Journal of Building Engineering 27 (2020) 101007

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Journal of Building Engineering

journal homepage: http://www.elsevier.com/locate/jobe

Effect of graphene oxide on mechanical and durability performance

of concrete
S.C. Devi a, *, R.A. Khan b
a
Deptt. of Civil Engg, Dr. B. R. Ambedkar NIT Jalandhar, Punjab, 144011, India
b
Deptt. of Civil Engg, Z. H. College of Engg. & Tech, AMU, Aligarh, Uttar Pradesh, 202002, India

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

Keywords: Graphene oxide (GO) may have a huge impact in construction industry in near future. Because of the oxygenated
Graphene oxide functionalities attached on the aromatic structure, it has better dispersibility property than any other graphene-
Mechanical properties based derived. Many of the researchers have given their views on the influence of GO on the mechanical and
Water permeation
durability properties in ceramic matrix. Five mixes were prepared with inclusion of GO (0%, 0.02%, 0.04%,
Hydrates of cement
Nano-reinforced concrete composites
0.06% and 0.08% by weight of cement). Tests on mechanical and water permeation properties were conducted.
The compressive and tensile strength of the mix with 0.08% GO has shown a better result compared to rest of the
mixes. The sorptivity and permeability of the nano-reinforced concrete mixes in addition of GO were observed to
have reduced with increasing GO content in the concrete compared to the control mix. The synthesized GO was
structurally characterized by means of FE-SEM/EDX, FT-IR and XRD. Microstructural analysis was carried out
using SEM/EDX on 90 days old concrete mixes and the quality of the concrete mixes was checked with UPV test.

1. Introduction composites [2,3].

Graphene oxide is also a carbon-based nanomaterial. Graphene oxide
Cement is the basic binding material used in concrete with the major was first-hand prepared by Benjamin C. Brodie [4] in 1859 by chemical
drawback of being brittle with low tensile strength. With due course of exfoliating graphite (further modified by Hummer). Like graphite, gra­
time these drawbacks were taken care with the introduction of steel phene oxide has aromatic structure like any other graphene
reinforcement and fibers. But the introduction of nanomaterials in based-derived, but due to the chemical reactions occurred, some of the
cement-based composites have enhanced the properties such as tough­ covalent bonds were broken down and functional groups such as epoxy,
ness, flexural, tensile and durability properties by improving at the carbonyl, hydroxyl, phenol etc. were attached on the sp2 aromatic
nanoscale of the concrete. Nanotechnology has proved that composites monolayer structure (about one atom-thick) [5,6]. The functionalities
can be modified/re-engineered with a small inclusion of nano-materials have its perk when introduced to cement-based composites. These
[1]. Carbon Nano-Tubes (CNTs), graphene-derived, Carbon nanofibers oxygenated functionalities are hydrophilic in nature and easily adsorbs
(CNFs), nanosilica, etc. are very popular among all the nanomaterials. free radicles of water from the cement composite prepared. Graphene
Nanocomposites has proven its ability to enhance the properties of the oxide has large specific surface area with higher aspect ratios. Generally,
parental material. Nanomaterials in concrete industry have become a nanomaterials have one big disadvantage with their dispersibility
trend as it has many advantages from enhancement in mechanical property but in case of GO, it has dominance over any other nano­
strength to filling the voids at nano-level. The chemistry of cement and materials because of the oxidative functionalities which allow to
nanomaterials such as CNTs, graphene, graphene oxide (GO), disperse easily in water. Chuah et al. have mention that the degree of
graphene-based nanomaterials are observed to have improved the me­ sonication was independent for GO dispersion in water but tend to
chanical, thermal, electrical, optical etc. properties of the cement com­ reagglomerate as the abhorent forces provided by oxygenated functional
posites. Many of the researchers have worked on the mechanical and groups at GO sheets was overpowered by van der Waals forces between
durability properties on nano-reinforced cement composites. And as the GO nanosheets [7]. However, a compatible surfactant (poly­
usual it has shown better results than the conventional cement carboxylate ether-based) stabilized the GO dispersion in cement-based

