Edge-Oxidized Graphene Oxide as Additive in

Fiber-Reinforced Concrete: Effects on

Fresh and Hardened Properties
Mohammad Khawaji 1; Byoung Hooi Cho, Ph.D. 2; Boo Hyun Nam, Ph.D., M.ASCE 3;
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Yousef Alharbi, Ph.D. 4; and Jinwoo An, Ph.D. 5

Abstract: This study experimentally investigates the effects of edge-oxidized graphene oxide (EOGO), which is a low-cost carbon-based
nanomaterial, on fresh and hardened properties of normal portland cement concrete (PCC) and fiber-reinforced concrete (FRC). Interestingly,
adding EOGO to normal concrete mixtures improves the workability of concrete. In this regard, EOGOs as an additive were applied to FRCs
in order to improve FRCs’ low workability without losing mechanical enhancement due to EOGOs. Two fiber types of basalt fiber (BF) and
steel fiber (SF) were used in this study. First, 0.05% of EOGO by the cement weight was mixed in basalt FRC (BFRC) mixture, which is 0.1%
of the BF by the concrete volume. Second, considering the results of BFRC, 0.1% of EOGO was employed in steel FRC (SFRC) mixture with
1.0% of SF by the concrete volume. Testing was aimed at investigating the effects of EOGO on the workability and mechanical strengths of
the FRC mixtures. The test results illustrate that the EOGO improves workability more than 100% in the SFRC mixture but about 20% in
the BFRC mixture. The EOGO provides a slight increase of both compressive and flexural strengths for normal concrete and SFRC mixtures.
In contrast, it was observed that the EOGO increases the flexural strength of SFRC in terms of initial crack generation and range of elastic
behavior. The EOGO-SFRC required more than 30% of energy to reach the initial crack point than the SFRC mixture. DOI: 10.1061/(ASCE)
MT.1943-5533.0003092. © 2020 American Society of Civil Engineers.
Author keywords: Edge-oxidized graphene oxide (EOGO); Basalt fiber-reinforced concrete (BFRC); Steel fiber reinforced concrete
(SFRC); Workability; Mechanical properties; Flexural behavior.

Introduction in single-walled, double-walled, or multiwalled. CNFs are formed

in a cylindrical nanostructure, and GO is a single-layered carbon
Over the past decades, several types of nanomaterials, such as network with a functionalized oxygen group.
nanosilica (nano-SiO2 ), nano-titanium dioxide (nano-TiO2 ), car- GO has a two-dimensional sheet form that has sp2 -orbital bond-
bon nanotubes (CNTs), carbon nanofibers (CNFs), and graphene ing carbon atoms (Lin et al. 2016; Warner et al. 2012). GO has
oxide (GO), have been introduced to cement composites for per- unique properties like high strength, high toughness, large surface
formance enhancement. Particularly, carbon-based nanomaterials area, and surface functionalization (Li et al. 2015; Lu et al. 2017;
significantly improve mechanical properties of cementitious com- Wu et al. 2017). The large surface area of GO that has a large
posites with high Young’s modulus and tensile strength (Ferro et al. amount of functionalized oxygen groups works as nucleation sites
2011; Kim et al. 2016; Lee et al. 2018a; Safiuddin et al. 2014). for the formation of hydration products and regulates and refines
They are composed of carbon atoms that connected with C–C the microstructure of cement hydration products (Lv et al. 2013;
bonds. From a morphological perspective, CNTs could be formed Wang et al. 2017; Zhao et al. 2017). GO plays a role in accelerating
the rate of cement hydration due to its nucleation effect (Li et al.
1
Graduate Research Assistant, Dept. of Civil, Environmental, and 2017a; Yang et al. 2017) and acts as fibers holding the tensile
Construction Engineering, Univ. of Central Florida, 12800 Pegasus Dr., stresses that initiated inside the cement paste matrix (Li et al.
Suite 211, Orlando, FL 32816. ORCID: https://orcid.org/0000-0002-3236 2017c), and GO fills and bridges, in nano-scale, the products of
-252X. Email: [email protected] cement hydration (An et al. 2018a). Incorporating GO in low
2
Postdoctoral Research Associate, Dept. of Civil, Environmental, and percentages in cementitious composites have shown improved
Construction Engineering, Univ. of Central Florida, 12800 Pegasus Dr.,
mechanical properties of cement paste and mortar where the com-
Suite 211, Orlando, FL 32816 (corresponding author). ORCID: https://
orcid.org/0000-0001-8897-7120. Email: [email protected]
pressive and flexural strength are improved in ranges of 30%–38%
3
Associate Professor, Dept. of Civil, Environmental, and Construction and 26%–70%, respectively, and the tensile strength is improved as
Engineering, Univ. of Central Florida, 12800 Pegasus Dr., Suite 211, well up to 40% for cement paste and mortar by incorporating GO in
Orlando, FL 32816. Email: [email protected] percentages of 0.03%–0.06% by the cement weight (Al-Muhit et al.
4
Assistant Professor, Dept. of Civil Engineering, King Saud Univ., 2015; Chuah et al. 2018; Gong et al. 2015; Li et al. 2017c; Lu and
P.O. Box 800, Riyadh 11421, Saudi Arabia. Email: [email protected] Ouyang 2017; Lv et al. 2014; Mohammed et al. 2016; Mokhtar
5
Assistant Professor, Dept. of Engineering, Univ. of Mount Union, 1972 et al. 2017; Pan et al. 2015; Wang et al. 2015). Even though adding
Clark Ave., Alliance, OH 44601. Email: [email protected]
GO to the cement composite materials enhances the mechanical
Note. This manuscript was submitted on April 16, 2019; approved on
August 26, 2019; published online on January 22, 2020. Discussion period properties, GO reduces the fluidity of cement composite mixtures
open until June 22, 2020; separate discussions must be submitted for in- in the range of 23%–60% where the GO percentages are in the range
dividual papers. This paper is part of the Journal of Materials in Civil of 0.01%–0.08% by the cement weight because GO has a large sur-
Engineering, © ASCE, ISSN 0899-1561. face area that requires more water to become wet. Regarding the

