mechanical properties of prepared graphene oxide in...

International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol: 19 No: 04 1

192304-8686-IJCEE-IJENS © August 2019 IJENS I J E N S

Mechanical Properties of Prepared Graphene Oxide

in Concrete Nanocomposites

Mohammed A. Mutar1,Ahmed A. Moosa2, Zainab H. Mahdi3 1- Master’s Student in Department of Materials Engineering Technology, Technical Engineering College – Baghdad, Middle

Technical University, Baghdad, Iraq, [email protected] .

2- Professor in Department of Materials Engineering Technology, Technical Engineering College – Baghdad, Middle

Technical University, Baghdad, Iraq, [email protected] .

3-Assis Prof in Department of Building and Construction Technology Engineering, Technical Engineering College– Baghdad,

Middle Technical University, Baghdad, Iraq, [email protected] .

Abstract-- Graphene oxide (GO) is important in engineering

applications such as in concrete technology. After prepared GO

from EG in a domestic microwave heating time(80s). GO was

added to the mixtures at five different ratios (0.01, 0.05, 0.1, 0.3,

and 0.5) % by weight of cement. These ratios were studied to

choose the optimum percent of GO in concrete. Thus, the best

ratio was 0.05% of GO by weight of cement, which gives the

highest compressive strength in graphene oxide concrete

nanocomposite (GOCNC). So, the percentages increase in the

compressive strength, flexural strength and split tensile strength

of GOCNC with 0.05% GO and 3% superplasticizer by weight

of cement were 64% ,29% and 22.2% respectively at curing time

28 days compared to the reference specimens. Thus, the addition

of GO to concrete mixture enhances the compressive, split

tensile and flexural strengths. Using scanning electron

microscopy (SEM) images for 0.05%GOCNC showed that GO

layers is well dispersed and no GO agglomeration.

Index Term-- Exfoliated graphite(EG), Graphene Oxide (GO),

Oxidation, Graphene Oxide Concrete

Nanocomposite(GOCNC), compressive strength, flexural

strength, split tensile strength.

1. INTRODUCTION

Over the past few decades, the need for high-performance

materials and structural components led to the rapid

development of new categories of materials. The

revolutionary vision of nanotechnology states that the

essence of nanotechnology is the ability to work at the

molecular level, atom by atom, to create large structures with

a fundamentally new molecular organization (Alkhateb et

al.,2013)[1]. Carbon, for a long period of time is known to

exist in two natural crystalline allotropic forms known as

graphite and diamond. The carbon atoms arrangement in

these materials give different properties. For example,

graphite is soft and black and the stable while diamond is hard

and transparent (Dai et al.,2012)[ 2]. Graphene as a two-

dimensional form of graphite, was isolated in 2004 by

Novoselov et al. of Manchester University, UK (Novoselov

et al.,2012)[3]. Graphene is a flat single sheet from graphite

layer and has (2D) structure with a monolayer of carbon

atoms packed into a honeycomb crystal plane (Geim ,

2009)[4]. Graphene has considered as the fundamental

building block for all sp2 graphitic materials including (0D)

fullerenes, (1D) carbon nanotubes and stacked into (3D)

graphite. Graphene has attracted great interests from

scientists and engineers because of the extraordinary

properties and wide applications (Geim and Novoselov

,2007)[5]. Graphene oxide (GO) is a layer of graphene

decorated with high-density oxygen functional groups like

hydroxyl (OH) and epoxy group on its basal plane, and

carboxyl at its edge, (Dreyer et al.,2010)[6]. The vision of

nanotechnology has opened a strong public domain for

further research in the use of nanomaterials for a variety of

applications. New categories of nanomaterials such as carbon

nanotubes, nanomaterials, nanotube and quantum atoms are

assembled into atoms using various applications of advanced

technology, for example, electronics, biomedical, energy and

environment. For applications in the civil infrastructure (such

as bridges, dams and buildings), these materials are still

expensive and cannot be produced only in relatively small

quantities, which limits their applications. Recent research

has revealed that conventional concrete can be characterized

by a thorough examination of components containing

complex nanomaterials. In these cases, the properties of the

macroscopic material can be altered radically by

manipulating the nanoparticle during its own manufacturing

process (Alkhateb et al.,2013)[1]. Although cement building

materials are widely used in large quantities and in huge

quantities, the basic characteristics of these materials such as

compressive strength, splitting tensile strength, creep,

shrinkage, flexural strength, and durability depend largely on

structural elements and phenomena that are effective in micro

and most important in the nanometer (Shah et al.,2011)[7].