* Corresponding author.
E-mail address: [email protected] (S.C. Devi).

https://doi.org/10.1016/j.jobe.2019.101007
Received 27 November 2018; Received in revised form 16 October 2019; Accepted 17 October 2019
Available online 20 October 2019
2352-7102/© 2019 Elsevier Ltd. All rights reserved.
S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

composites. 1675 kg/m3 and 1690 kg/m3 respectively. Table 1 shows the physical
Addition of GO in cement-based composites have an adverse effect properties of the OPC. And MG SKY 8765 (polycarboxylate based) super
on the workability due to its large surface area that tend to absorb more plasticizer were procured from local dealer conforming to IS 9103:1999
water molecule to get wet and a bulky lateral size with high capacity for [21].
water retention created due to cluster of GO nanosheets [8,9]. Regard­
less of the above mention disadvantage of GO, incorporation of small 2.2. Mix proportions and casting
content of GO of about 1% by weight of cement (bwoc) have improved
the compressive strength by 63% [10]. The addition of 0.05% GO A total of five mixes were prepared and tests were performed on both
(bwoc) was reported to enhanced the compressive strength by 15–33% fresh concrete and hardened concrete at different curing ages. The
and flexural strength by 41–58% [3,11]. Shang et al. have stated that the binder, fine and coarse aggregate was kept constant at 384 kg/m3,
compressive strength with 0.04% GO inclusion to the cement paste was 715 kg/m3 and 1113 kg/m3 respectively (1:1.86:2.89) with w/b ratio
improved up to 15.1% compared to plain cement paste [12]. The 0.45. GO were added with varying percentage content by weight of
compressive strength and tensile strength were increased by over 40% cement from 0 to 0.08% with an increment of 0.02%. The mix pro­
with 0.03% GO inclusion by weight of cement (bwoc) to OPC paste at 28 portions are given in Table 2. The GO was allowed to dispersed using
days curing age [13]. Mohammed et al. concluded that the addition of 500 W cup-horn high intensity ultrasonic processor [22] in an aqueous
GO led to enhancement of water sorptivity and chloride penetration solution containing 0.05% (bwoc) super plasticizer (used as surfactant)
values whereas it reduces the pore size of the GO reinforced cement kept constant for all the mixes in a sonicator with ultrasonic energy of
paste indicating the improvement of resistance to chemical ingress [14]. about 2000J/min at cycles of 20s (to avoid overheating) operated at
Some researchers have quoted that GO inclusion accelerated the heat of 50% constant amplitude for 30 min. Further, the solution was stirred on
hydration. The GO sheets with oxygenated functionalities make more a 2000 ml capacity magnetic stirrer till the ingredients were introduces
approachable to the cement particles, thus allowing the nanosheets to to the mixer. The 10% and 20% of total water of the mix were used in the
act as nuclei for the cement phases boosting the reaction of cement with exfoliation process using sonicator and magnetic stirrer respectively.
water [14]. Wang et al. have mentioned that the microstructure of the The mechanical exfoliation was carried out with different loading levels
GO reinforced cement matrix have massive crystal structure covering of GO (0.02%, 0.04%, 0.06% and 0.08%).
implying leaching of calcium hydroxide (CH) during the hydration A homogeneous mixture of cement, sand, coarse aggregate and 70%
stages have been improved at 28 days curing age [15]. of water was prepared in a power-driven laboratory (220–240 V power
The GO inclusion cement matrix is in trend due to its exceptional input) mixer of 300L capacity at 22–24 rmp for 3 min. The remaining
properties. Interest in GO has grown worldwide in various fields as GO is 30% water with exfoliated GO nano-sheets was added to the mixer and