© ASCE 04020028-1 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 aspect of workability, it has been believed that GO agglomerates in- the fresh concrete workability (Arslan 2016; Branston et al. 2016;
side the cement composite matrix and captures the water, so it causes Dong et al. 2017; Jiang et al. 2014; Kizilkanat et al. 2015). Previous
a reduction in the free water quantity and in the workability of the researches recorded that the compressive strength of steel FRC
cement composites (An et al. 2018b; Gong et al. 2015; Li et al. (SFRC) was enhanced by 24% when 0.75% of hooked-end steel fi-
2017b; Lu and Ouyang 2017; Lu et al. 2017; Lv et al. 2016; Pan ber by the total concrete volume was added (Hasan-Nattaj and
et al. 2015; Shang et al. 2015; Wang et al. 2015). While those re- Nematzadeh 2017), and the flexural strength of SFRC was improved
searches are conducted on the cement paste and mortar mixture, it more than double the value of normal concrete when 2.5% of cor-
has barely performed on cement concrete composites with a coarse rugated steel fiber by the total concrete volume was added (jun Li
aggregate matrix (Devasena and Karthikeyan 2015; Lu and Ouyang et al. 2017). In addition, adding a small amount of basalt fiber (BF),
2017; Mohammed et al. 2017a, b). 0.85% by the cement weight, improves the concrete compressive
Edge-oxidized graphene oxide (EOGO) produced by a new me- strength by 7% (Arslan 2016) while adding the BF in a fraction
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chanochemical method could achieve cost reduction compared of 7.50% by the weight of cement enhances the concrete flexural
with the conventional GO produced by the Hummers method strength by 34% (Kizilkanat et al. 2015). However, the workability
(Garmor 2015). Hummers method passes through three main steps: of SFRC and basalt FRC (BFRC) have shown reductions for all
oxidation, purification, and exfoliation of graphite, and these proc- cases compared with the normal PCC with possible decreases up to
esses produce high manufacturing cost (Zhao et al. 2017). In 50% or less (Dong et al. 2017; Hasan-Nattaj and Nematzadeh 2017;
contrast, the newly developed mechanochemical method uses a Jiang et al. 2014; jun Li et al. 2017; Kizilkanat et al. 2015).
ball-milling process associated with a non-toxic oxidizing agent In this study, the effects of EOGO on FRC (both BFRC and
to mill the graphite powder, so few layers of EOGO are produced SFRC) properties were studied. A workability test was performed
as a flake shape. Since this mechanochemical method has a low to determine the fresh properties of the FRCs. Compressive and
cost, EOGO nanoflakes can be expected to incorporate practically, flexural strength tests were performed to measure the mechanical
in a large amount, in the concrete industry. The effects of EOGO on properties of the FRCs. In the first step, different percentages of
the fundamental mechanical properties of cement paste and mortar EOGO were mixed in normal PCC. Second, considering the results
mixture have been examined to analyze the microstructure and of the first step, a selected dosage of EOGO was added into the
chemical compositions (Al-Muhit et al. 2015; An et al. 2018a; basalt fiber-reinforced concrete (BFRC). Finally, the EOGO was
Chuah et al. 2018; Gong et al. 2015; Li et al. 2017a, b, c; Lu and mixed in SFRC mixtures with the consideration of the results of
Ouyang 2017; Lv et al. 2013; Mohammed et al. 2016; Mokhtar the first and second steps. In addition, the flexural behavior of
et al. 2017; Pan et al. 2015; Wang et al. 2015, 2017; Yang et al. EOGO mixed SFRC was discussed and associated with the first
2017; Zhao et al. 2017). The results of a preliminary study show crack initiation and its ductility.
that the EOGO improves the workability of the cement concrete;
thus, in the proposed study, the enhanced workability in concrete
due to EOGOs was explored in fiber-reinforced concrete (FRC), Experimental Program
which is a low-workable concrete mixture.
Different kinds of fibers have been commonly used in concrete to
improve the mechanical capabilities of the cementitious materials. It Materials
has widely known that steel fiber (SF) improves the toughness of
cement composites and increases the ductility of the concrete mate- Edge-Oxidized Graphene Oxide
rials but dramatically reduces the workability (Abbass et al. 2018; In this study, EOGO was used as an additive in the cement concrete
Boulekbache et al. 2016; Lee et al. 2018b; Leone et al. 2018; Li mixtures. Fig. 1 shows a schematic diagram of how EOGOs are
and Li 2017; Liang and Wu 2018; Mahmod et al. 2018; Yoo produced through the mechanochemical process with ball milling
et al. 2017). Basalt fiber (BF), which is a relatively new type of fiber and non-toxic oxidizing agent (An et al. 2019). In a custom tank
offering innovative applications in concrete composites, has been re- with a capacity of 1.4 L, stainless steel balls of 6 mm diameter and
ported to improve the concrete mechanical properties, such as com- 1 g weight each are employed to mill the graphite into nanoflakes at
pressive, flexural, and tensile strengths, but to significantly reduce a rate of 700 rpm (Blair et al. 2014), and the non-toxic oxidizing