Thus, graphene oxide(GO) is a good additive for the concrete

due to its high aspect ratio, excellent dispensing in water and

improved mechanical properties. The mechanical properties

of graphene oxide-cement composite (GOCC) depend upon

the GO content as well as the shape of the nucleated crystal

mailto:[email protected]





upon hydration (Lv et al.,2014)[8]. In addition, (GO) can

enhance the mechanical properties by inhibiting the

propagation of cracks microstructural. It can also be used as

oil adsorption material in underwater construction structures

(Rafiee et al., 2013)[9]. The main aim of the present study

was to prepare GO from EG. Then to investigate the effect of

GO on some mechanical properties of graphene oxide

concrete nanocomposite (GOCNC), such as the compressive

strength, flexural strength or modulus of rupture, splitting

tensile strength tests.

2. MATERIALS AND EXPERIMENTAL

Natural graphite powders (99.8%, Sigma, Germany), nitric

acid (HNO3,69 %), concentrated sulphuric acid (H2SO4, 98%,

ROMIL, UK), Potassium Permanganate (KMnO4),

Hydrochloric acid (HCl, 37%, CDH), Hydrogen Peroxide

(H2O2, 30%, GMBH, Germany) were used for the preparation

of graphene oxide. Sand is sieved particles size range

between (150-600 µm) which was (SO3 = 0.041),

Superplasticizer: Sika Visco Crete(hi–tech1316), and

commercially available ordinary Portland cement, Baziyany

brand type I.

The experimental methods have been used to prepare

expanded graphite (EG), graphene oxide (GO) and graphene

oxide concrete nanocomposite (GOCNC). The EG was

prepared from graphite powder and then GO was prepared

from EG. Characterization methods were Fourier Transform

Infrared spectrophotometer (FTIR), X-ray Diffraction

(XRD), and Atomic Force Microscopy (AFM) have been

used to confirm the success of conversion EG to GO layers.

Furthermore, GOCNC mixture would be prepared using

different percent of GO to study its mechanical properties,

such as compressive strength, splitting tensile strength,

flexural strength and using scanning electron microscopy

(SEM) of GOCNC.

3. PREPARATION OF EXPANDED GRAPHITE BY

MICROWAVE IRRADIATION

The EG was prepared by mixing graphite powder (1g) with

concentrated HNO3 (2g) and KMnO4 (1g) in weight ratio

(1:2:1) (Wei et al., 2008) [10]. To obtain expanded

graphite(EG), the mixture was stirred by hand in a glass flask

at room temperature. Then, the mixture was put in a domestic

microwave to be irradiated for 80 sec. Figure1shows the

obtained EG powder before and after washed using distilled

water for several times until the pH of 7. Thereafter, the wet

EG powder was dried at 110°C for six hours .

Fig. 1: (a) Expanded graphite (EG), (b) EG after washing and filtration

4. PREPARATION OF GRAPHENE OXIDE (GO) USING EG

Graphene oxide (GO) was prepared by using the EG(80s) (1g) with mixed H2SO4 (20ml). Then, the mixture was transferred to

an ice bath at temperature (0-5OC) to prevent overheating and explosion. Under magnetic stirring KMnO4 (3g) have been slowly

added to the mixture for 20 min. The mixture color has become dark blue, which was transferred to water bath at (35- 45OC) for

30 min. Afterwards, distilled water (50 ml) was slowly added with continuous stirring. The mixture was transferred to water bath

at (80-98OC) with stirring for 15 min. until mixture color become Brown, as shown in Figure 2a. Thereafter, 140 ml of water

was added to the mixture with magnetic stirring for 15 min. The reaction terminated by adding 15 ml of hydrogen peroxide

(H2O2 30%) with stirring for one hour, until the color become bright Yellow, as shown in Figure 2b.

a b



Fig. 2:(a) Mixture color became Brown, (b) Color was changed to bright Yellow

Then, the GO washed in distilled water and dried in an oven at 50OC, Figure 3 shows the prepared GO in the present study.