way cheaper compared to extremely expensive multi-walled CNTs, rotated for another 2 min. The fresh concrete was then poured on the
single-walled CNTs and CNFs (which is 250, 1280 and 218 times more oiled moulds of respective shape and sample sizes. After 24 h and water
than price of GO per 100g) [16]. Thus, GO became the best candidate for cured for 7, 28, 56 and 90 days in a temperature (27 � 2 � C and 90%
this investigation. This investigaton was carried out to develop a humidity) regulated curing tank till the age of testing.
nano-reinforced concrete composite in addition of GO with varying
percentage by weight of cement. No study has been reported on GO
inclusion in concrete (with natural coarse and fine aggregate) compos­ 2.3. Test method
ites with regards to workability, compressive strength, tensile strength,
water permeation, sorptivity, quality of the nano-reinforced concrete 2.3.1. Slump test
composites and the cost analysis to get a clear picture whether this Workability is the ability to be mixed, handled, transported and
investigation will be helpful for practical application in construction placed with a minimum loss of homogeneity i.e. segregation or bleeding.
industry. Workability of the fresh concrete was performed as per IS: 6461 (Part
VII)- 1973 [23] and the designed slump value for the control mix i.e. 0%
GO content concrete mix was 100 mm. The slump value was evaluated
2. Experimental program
using slump cone test after pouring the fresh concrete in the cone (200ɸ
mm, 100 ɸ mm and 300 mm height) in four layers (1/4 of height of the
2.1. Materials
mould) by tamping each layer 25 times and lifted and the height of
coned concrete was measured. The slump value for different mixes were
Raw GO was synthesized using modified Hummer’s method [17,18],
recorded and the influence of GO in the fluidity of the nano-reinforced
graphite powder (10g) and sodium nitrate, NaNO3 (5g) were allowed to
concrete composites.
react with conc. sulfuric acid, H2SO4 (230 mL) at 20 � C temperature on
heater stirrer for over a period of 30 min and then gradually added
2.3.2. Mechanical properties
potassium permanganate, KMnO4 (30g). The resulting mixture were
As per code IS: 516–1959 [24] and IS: 5816–1999 [25], the test was
heat up to 35 � C for another 30 min and slowly diluted with 230 ml
conducted on 100 mm cubes for compressive and splitting tensile
water. The mixtures were then heated up to 98 � C for 15 min and 3%
strength (diagonally splitting the cube, stress (σ) ¼ 0.5187 Load/Side2)
hydrogen peroxide (H2O2) were added to complete the reaction fol­
lowed by 400 mL deionized (DI) water and allowed to settle. And finally,
washed the dilute solution of GO with 1:10 HCl and 4 L DI water until Table 1
the pH of the filtrate was up to 7. The filtered paste was then oven dried Physical properties of OPC.
at 65 � C for 24 h to obtained required GO powder. The chemicals used Characteristic Properties OPC
were procured from LOBA chemicals. And the GO obtained was then Specific Gravity 3.15
characterized structurally using SEM/EDX, XRD and FT-IR techniques to Specific Surface Area (m2/kg) 300
check the composition of the near surface, crystalline structure and to Compressive Strength (MPa)
3 Days 24.6
identify the functional groups present.
7 Days 34.3
OPC 43 grade, meeting the specification as per IS 8112:1989 [19], 28 Days 45.2
fine aggregate used were locally available which lie in Zone II, con­ Standard Consistency (%) 32
forming IS 383: 1997 [20], and natural coarse aggregate of maximum Initial Setting Time (Minutes) 62
nominal size 12.5 mm. The fineness modulus, specific gravity and bulk Final Setting Time (Minutes) 270
Loss of Ignition (%) 2.04
modulus of fine and coarse aggregate were 2.74 and 7.54, 2.67 and 2.64,