Fig. 1. Production procedure of EOGO nanomaterial. (Reprinted from Composites Part B: Engineering Vol. 173, J. An, B. H. Nam, Y. Alharbi, B. H.
Cho, and M. Khawaji, “Edge-oxidized graphene oxide (EOGO) in cement composites: Cement hydration and microstructure,” 106795, © 2019, with
permission from Elsevier.)

© ASCE 04020028-2 J. Mater. Civ. Eng.

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 Table 1. Chemical components and physical properties of EOGO 100
Experimental
Parameter Value
80 High

Percent (%) passing

Carbon (%) 90–95
Low
Oxygen (%) 5–10 60
Surface area (m2 =g) 200–300
Nominal particle size (nm) 500
40
Density (g=cm3 ) ∼1.0

20

agent is added to generate functionalized oxygen group on the pro- 0

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0.01 0.1 1 10
duced graphite nanoflakes (Garmor 2015). This process provides
(a) Particle size (mm)
EOGO nanoflakes consisting of multiple layers of carbon sheets
(e.g., up to ten layers), and reactive functionalized oxygen groups 100
are attached to the periphery of each layer. These physical and
Experimental
chemical characteristics of EOGO nanoflakes were investigated 80 High

Percent (%) passing

in a previous study using attenuated total reflectance-Fourier trans-
Low
form infrared (ATR-FTIR) spectroscopy and Raman spectroscopy
60
techniques (An et al. 2019). Via this process, EOGO contains a
lower amount of reactive oxygen than conventional GO nanosheet
40
produced by a chemical treatment (referred to Hummers method),
which reaches about 30% oxygen (Lv et al. 2013). EOGOs contain
20
about 5%–10% oxygen, and the remaining non-oxygen composi-
tion is mainly carbon. Table 1 shows the chemical components and
physical properties of EOGO. Fig. 2 shows the images of scanning 0
1 10 100
electronic microscopy (SEM) and transmission electron micros- (b) Particle size (mm)
copy (TEM) of the EOGO used in this study. The purpose of
SEM images is to identify the size and morphology of the nano- Fig. 3. Gradation curve of aggregates: (a) fine aggregate; and (b) coarse
material, while TEM images are useful for imaging a sample’s layer aggregate.
conditions with a significantly higher resolution if they are com-
posed of either a single or multiple ultrathin layers (Lin et al.
2016; Warner et al. 2012). The SEM image of EOGO shown in
Fig. 2(a) clearly identifies the flake shape of EOGO. The nominal (ASTM 2018a) standards for concrete aggregates. Figs. 3(a and b)
particle size was statistically determined; 90% of the particles have show the gradation curves of the fine and coarse aggregates used
diameters less than 800 nm, and their nominal size was computed in this study, respectively. Table 2 summarizes the properties of
as 500 nm (Alharbi et al. 2018). The TEM image of EOGO shown those fine and coarse aggregates. All aggregates were oven-dried
in Fig. 2(b) presents the multilayer condition of the EOGO flake at 110°C for 24 h to achieve a dry condition. The oven-drying pro-
(An et al. 2019). cedure follows ASTM C127 (ASTM 2015a) and ASTM C128
(ASTM 2015b) for coarse and fine aggregates, respectively.
Portland Cement Concrete
Ordinary portland cement (OPC) Type I satisfying the requirement Fibers
of ASTM C150 (ASTM 2018b) was mixed in the concrete mix- In this experimental study, two types of fiber were employed, BF
tures. In the concrete mixture, standard sand and granite were used and SF, that have totally different physical properties, such as the
as fine aggregate and coarse aggregate, respectively. The fine and type of raw material, specific gravity, strength, and water absorp-
coarse aggregates satisfy the requirement specified in ASTM C33 tion capability, although the concrete containing these two fibers

Fig. 2. Images of EOGO: (a) SEM (reprinted with permission from Alharbi et al. 2018); and (b) TEM (reprinted from Composites Part B:
Engineering Vol. 173, J. An, B. H. Nam, Y. Alharbi, B. H. Cho, and M. Khawaji, “Edge-oxidized graphene oxide (EOGO) in cement composites:
Cement hydration and microstructure,” 106795, © 2019, with permission from Elsevier).