Fig. 3: prepared graphene oxide(GO)

5. CONCRETE MIX DESIGN

The key features of GOCNC mixtures design include high

ratio of weight of sand / weight of cement (WS /WC =1/1),

fine sand with a particle size between 150 -600 µm, the

dosage of ratio of weight of water/ weight of cement

(WW/WC=0.35) and the weight of superplasticizer(PCE) /

weight of cement (WPCE/Wc) is 0.03. GO added to the

mixtures at five different ratios (0.01, 0.05, 0.1, 0.3, and 0.5)

% by weight of cement (weight of GO/weight of

cement=WGO /WC). These ratios of GO have been studied to

choose the optimum percent of GO, which gives the higher

compressive in nanocomposite. These mixtures have been

carried out in rotary mixer as follows.

Graphene Oxide has been added to water under sonication.

Then, superplasticizer was added to GO solution and the

mixture has been sonicated for 60 min. Then, the cement

added to the mixture (GO, water and superplasticizer) with

mixing for 60 sec. at low speed. The mixture was allowed to

rest for 2.5 min. and then, mixing was continued for 60s at

high speed. After that, the sand has been added gradually in

rotary mixer into (GO, water, superplasticizer and cement)

for 60 sec. at low speed, and at medium speed for a 120 sec,

then continuous for 30 sec. in high speed. Next, the fresh

concrete has been poured into the mold directly. The results

indicated that the additive 0.05%GO by weight of cement

gives compressive strength higher than other ratios when

tested at 7 days as shown in Table I, therefore this ratio

adopted to find compressive strength, flexural strengths and

splitting tensile strength at 7, 14 and 28 days. Table I shows

the details of weights materials that used in reference

specimens (Re) and GOCNC mixtures that used throughout

this investigation.

a b



Table I

Weights of Re and GOCNC mixtures

Mixes Wc (g) Ww (g) Ws (g) WGO (g) WPCE (g) Compressive strength )MPa( at 7days

Re

0.01% GOCNC

0.05% GOCNC

0.1% GOCNC

0.3 % GOCNC

0.5% GOCNC

435

433.56

434

434.7

434

434

152

152

152.88

152

152

152

435

435

435

434.7

434.7

434

0.0

0. 44

0.22

0.44

1.3

2.17

13

13

13

13

13

13

39.5

66.5

71

63.5

51

45

6. RESULTS AND DISCUSSION

The prepared GO from EG by using microwave (700W) for

80 sec. was characterized by X-Ray Diffraction (XRD)

(MiniFlex II, Rigaku Co., Japan), Fourier Transform Infrared

((FTIR)-Prestige 21 Shimadzu Co., Japan) and Atomic Force

Microscope ((AFM) Model: NT-MDT Ntegra, Russian

Federation) to prove successful production of GO.

6.1.X-RAY DIFFRACTION(XRD)

Figure 4(a) shows the XRD pattern of prepared EG

confirmed the crystalline structure of EG with a sharp peak

at (2θ=25.9o) corresponds to d-spacing of 0.344nm, in plane

(002). While the peak of the pristine graphite was at

(2θ=26.6°) in plane (002), which corresponds to an interlayer

distance of 0.338 nm (Moosa and Jaafar, 2017)[11], as shown

in Figure 4(b).

Fig. 4:XRD of (a) EG, (b) pristine graphite(Moosa and Jaafar, 2017)[11]

Thus, the GO that has been prepared from EG (80 s) , which it had ratio of WGO/ WW (0.5 mg/mL) was sonicated in ultrasonication

bath for one hour in distilled water. XRD pattern of sonicated GO shows new sharp peak (2θ=10.64o) with new interlayer

distance (d-spacing=0.83 nm) as shown in Figure 5.

b

2θ=26.6°



Fig. 5: XRD of GO prepared from EG at (80s)

The results confirmed complete conversion of EG into GO.