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Table 2
Quantity of materials used in kg/m3.
Mix Description OPC GO (g) Water Fine Aggregate Coarse Aggregate SP (mL)

M1 OPC0GO 384 0 173 715 1113 192

M2 OPC0.02GO 384 76.8 173 715 1113 192
M3 OPC0.04GO 384 153.6 173 715 1113 192
M4 OPC0.06GO 384 230.4 173 715 1113 192
M5 OPC0.08GO 384 307.2 173 715 1113 192

� SP – (Carboxylate based) Super Plasticizer, GO – Graphene Oxide.

for each curing age 7, 28, 56 and 90 days on 200T capacity Compression high vacuum at an accelerating voltage of 15 KV with working distance
Testing Machine (CTM). The load was allowed gradually without shock of 13 mm.
and increased at the constant rate of 3.5 N/mm2/minute until cube
failed. 3. Result and discussion

2.3.3. Test for water permeation property 3.1. Structural characterization of synthesized GO

2.3.3.1. Initial surface absorption. The initial surface absorption test The structural characterization of synthesized GO (powdered) was
(ISAT) were performed on 150 mm cubes, as per BS 1881: Part 208:1996 carried out using field emission scanning electron microscopy (FE-SEM)
[26], this was conducted to test the rate of flow of water into concrete and energy dispersive x-ray spectroscopy (EDX) on BRUKER QUANTA
surface per unit area at specified interval. The specimens were oven FEG 450 to obtained the element composition and surface morphology.
dried at 105 � C until the weight was not more than 0.1%. The setup for Fig. 1(a) and (b) the scanning electron microscopy images and the EDX
the test was made in such a way that a 78 mm diameter cap is clamped to analysis of synthesized GO showing wrinkled surface with elemental
the cube surface providing an area of water contact with the surface to composition of near surface, the percentage of carbon content (C) and
be tested of not less than 5000 mm2. The water was allowed to flow oxygen (O) was observed to be high which indicates the attachment of
through the inlet from the reservoir of diameter 100 mm which was oxidative functional groups as shown in Table 3. The large surface area
fitted with tap to an outlet attached with scale. The water head was of GO nanosheets interlaced with weak van der Waals bond which under
maintained between 180 mm and 220 mm for the test. The tap was the microscopy appears to be crinkly.
opened and measurements taken for 1 min at interval 10 min, 30 min The X-ray diffraction pattern for GO powder was obtained using
and 60 min from start of the test. The rate of flow was measured in PANalytical EMPYREAN diffractometer with Cu Kα ¼ 1.54060 Å, scan­
mL/m2s. The tests were performed on 28, 56 and 90 days curing period. ned at angular range of 2θ ¼ 5� –100� with fixed divergence slit of
0.2177� of step size of 0.0080 and step time of 12.0650 s, operated at
2.3.3.2. Sorptivity. A 100 � 200 mm cylinder was cut into 100 � 50 mm 40 mA and 45 kV to distinguishes the interplanar spacing and the crys­
disc and preconditioned by oven drying at 105 � C until the difference in talline nature. The XRD spectra of the GO is shown in Fig. 1(c)
weight of the specimen was not more than 0.1%. The test was performed appearance of diffraction peak at 2θ ¼ 10.8� indicating an interlayer
as per ASTM 1585–04: 2009 [27]. The circumferential area was coated spacing of 0.814 nm, which is assigned to (001) diffraction peak of
with epoxy paint and both the circumferential and top surface were graphitic oxide. Fourier transmission infrared (FT-IR) spectra spots the
tightly sealed using polyethylene sheets to block evaporation. The presence of functional groups of GO. This is due to the disruption of
weight of the disc was measured at 0, 1, 5, 10, 30, 60 min and for every oxygen containing functional groups on the sp2 hybridization. The FT-IR
1-h interval up to 6 h from the start for initial rate of absorption Trends spectra in Fig. 1(d), alkenic bonds (-C– – C- stretch) was observed at
of plots of cumulative water absorption and square root of time 1619 cm 1, Hydroxyl (-OH) and carbonyl groups (C– – O) were seen at
1 1
(mL/√S) for all concrete mixes containing graphene oxide (GO) 0%, peaks 3218 cm and 1711 cm . and at 870 cm-1 peak confirms C–O
0.02%, 0.04%, 0.06% and 0.08%.at 28, 56 and 90 days curing periods stretch in epoxides with further support by absorption peak at 1032 cm-
were evaluated. 1, thus confirming the presence of oxidative functionalities on the GO
nanosheets.
2.3.4. Ultrasonic pulse velocity
The ultrasonic pulse velocity (UPV) was generated by an electro- 3.2. Workability
acoustical transducer, transmitted on one surface of the concrete cube
and receiving (frequency of 54 KHz) the same by a similar transducer in The mix, M5 with 0.08% was observed to have significantly lower
contact with the surface at the other end. A thin layer of coupling gel was slump tailed by M4 (0.06% GO), M3 (0.04% GO) and M2 (0.02%)
applied to facilitate higher signal. The ultrasonic pulse velocity was compared to the control mix M1 with 0% GO. Fig. 2 shows the com­
carried out according to IS 13311(Part 1): 1992. The principle of eval­ parison of the GO reinforced concrete composites with the parent
uating the quality of concrete comparatively higher velocity was ob­ designed mix. The slump value of the nano-reinforced concrete com­
tained on the Pundit Lab when the quality of concrete in terms of posites reduces with increase in percentage GO content. Thus, incor­
density, homogeneity and uniformity is good. In case of poorer quality, poration of GO in the concrete mixes reduces the workability.
lower velocities are obtained. Ranges of velocities of UPV test are given Comparable results were reported on reduction of fluidity and increase
in IS 13311(Part 1): 1992 [28]. The tests were conducted at 28, 56 and in viscosity with increase in GO content [7,29]. The high specific surface
90 days curing period. area of GO (theoretical value of 2620 m2/g) adsorbs water from fresh
mix to wet the GO nano-sheets [9]. Also, the hydrophilic oxygenated
2.3.5. Microstructural observation functionalities attached on the GO nanosheets absorbs the water mole­
The samples of the GO-reinforced concrete mixes using scanning cule and remains entrapped due to flocculation and agglomeration for­
electron miroscopy-energy dispersive X-ray spectroscopy, SEM EDX on mation caused by electrostatic interaction between GO and cement
JEOL JSM-6510LV. The samples were made conductive by gold coating particles [12,13]. Hence, with increases in GO content in the mixes the
prior to microscopy analysis by sputtering method. To examine the slump value of the mixes decreases linearly.
samples at 90 days of curing, the secondary electron detector was used at