© ASCE 04020028-3 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 Table 2. Properties of fine and coarse aggregates the dry EOGO powder was uniformly distributed in cementitious
Properties Fine aggregate Coarse aggregate mixtures. A previous study reported that the dry mixing method has
shown similar performance for both fresh and hardened properties
Specific gravity 2.66 2.69
compared with the water-sonication method, which can confirm
Absorption (%) 0.52 0.60
the uniform distribution of EOGO in the cementitious matrix (An
et al. 2018b).
Three different series of concrete mix designs were employed
in this study. First, different amounts of EOGO (0.01%, 0.05%,
and 0.10% by weight of cement) were mixed in concrete. The test
results indicated the EOGO increases the workability of concrete.
The details are discussed in the Results and Discussion Section. The
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EOGO was then applied to FRC mixtures to compensate for the re-
duced workability due to the fibers to maintain the high mechanical
performance of concrete. BFRC and SFRC were chosen to verify the
efficiency of EOGO in the concrete workability, and the mechanical
strengths were then measured on those FRC mixtures. Second, the
BFRCs were mixed and tested. For the BFRC mixing group, 0.05%
of EOGO (by the cement weight) and 0.10% of basalt fiber (by the
concrete volume) were designed in accordance with the standards
ACI 211.1, ACI 211.3, ACI 318, and ACI 302 (Kosmatka and
Wilson 2011). The 0.05% of EOGO was selected based on the re-
sults of the first test with the normal PCC mixture. Third, the
Fig. 4. Fibers used in this study: (a) BFs; and (b) corrugated SFs. SFRCs were then designed based on the testing results of normal
PCC and BFRC. For the SFRC mixing group, four different con-
crete mixes including normal concrete (Control), EOGO-concrete,
SFRC, and EOGO-SFRC were prepared. The selected percentages
may not be sufficient for predicting the behavior of other types of of EOGO and SF were 0.1% (by the weight of cement) and 1.0%
FRC. BF with a length of 25 mm and a diameter of 10–22 μm was (by the concrete volume), respectively. The 0.1% of EOGO was
used in the BFRC mixtures. The specific gravity was 2.67, and the selected because the study focused more on the enhancement of
water absorption was 11%. In contrast, a SF with corrugated shape workability rather than the improvement o mechanical properties.
was used in this study to prepare the SFRC mixtures. The corru- Tables 4 and 5 show the actual mix design adopted in this study and
gated SF had a length of 25 mm and an aspect ratio of 43 with a present the percentages of EOGO, basalt fiber, and steel fiber used
minimum tensile strength of 345 MPa. The SF meets the physical in the BFRC and SFRC concrete mixtures, respectively.
property requirements of the ASTM A820 standard [ASTM A820
(ASTM 2011)]. Fig. 4 shows the photos of basalt and SFs, and Mixing Procedure
Table 3 provides the physical properties of both fibers. Mixing concrete matrixes followed ASTM C192 (ASTM 2016a),
the standard practice for making and curing concrete test specimens
in the laboratory. Coarse and fine aggregates were first placed in a
Mix Design and Specimen Preparation mixer with a small amount of water to make the aggregates have a
pre-wet condition, and the mixer was started to rotate and cement
Mix Design that was pre-mixed with EOGO and fibers were added in the mixer.
The EOGO was mixed in normal PCC and FRC mixtures to inves- The mixer was rotated until all components were uniformly distrib-
tigate the effects of EOGO on fresh and hardened properties of uted in the mixture by visual inspection. Afterward, water was
the different types of concrete mixtures. The water to cement placed in the mixer, and the mixture was consecutively mixed
(w/c) ratio of 0.5 was used for all cases, and the proportion of for 3 min followed by 3 min rest. Lastly, the mixture was remixed
cement∶sand∶aggregate was 1.0∶2.1∶2.3. The EOGO as a dry pow- for an additional 2 min.
der was manually mixed with the cement prior to the addition of
water. First, a designated amount of EOGO was mixed with 1 kg of Specimen Preparation
cement in a sealed plastic bag by hand for 20 min. Afterward, the Testing specimens were prepared for slump, compressive, and flexu-
dried cement-EOGO mixture was remixed with the whole amount ral strength tests following ASTM C192 (ASTM 2016a). Standard
of cement to be used in a concrete batch by scoop for another cylinder (100 × 200 mm) and beam (100 × 100 × 350 mm) speci-
20 min. This process occurred 1 day before starting the concrete mens were cast to measure the mechanical properties of the hardened
mixing. This dry powder mixing method may give more practical concrete. The concrete cylinder and beam testing specimens satisfy
benefit in the construction field when it can be ensured that the the requirements of ASTM C39 (ASTM 2016b) and ASTM C78
EOGO powder is uniformly distributed in the mixtures. In this re- (ASTM 2018c), respectively. Three (3) samples of each mix ID
gard, one of the previous studies provide indirect information that for both curing ages of 7 and 28 days were prepared for repetitive

