GO (RHA10 GO-3) in compari-
son with the mix with only RHA (RHA10 GO-0). This
increase in silica content in RHA10 GO-3 is due to
better hydration in the mix as compared with RHA10
GO-0.
• The study concludes that through a proper engineered
mix with 10% RHA (partially replaced cement by
weight) and 0.075% addition of GO, the production of
a sustainable and green concrete is practicable with a
reduced impact on the environment and high performing
mechanical and durability properties. The work showed
in this study is not limited to prepare HPC but the meth-
Innovative Infrastructure Solutions (2021) 6:5 Page 15 of 16  5
odology can also be applied on other types of concrete
as well.
Acknowledgements  The authors would like to acknowledge and thank
the constant support and motivation of School of Civil Engineering,
Vellore Institute of Technology, Tamil Nadu.
Funding information  Not applicable.
Compliance with ethical standards  16. Long WJ, Zheng D, Duan HB, Han N, Xing F (2018) Perfor-
Conflict of interest  The authors declare no conflict of interest in per-
forming the present investigation.
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