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 1. (a) FE-SEM, (b) EDX, (c) XRD and (d) FT-IR of GO nanosheets.

have minimum increase in compressive strength of 26%. Previous

Table 3
studies have mentioned that inclusion of small portion of GO nanosheets
Chemical composition for GO.
in cement-based composites has improved the compressive strength at
Element Weight % large scale [3,12,13,30–32].
O 47.62 Lin et al. (2016) confirmed that GO acts as catalyst and helped
C 45.34 accelerating cement hydration without causing any changes in the
S 4.86 oxygenated functional groups attached in GO nanosheets [33]. These
N 1.95
Mn 0.23
functional groups act as active sites that attracts cement particles. The
high surface area to mass ratio of GO nanosheets assists the nucleation
Total 100
for formation of cement hydrates and develops strong covalent bonds at
the interface of cement matrix and dispersed phase (i.e. GO). Thus, in­
3.3. Mechanical properties clusion of GO reinforced the concrete composites at nano-level which
results in enhancement of the compressive strength of GO
3.3.1. Compressive strength nano-reinforced concrete composite compared to control mix.
The compressive and splitting tensile tests were conducted on a
compression testing machine at 7, 28, 56 and 90 days curing period. The 3.3.2. Tensile strength
mixes with GO have better compressive as well as tensile strength than Fig. 4(a) and (b) illustrates the impact of GO on the tensile strength of
the control mix, M1. The mix with 0.08% GO, M5 have the maximum nano-reinforced concrete composites. It can be observed that the mix
improvement followed by M4 (0.06% GO), M3 (0.04% GO), and M2 with 0.08% GO content shows maximum improvement of 38% and the
(0.02% GO). Fig. 3(a) and (b) represents the comparison in compressive minimum of 5% for mix containing 0.02% GO by weight of cement, in
strength and percentage increase in compressive strength of the mixes at tensile strength at 90 days curing. Various investigations on effect of GO
different curing ages. It can be observed the gradual increase in strength inclusion in cement-based composites have concluded that GO accel­
with increase in concentration of GO in the concrete mixes at different erate hydration, improve tensile and flexural strength, refining the
hydration time. The mix with 0.08% GO exhibits the maximum mechanical interlocking at the GO reinforced cement matrix interface
compressive strength after 90 days curing with 49% improvement [13,29,31,34]. Densification of microstructure may have been caused
compared to control mix. And the mix with 0.02% GO was observed to due to the high aspect ratio and filler effect of GO at nano-scale resulting