Table 3. Physical properties of different fibers used in this study

Length Diameter Aspect Specific Tensile Absorption
Fiber type Material (mm) (μm) ratio gravity strength (MPa) (%)
Basalt fiber (BF) Naturally mined igneous rock 25 10–22 — 2.67 1,100 11
Steel fiber (SF) Low carbon steel 25 — 43 7.86 ≥345 —

© ASCE 04020028-4 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 Table 4. Mix design used in EOGO and basalt fibers concrete mixtures
Mix ID Cement (kg=m3 ) Water (kg=m3 ) Coarse aggregate (kg=m3 ) Fine aggregate (kg=m3 ) EOGO (g=m3 ) BF (kg=m3 )
CONTROL 384.50 192.25 881 800 0.0 0.0
EOGO 384.50 192.25 881 800 192.25 0.0
BFRC 384.50 192.25 881 800 0.0 2.67
EOGO-BFRC 384.50 192.25 881 800 192.25 2.67

Table 5. Mix design used in EOGO and steel fibers concrete mixtures
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Mix ID Cement (kg=m3 ) Water (kg=m3 ) Coarse aggregate (kg=m3 ) Fine aggregate (kg=m3 ) EOGO (g=m3 ) SF (kg=m3 )
CONTROL 384.50 192.25 881 800 0.0 0.0
EOGO 384.50 192.25 881 800 384.50 0.0
SFRC 384.50 192.25 881 800 0.0 78.6
EOGO-SFRC 384.50 192.25 881 800 384.50 78.6

testing. The specimens were demolded after 24 h of casting, and they bottom cube mold is filled by the self-compacted concrete mixture.
were stored and cured in a water bath that had a relative humidity of The excess of concrete remaining above the level of the top of the
100% and a laboratory ambient temperature of 23°C until testing. cube mold is cut off without any artificial compaction. The weight
The compressive and flexural strength tests were performed at the of the bottom cube filled with concrete is recorded as a partially-
ages of 7 and 28 days for all mixtures. compacted concrete weight. Afterward, the bottom cube mold is
fully compacted by a hand vibrator, and the weight of the cube
mold is measured as a fully compacted concrete weight. The com-
Test Procedure paction factor can be computed by Eq. (1). Table 6 could be used to
evaluate the workability of concrete based on the compaction factor
Workability value [BS-1881:Part103 (BSI 1983)]
A slump cone test was performed to evaluate the effect of EOGO
Compaction factor ¼ ðW p − W e Þ=ðW f − W e Þ ð1Þ
on the workability of different concrete mixtures according to the
ASTM C143 standard [ASTM C143 (ASTM 2015c)]. Six consecu- where W p = weight of the cube mold with partially-compacted con-
tive slump readings (for each mix ID) were measured from one crete (kg); W f = weight of the cube mold with fully compacted
batch of the concrete mixture. The mixture materials used for each concrete (kg); and W e = weight of the empty cube mold (kg).
slump test were remixed with the rest of the concrete mixture in the
same batch, and the slump tests were consecutively performed six Strength Tests
times using an identical method. The six consecutive slump tests A universal testing machine (INSTRON-5594-E1-F4-G1) was used
were finished in 30 min after mixing the mixture, and the speci- for compressive and flexural strength tests in accordance with
mens for strength tests were cast using the rest of the mixture. This ASTM C39 (ASTM 2016b) and ASTM C78 (ASTM 2018c),
ensures the quality of the specimens and the consistency between respectively.
the materials for the slump test and specimens for the strength test. Compressive strength tests were performed on the cylinder
By this method, the consecutive slump tests were duplicated and specimens cured for both 7 and 28 days. A four-point loading
averaged for three batches for each mix design (CTRL, EOGO, flexural strength tests were performed on the concrete beam spec-
SFRC, and EOGO-SFRC). imens cured for 7 and 28 days, and the modulus of rupture (R) of
In addition, a compaction factor test [BS 1881 Part 103 (BSI the samples was determined by Eq. (2)
1983) and ACI 211.3 (Neville and Brooks 1987)] was performed
on the SFRC mixtures to investigate their workability under the R ¼ PL=bd2 ð2Þ
construction environment where the reinforced rebars exist. The
compaction factor tests were conducted after the sixth reading of where R = modulus of rupture (MPa); P = maximum applied load
the slump test. The compaction factor test apparatus was custom- (N); L = span length (mm); b = average width of specimen at frac-
ized for this study based on the total energy conservation concept ture (mm); and d = average depth of specimen at fracture (mm).
(equivalent volume of hoppers and dropping height), and the ap-
paratus is shown in Fig. 5(a). Two different cube molds with the
Results and Discussion
same dimensions (150 × 150 × 150 mm) were used to measure
the compaction factor for two different cases: (1) without rebars
and (2) with double-layered #6 rebars, as shown in Fig. 5(b). The Effects of EOGO on Normal PCC
purpose of using two different cube cases is to evaluate the ability
of fresh concrete to flow through rebars as a simulation of actual Workability
concrete pouring conditions in construction fields. Fig. 6 presents the results of the slump test for the EOGO mixed
The compaction factor test is conducted by placing the concrete normal PCC. It shows that the slump value of the concrete increases
to fully fill the upper hopper without artificial compaction. Then, as the EOGO content increases. Adding 0.01% of EOGO could
the gate underneath the upper hopper is opened, so the concrete increase the concrete slump 26% compared to the control mixture.
naturally moves downward to the lower hopper by only the con- Moreover, adding 0.05% and 0.10% of EOGO improves the con-
crete weight. Next, the gate underneath the lower hopper is opened, crete workability by about 36% and 42%, respectively. This in-
and the concrete also drops down only by its weight. Then, the creased slump in concrete due to EOGO is opposite to our previous