Additionally, the absence of impurity peaks explained the

high purity of the prepared GO. The oxidation process of

graphite to GO occurred due oxygen-group intercalation on

the inner and outer surfaces of graphite, which lead to the

loose stack of GO sheets (Viana et al.,2015)[12]. During the

steps oxidation of the graphite sheets react with oxygen

functional groups increased the distance between the layers

in accordance with the degree of oxidation of EG and the

quantity of molecules inserted into the interlayer spacing

(Esmaeili, et al.,2014)[13],(Song et al., 2014)[14].

6.2. ATOMIC FORCE MICROSCOPY (AFM)

Atomic force microscopy (AFM) has been used to

measurement and characterization graphene oxide (GO).

Figure 6 shows the thickness, lateral size and morphology of

GO, that was prepared from EG (80s). The thickness and

lateral size of GO layers were 0.52 nm and 439 nm

respectively. (Song et al., 2014)[14] reported that the GO

layers have a thickness of 2∼3 nm, and this was slightly

thicker than single layer of graphene. Therefore, this study

result indicated to formation single layer of GO.

Fig. 6: AFM of GO from EG (80s)

6.3 FOURIER TRANSMISSION INFRARED (FTIR) OF GO

The surface of GO had oxygenated groups such as epoxy (C-

O), hydroxyl (-OH), carboxyl(C=O) groups, which were

measured by FTIR. Figure 7 shows FTIR peaks for GO

prepared from oxidation of EG. The peak 3437 cm-1 exhibit

the characteristic of hydroxyl(O-H). The peak at 1728 cm-1

carboxyl bands (C=O) and the peak at 1400 cm-1 is for

aromatic (C=C). The peak at 1076 cm-1 indicated the

presence of epoxy (C-O) (Gholampour et

al.,2017)[15],(Pang and Sun, 2014) [16], (Senevirathna et

al., 2014) [17].

2θ=10.64o



Fig. 7: FTIR of GO prepared from EG (80 sec)

In this work, the result of the d-spacing was 0.831 nm, 2θ=10.64o and the minimum thickness of GO layer is 0.512 nm

for GO prepared from EG (80s). Thus, the data of AFM, XRD and FTIR images showed successful preparation of GO form

graphite.

7. MECHANICAL PROPERTIES OF GRAPHENE OXIDE- CONCRETE NANOCOMPOSITE (GOCNC) 7.1 COMPRESSIVE STRENGTH

The compressive strength test was performed of GOCNC, through numerous experiments were conducted using several percent

of GO (0.0, 0.01, 0.05, 0.1, 0.3 and 0.5) % by weight of cement. The results showed the highest compressive strength for

specimens containing 0.05%GO of the cement weight at curing time 7 days , as shown in Table II and Figure 8. The reason may

be due to this ratio is the quantity required to interact with cement compounds and formation of a solid material or the quantity

necessary for the full staffed spaces of existing through the structure of specimens. The results indicated that the compressive

strength increases with increasing GO ratios until it reaches 0.05% of the cement weight. However, after 0.05% the compressive

strength decreases because of the agglomeration of GO. This result is an agreement with other researchers (Lu and

Ouyang.,2017)[18], (Gholampour et al.,2017)[15]. The effect of 0.5%GO on compressive strength with curing time is shown

in Table II and Figure 8. The compressive strength of 0.05%GOCNC specimens increases with progress curing time. The

percentages of increases were 79.7% at 7 days, 65.9% at 14 days and up to 64 % at 28 days as shown in Figure 9. These results

are in agreement with other researchers (Devasena and Karthikeyan,2015)[19], (Lu and Ouyang ,2017) [18]. Table II

Compressive strengths for various types of mixtures

Mixes

Compressive strength (MPa)

7days 14 days 28 days

Re 39.5

66.5

71

63.5

51

45

47

_

78

_

_

_

51.2

_

84

_

_

_

0.01% GOCNC

0.05%GOCNC

0.1%GOCNC

0.3 %GOCNC

0.5%GOCNC



Fig. 8: Compressive strengths of GOCNC at 7 days

Fig. 9: Effect of curing time on compressive strength of 0.05%GO

7.2 FLEXURAL STRENGTH

Figure 10 shows the flexural strength of 0.05%GOCNC mixtures that contain 0.05% of GO at curing time 7, 14 and 28 days.