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 2. Comparison of slump value of different mixes.

Fig. 3. (a) Compressive strength for all mixes, (b) percentage increase in compressive strength (%) at different curing age of 7, 28, 56 and 90 days.

an improved mechanical strength. curing ages. However, inclusion of GO in mortar with varying concen­
Table 4 represents the reinforcing effect of GO in the compressive tration ranging from 0.01% to 0.05%, 0.1%–0.125% up to 1% have been
strength of concrete composites of the current investigation compared to recorded to enhanced the compressive strength by 12.2–59%, 28–56%
the previous studies on GO incorporation in cement-based composites. It and 63–86% respectively, at different curing age. Similarly, in the cur­
was observed that inclusion of 0.03% and 0.05% GO in cement paste has rent study, inclusion of 0.02%–0.08% with an increment of 0.02% of GO
improved the strength by 40–67% and 15–33% respectively, at different in concrete have improved the compressive strength by 21–55% which

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 4. (a) Splitting tensile strength for all mixes (b) percentage increase in tensile strength (%) at different curing age of 7, 28, 56 and 90 days.

cured specimens. The minimum and maximum absorption rate was

Table 4
observed to be achieved by mix prepared with 0.02% and 0.08% GO
Comparison of compressive strength in cement-based nanocomposites rein­
addition in concrete composite which was observed to have reduced the
forced with GO.
absorption rate with reference to control mix by 6.5% and 34%
Matrix GO concentration w/c % increase in compressive Source respectively, at 90 days curing age. A gradual reduction in surface ab­
% (bwoc) strength at different curing
age
sorption of the nano-reinforced concrete mixes was clearly observed for
28 and 56 days curing period. Earlier investigations have reported that
Paste 0.03 0.5 40–67 [13]
GO incorporation in cement-based composites fabricates by reassem­
Paste 0.05 0.5 15–33 [3]
Mortar 0.01–0.05 0.37 12.2–59 [31] bling GO sheets due to weak van der Waals bond with the matrix [36,
Mortar 1.00 0.45 63–86 [30] 37]. Also, the nanosheets when interlocked with more GO sheets gets
Mortar 0.1–0.125 0.45 28–56 [16] deposited acting as a protective cloak which enhanced the resistance to
Concrete 0.02–0.08 0.45 21–55 Current chemical ingress. Thus, the mixes made with GO have shown lesser
study
surface absorption for both the curing age relatively to the control mix,
which may be due to the fact that GO as a filler material filled the voids
may be attributed to the strong interfacial bonding between the matrices at nano-level and not allowing further absorption of water molecule at
arising from the two-dimensional crumpled structure with high specific respective interval of time.
surface area of GO [35]. The reinforcing effect of GO on strength of
concrete makes GO a promising reinforcement in cement-based concrete 3.4.2. Sorptivity
composites. This method was used to govern the rate of absorption of water by
evaluating the increment in mass caused by the water absorption (only
one face of the sample) with respect to time. It was observed that the
3.4. Water permeation property
sorptivity (mm/s1/2) for all the mixes with GO inclusion for 28, 56 and
90 days curing as shown in Fig. 6, has lesser value than control mixed.
3.4.1. The initial surface absorption test
The percentage reduction in rate of absorption was maximum for mix
The initial surface absorption test (ISAT) was conducted on all the
prepared with 0.08% GO inclusion at 90 days curing about which was
five mixes on a 150 � 150 � 150 mm cube of 28 and 56 days curing age.
observed to be 46% and the minimum reduction was recorded to be 18%
The absorption rate was obtained by assessing the uniaxial water
of mix made with 0.02%GO compared to the control mix. Mohammed
penetration on to the surface of the concrete. The results of the test are
et al. mentioned that addition of GO influences the transport properties
shown in Fig. 5. It was recorded that the absorption was high for all the
in cement matrix which improved the gel pores and strengthened the
mixes at their 28 days of curing compared to the result of the 56 days