© ASCE 04020028-5 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

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Fig. 5. Schematic of compaction factor apparatus customization: (a) hoppers and bottom cube positions; and (b) different cube cases.

Table 6. Relationship between the compaction factor and the degree of 250
concrete workability [BS-1881 (BSI 1983)] 36% 42%
200 26%
Compaction factor value Degree of workability
Slump (mm)

∼0.78 Very low 150

0.78 ∼ 0.85 Low
0.85 ∼ 0.95 Medium 100
0.95∼ High
50

0
study of EOGO on cement paste and cement mortar (Alharbi et al. CONTROL EOGO-0.01% EOGO-0.05% EOGO-0.10%
2018). More discussion is present in later sections. Mix ID

Compressive and Flexural Strengths Fig. 6. Results of the slump test for EOGO-concrete.
Figs. 7(a and b) show the results of compressive and flexural
strength tests for the EOGO-concrete with 7 and 28 curing days,
respectively. The results show that the EOGO slightly enhances the the 7-day cured samples. In this study, the highest flexural strength
compressive strength for both the 7-day and 28-day cured speci- is shown at 0.05% of EOGO and a decreasing trend is shown,
mens. The improvement by adding the EOGO is clearer in 28 days exhibiting a 16% increment over the control mixture.
than in 7 days. In the 0.1% EOGO mixture, the compressive
strength is improved by about 16% for the 28-day cured specimen, Discussion
while 13% of increment is shown for the 7-day cured samples. Interestingly, the workability of concrete is enhanced by EOGO,
However, the relationship between the amount of EOGO and the which is the opposite of previous studies that show the workability
compressive strength is not clear in the EOGO-reinforced concrete. of cement paste and mortar decreases with an increasing amount of
The results of the flexural strength test show a small improvement EOGO (An et al. 2018b). The only difference between concrete
by adding the EOGO, particularly for the 28-day flexural strength. mixture and cement paste and mortar mixtures is the presence
For the 28-day cured sample, the EOGO gives a beneficial effect on of coarse aggregate. Therefore, it could be logically assumed that
the flexural strength, whereas little enhancement was observed for the coarse aggregate may influence the opposite phenomenon of

© ASCE 04020028-6 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 50 200
Compressive strength (MPa) 36%
7-day 28-day 1.14 1.11 1.16
40 150
1.00

Slump (mm)
1.13
30 1.08
1.00 1.08
100
20 20%
50
10

0 0
CONTROL EOGO-0.01% EOGO-0.05% EOGO-0.10% CONTROL EOGO BFRC EOGO-BFRC
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Mix ID
(a) Mix ID
Fig. 8. Slump test results for EOGO-BFRC mixtures.
10
7-day 28-day 1.16
Flexural Strength (MPa)