The flexural strength of 0.05% GOCNC and Re increased with increasing of curing time. The percentages were increased of the

flexural strength at 0.05%GOCNC specimens were 117% at 7 days, 64.4 % at 14 days and up to 29 % at 28 days. The increases

in flexural strength of 0.05% GOCNC is due to the reductions in the total porosity and due to the increases in the degree of

hydration of the cement paste which increase the density of concrete as explained by (Devasena and Karthikeyan,2014)[19] ,

(Lu and Ouyang.,2017)[18].

Fig. 10: Effect of curing time on flexural strength of 0.05%GOCNC and Re

7.3 SPLITTING TENSILE STRENGTH

Figure 11 shows the splitting tensile strength of the 0.05%

GOCNC and Re specimens at curing time 7, 14 and 28 days.

The splitting tensile strength of 0.05% GOCNC increased

with progress curing time more than reference specimen. The

percentages of increases were 78% at 7 days, 56 % at 14 days

and up to 22.2% at 28 days. The increase in the splitting

tensile strength is may be due to the 0.05%GO ratio leads to

0 0.01 0.05 0.1 0.3 0.5

GOCNC at (7day) 39.5 66.5 71 63.5 51 45

0

10

20

30

40

50

60

70

80

Com

pre

ssiv

e S

tren

gth

(M

Pa)

WGO /WC %

7 14 28

GOCNC 11.7 12.5 14

Re 5.4 7.6 11.23

0

2

4

6

8

10

12

14

16

Fle

xura

l St

ren

gth

s(M

Pa)

Age(days)

7 14 28

GOCNC 71 73 84

Re 39.5 47 51.2

0

20

40

60

80

100

Co

mp

ress

ive

Stre

ngt

h(M

Pa)

Age ( days)



the decrease in the porosities and enhancement of

densification of matrix (Kim et al.,2017)[20], (Babak et

al.,2014)[21].

Fig. 11: Effect of curing time on splitting tensile strength of 0.05%GOCNC and Re

8. SEM OF CONCRETE NANOCOMPOSITE

The scanning electron microscopy (SEM) microstructural analysis of the Re and 0.05%GOCNC specimens cured to 28 days are

shown in Figure 12 and Figure 13. The reference concrete specimen was porous as shown in Figure 12 (a) and (b).

Fig. 12: SEM images of fracture surface of Re (a) low magnification; (b) Higher magnification

SEM images of 0.05%GOCNC shows that GO layers are well dispersed and no GO agglomeration. The 0.05%GOCNC

specimen was dense with low porosity as shown in Figure 13. The reduction in the porosities were the reason for the increases

in the values of mechanical properties and improvement durability of concrete.

Fig. 13: SEM images of fracture surface of 0.05% GOCNC (a) low magnification; (b) Higher magnification

7 14 28

GOCNC 7.3 7.8 7.97

Re 4.1 5 6.52

0

2

4

6

8

10

Split

tin

g te

nsi

le(M

Pa)

Age(days)

a b

a b



9. CONCLUSIONS

In this research was prepared EG, then confirmed complete

conversion of exfoliated graphite (EG) to graphene oxide

(GO). Afterward, GO was added to concrete, the

compressive strength of GOCNC was increased with

increasing WGO /WC ratio. The best ratio of WGO/ WC was

0.05% for GOCNC which gives the highest value of

compressive strength. Less than 0.05% GO is uniformly

distributed in concrete, and greater than 0.05% the

compressive strength decreased because of the agglomeration

of GO. The percentages of increases in the compressive

strength, flexural strength and splitting tensile strength of

GOCNC with 0.05% GO and 3% Sika Visco Crete (hi –tech

1316) were 64% ,29% and 22.2% respectively at curing time

28 days compared to the reference sample(Re). The addition

of GO to concrete mixture enhanced the compressive, split

tensile and flexural strengths. SEM of the best ratio (WGO/

WC = 0.05%) in GOCNC showed that GO was well dispersed

and no agglomeration.

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