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 5. Initial surface absorption rate for 28, 56 and 90 days curing of the GO-reinforced concrete composites.

Fig. 6. Sorptivity of the mixes for 28, 56 and 90 days.

microstructure of the matrix [13,14]. It can be observed that with in­ cement hydrates was indeed accelerated with GO incorporation in the
crease in GO concentration level the porosity of the GO reinforced cement matrix.
concrete mixes have been reduced, i.e. the nucleation for formation of

Fig. 7. Ultrasonic Pulse Velocity for all the mixes for 28 and 56 days.

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

3.5. Ultrasonic pulse velocity more than 4.5 km/s means an excellent quality of concrete as catego­
rized by IS 13311.
The quality of the concrete was determined by conducting UPV test It was observed that velocity of all the mixes at 28 days curing age
on the hardened concrete of all mixes on 28, 56 and 90 days curing were of good quality concrete. But at 56 days curing the mix with 0.08%
period. The homogeneity of the concrete was obtained from the fact that GO content was recorded to have higher velocity compared to the
the pulse velocity of transducer passes through at a high or low velocity. remaining mixes falling under excellent quality. And at 90 days curing
Fig. 7 Represents the quality of the concrete mixes in comparison to the the velocity of mixes with GO with 0.08% was observed to be highest
control mixed. The pulse velocity less than 3 km/s means a very poor followed by 0.06%, 0.04% and 0.02% GO concentration which reduced
quality, between 3 and 3.5 km/s a medium, 3.5–4.5 km/s a good one and to excellent quality concrete. Whereas the velocity of the control mix

Fig. 8. SEM images for (a) M1 (CM), (b) M2 (0.02% GO), (c) M3 (0.04% GO), (d) M4 (0.06% GO) and (e) M5 (0.08% GO) for 90 days curing at 50 μm and 1 μm
magnification.

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 8. (continued).

was observed to be less than 4.5 km/s. This may be attributed to the for spectrum 1 to 5 as shown in Fig. 8. The EDX analysis of mixes (a)
nanofiller effect of GO densifying the concrete at nano-level. Thus, control mix (b) 0.02% GO (c) 0.04% GO (d) 0.06% GO and (e) 0.08%
improving the homogeneity and quality of concrete reflecting on the GO incorporation at 90 days curing age is shown in Fig. 9. The Ca/Si
mechanical and durability characteristics of the concrete. ration for control mix and mixes with GO 0.02%, 0.04% and 0.06% were
higher than 2 which specifies the hydrated products of the late stage of
3.6. Microstructural analysis hydration and C–S–H comprises of interlocked and interweaved foils
[39]. However, the Ca/Si ratio of mix with 0.08% GO concentration was
SEM analysis were performed for all the mixes at 90 days curing age observed to be 0.2 which is much lesser than 1.5 indicating the rapid
at different magnification range i.e. 50 μm and 1 μm near the interfacial formation C–S–H and C–H which resembles fibrillar materials entan­
transition zone (ITZ). The hydrated cement (crystals) was observed in gling to one another due to undergoing hydration of cement particles
the SEM micrographs of 90 days cured concrete composites as shown in [40]. Hence, GO inclusion (0.08%) has help the unreacted cement par­
Fig. 8 (a) control mix (b) 0.02% GO (c) 0.04% GO (d) 0.06% GO and (e) ticle to hydrate at later age which affect the mechanical and durability
0.08% GO. Densified hydrated cements with low density C–S–H in as­ behavior in a positive manner.
sociation with C–H is visible in Fig. 8 (a) with microcracks attributed to
aggregate settlement in fresh state which led to the presence of excess 4. Cost analysis
water content in the vicinity of the aggregate affecting the mechanical
behavior in negative way [38]. Fig. 8 (b) 0.02% GO content was The cost of casting the mixed designed were analyzed and reported in
observed to have dense platy cement hydrates associated with pores. Table 6. The cost of different nano-reinforced concrete composites was
However, the microstructure of concrete mix with 0.06% GO inclusion
undergoes significant improvement with densified hydrated crystals and
Table 5
lesser pores compared to mix with 0.04% and 0.08% GO content which
Composition of element present in the mix obtained from SEM/EDX analysis.
may be attributed to C–S–H formation in conjunction with C–H platy
crystals and ettringite (fibrous and needle shape crystals) in Fig. 8 (c), Element Spectrum 1 Spectrum 2 Spectrum 3 Spectrum 4 Spectrum 5