1.15
8
1.00 1.04 illustrating about a 20% increase of the workability at 0.05% of
6 EOGO-BFRC. It is likely due to the high absorption characteristics
1.00 1.04 1.03 1.03 of BFRC in the concrete mixture.
4
Compressive and Flexural Strength
2 The compressive and flexural strength tests were conducted on
the EOGO-BFRC with the curing of 7 and 28 days. The test results
0 are shown in Figs. 9(a and b). For a given mix design and curing
CONTROL EOGO-0.01% EOGO-0.05% EOGO-0.10% conditions, the BFRC and EOGO-BFRC show similar or lower
(b) Mix ID strength levels for both compressive and flexural strength for the
7-day and 28-day cured specimens, whereas EOGO slightly im-
Fig. 7. Mechanical strength for EOGO-concrete with normalized proves the strengths of normal PCC. In particular, it is interesting
values: (a) compressive strength for 7 and 28 days; and (b) flexural to note that the EOGO-BFRC illustrates even lower compressive
strength for 7 and 28 days. strength than the BFRC. In this aspect, the interaction between
EOGO and BF seems not to positively affect strength.
the workability of the EOGO-concrete mixture compared with Discussion
paste and mortar mixtures. In this regard, it seems that EOGOs Unlike the EOGO-concrete, adding EOGO in the BFRC mixtures
are primarily positioned between coarse aggregates and other parts does not significantly improve the performance of BFRC. This may
of the cement mixture. A possible assumption is that EOGO re- be attributed to the high absorption capacity of BFs (11%). The
duces friction or adhesion between the coarse aggregates and ag- absorption capacity of a typical granite coarse aggregate used in
glomerated cement mortar by coating the coarse aggregates. This this study is 0.6%. This high absorption of BF may absorb the
may result in a relatively smooth movement of the coarse aggre- EOGO with water and limits the dispersion of EOGO inside the
gates within the fresh EOGO-concrete mixture, exhibiting a more BFRC mixtures. Therefore, the EOGO may not work properly
flowable behavior than a normal PCC mixture. This observation of for the BFRC mixtures. Moreover, although all aggregates were
the EOGO-concrete is also in contrast to the workability results that first mixed with BF followed by cement with EOGO, and well
GOs reduce the workability of the cement paste and mortar mixture dispersion of BF in the dry mixture was confirmed, it was some-
without coarse aggregate (An et al. 2018b; Lee et al. 2018a). The what observed that the BF strands were clumped, known as balling
testing results indicate that EOGOs produce minor improvement of of fibers, by adding and mixing the water. It has been reported that
mechanical strength. Although it has been reported that GOs and BF is more susceptible to the balling effect than other types of fiber
EOGOs improve the mechanical properties in cement paste and like SF (Iyer 2014) and thus, it may negatively influence on the
mortar mixtures due to bridging and filling effects (An et al. 2018a; mechanical properties of concrete mixtures (Branston et al. 2016).
Li et al. 2017c), the EOGO seems not highly effective in concrete Based on the fresh and hardened properties of BFRC mixtures, the
mixtures. The possible reason might be the presence of a coarse actual benefit of adding EOGO in BFRC is quite limited. For the
aggregate that results in a more heterogeneous matrix. Despite next step, therefore, a steel fiber with zero water absorption was
overall enhancement in the workability and strength of the EOGO- selected, and the effects of EOGO on SFRC mixtures are investi-
concrete, adding 0.1% of EOGO caused a slight decrease in flexu- gated in aspects of the fresh and hardened properties. The results of
ral strength. Based on the testing results of the EOGO-concrete, the prior two testing tasks indicate that EOGOs mainly contribute
adding 0.05% of EOGO was recommended for the BFRC mix to concrete’s workability but not mechanical properties. Therefore,
design because 0.05% of EOGO provides the best performance in the SFRC design, 0.10% of EOGO was selected to maximize the
considering both workability and strength aspects. workability enhancement benefit of EOGO in the SFRC mixtures.
In addition, sufficient enhancement of mechanical properties can be
Effects of EOGO on BFRC contributed by SFs in the mixture.

Workability Effects of EOGO on SFRC

The result of the slump test for the EOGO-BFRC is shown in Fig. 8.
As seen in Fig. 8, the effect of EOGO in the workability of normal Workability
PCC was clear, exhibiting a 36% increase by 0.05% of EOGO com- The slump tests were performed and compared on the four different
pared with the control mixture. In contrast, the EOGO shows less concrete mixtures (control, EOGO, SFRC, and EOGO-SFRC) to
increase of the workability of BFRC mixture than the normal PCC, identify the effect of EOGO on low-workable concrete mixtures.

© ASCE 04020028-7 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 60 200
Compressive strength (MPa) 7-day 28-day 1.10 1.13 CONTROL EOGO
1.11
50
1.00 SFRC EOGO-SFRC
150
1.23
40

Slump (mm)
1.13 1.15
1.00
30 100

20
50
10

0 0
CONTROL EOGO BFRC EOGO-BFRC 0 5 10 15 20 25 30 35
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(a) Mix ID Elapsed Time (min.)

8
7-day 28-day 1.11 Fig. 11. Consecutive slump readings for different concrete mixtures.
1.09 1.11
Flexural strength (MPa)

1.00 1.00 1.06 1.09 1.05

6

4 Table 7. Compaction factor results of EOGO-SFRC mixtures

Bottom cube
2
Mix ID Without rebars (%) Longitudinal rebars (%)
CONTROL 94.8 83.9
0 EOGO 98.1 88.1
CONTROL EOGO BFRC EOGO-BFRC
(b) Mix ID SFRC 90.8 70.1
EOGO-SFRC 91.5 65.9
Fig. 9. Mechanical strength test results of 7 and 28 curing days for
EOGO-BFRC: (a) compressive strength for 7 and 28 days; and (b) flex-
ural strength for 7 and 28 days. repeated experiments. The results show that the slump readings
slowly decreased for the EOGO mixed SFRC mixture than other
types of concrete. Previous research has shown that slump values
are highly affected by water evaporation, cement hydration process,
150 and aggregate absorption of the concrete mixture during the mixing
42%
and delivering process (Alhozaimy 2009). In this respect, it could be
assumed that the simultaneous presence of EOGO and SF might
100 60% have a greater effect on the workability of the concrete mixture than
Slump (mm)

103% only the existence of EOGO.