(d) and (e) respectively. With varying GO concentration in the concrete OK 64.02 62.4 58.57 61.57 60.22
composites, the hydrated crystals continue to become complex-stacking Al K 2.51 2.19 1.16 2.01 10.98
Si K 9.59 4.74 5.81 7.01 23.98
one over the other, massive and thicker as observed from Fig. 8 implying
Ca K 23.88 17.11 20.84 20.72 4.82
addition of GO in concrete is a promising reinforcing agent in concrete. CK – 13.56 13.62 8.69 –
Table 5 represents the electron dispersive X-ray spectroscopy (EDX)
Total 100 100 100 100 100
analysis of the element percentage composition of the SEM micrographs

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Fig. 9. EDX analysis for (a) Spectrum 1 (CM), (b) Spectrum 2 (0.02%GO), (c) Spectrum 3 (0.04% GO), (d) Spectrum 4 (0.06% GO) and (e) Spectrum 5 (0.08% GO)
for 90 days curing.

evaluated using the commercialized market prices of the materials. The developing a concrete, has reduced the workability and significantly
economy index (compressive strength/cost per m3) was observed to enhanced the compressive strength by (21–55%), tensile strength by
have maximum value at mix M4 (with 0.06% GO inclusion) compare to (16–38%) and initial surface absorption and sorptivity tends to decrease
rest of the mixes. It shows that mix M4 is the optimum mix. with increase in GO content for 28, 56 and 90 days curing period. The
result of the non-destructive method (UPV) showed that the homoge­
5. Conclusion neity of the GO reinforced concrete composite remain intact with the
increment in GO concentration, mix prepared with 0.08% has the
The current investigation can be drawn in to the conclusion that maximum average velocity for all the curing ages compared to control
inclusion of GO with different percentage content by weight of cement in mix and the remaining mixes. But from the cost analysis and the

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S.C. Devi and R.A. Khan Journal of Building Engineering 27 (2020) 101007

Table 6
Cost analysis of different mixes.
Material (kg) Cost (Rs/Kg) Mix combination

M1 M2 M3 M4 M5

OPC 7.48 2872.32 2872.32 2872.32 2872.32 2872.32

FA 1.5 1072.5 1072.5 1072.5 1072.5 1072.5
CA 1 1113 1113 1113 1113 1113
GO 1200 0 92.16 184.32 276.48 368.64
SP 118 22.656 22.656 22.656 22.656 22.656
W 0.05 8.65 8.65 8.65 8.65 8.65
Total (INR) – 5089.13 5181.29 5273.45 5365.61 5457.77
Compressive Strength (MPa) – 36.45 46.21 51.17 53.74 54.438
EI (Strength/Cost) – 0.00716 0.00892 0.0097 0.01002 0.00997

Note- OPC-Ordinary Portland Cement, FA- Fine Aggregate, CA-Coarse Aggregate, GO- Graphene Oxide, SP- Super Plasticizer, W- Water, EI- Economy Index.

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