For further investigation of concrete workability, the compac-
50 tion factor test was conducted, and the results are summarized
in Table 7. The results indicate that the EOGO enhances the con-
crete workability except for the case of double-layered longitudinal
0 rebars for the SFRC mixture. In this experiment, the compaction
CONTROL EOGO SFRC EOGO-SFRC factor test method was modified by considering 25 mm SFs and
Mix ID
double-layered #6 rebars simultaneously, although it was originally
Fig. 10. Slump test results of EOGO-SFRC. designed for normal cement concrete without rebars. These size var-
iables may seem to affect the results for the case of the longitudinal
rebar placed SFRC mixture. Nonetheless, all other cases show con-
The test results presented in Fig. 10 clearly show that the EOGO sistent results that EOGO can help to enhance the flowability of the
dramatically improves the slump values for both normal concrete concrete mixtures. Therefore, EOGO has meaningful potential for
and SFRC. Regarding the EOGO-SFRC mixtures, EOGO enhances applications in the construction field because EOGO improves the
almost the same amount of the slump by an absolute value of 40 mm workability in low fluidity, concrete-like SFRC mixtures.
for the control and SFRC mixtures in this study. These are 42% and
103% increments of the slump value by ratio for the control and Compressive and Flexural Strength
SFRC mixtures, respectively. Although 1.00% of steel fiber de- The results of compressive and flexural strength tests are presented
creases the workability of concrete by 60% compared to the control in Fig. 12. Fig. 12(a) shows the compressive strength of the four
mixture, 0.10% of EOGO by weight of cement considerably recov- (4) mixtures for both 7-day and 28-day cured samples. Although
ers the workability of SFRC mixture. about 30% enhancement of compressive strength was measured by
The slump tests were repeated consecutively six (6) times for adding EOGO in the 7-day cured SFRC mixture, almost the same
30 min after mixing all the concrete mixtures, the change of the level of compressive strength was recorded for the 28-day cured
slump values with time is presented in Fig. 11. The slump reading specimens. Previous research has shown that EOGO can motivate
decreases as time passes, which is expected for all mixtures. About a accelerating a rate of cement hydration process due to reactive oxy-
10-mm drop of the slump value was observed for the EOGO-SFRC gen groups around the EOGO. The functionalized oxygen group
mixture during the testing time, whereas more than 30-mm decre- could trigger forming calcium silicate hydrate (C–S–H) gel in the
ments were measured during the testing for the control, EOGO- cement composites. It is defined as the nucleation effect of EOGO,
concrete, and SFRC mixtures. These trends were observed in and this may contribute to the enhanced early strength of the

© ASCE 04020028-8 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 50 25
Compressive Strength (MPa) 7-day 28-day 1.19 1.21 CONTROL EOGO
1.09 1.58
40 1.00 20 SFRC EOGO-SFRC

1.22
30

Load (kN)
1.09 15
1.00
20
10
L/600
10
5
0 L/150
CONTROL EOGO SFRC EOGO-SFRC 0
0 0.5 1 1.5 2 2.5
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(a) Mix ID
Displacement (mm)
8
7-day 28-day 1.38 Fig. 13. Load-displacement curves for four different concrete mixes.
Flexural Strength (MPa)

1.39
1.32 1.22
6
1.00 1.05
1.00 1.00
4 Table 8. Energy-absorption related parameters derived from the flexural
load-deflection curve
2 Mixture
Parameter SFRC EOGO-SFRC
0
CONTROL EOGO SFRC EOGO-SFRC P1 (d1 ) 16.91 (0.083) 20.69 (0.101)
(b) Mix ID PP (dP ) 18.66 (0.491) 20.69 (0.101)
TD
d1 0.76 1.00
Fig. 12. Mechanical strength test results of 7 and 28 curing days
PD
600 18.58 18.80
for EOGO-SFRC: (a) compressive strength for 7 and 28 days; and
TD
600 8.16 9.21
(b) flexural strength for 7 and 28 days.
PD
150 14.58 7.41
TD
150 34.80 28.29

cementitious matrix (Li et al. 2017a; Yang et al. 2017). In the SFRC
mixture, the initially hydrated cement component by the nucleation
the concrete, and this process is repeated until failure of the speci-
effect of EOGO helped to increase the compressive strength of the
men (jun Li et al. 2017). In the EOGO-SFRC, however, this
mixture with steel fiber at an early age. However, the results doe not
multiple-peak phenomenon is not clearly observed in that only a
show that the EOGO can improve compressive strength in terms of
single peak is recorded (Fig. 13). This difference could be due
long-term performance from the experimental results. The flexural
to the presence of EOGO in the mixture.
strength test results of the four different mix designs are plotted in
The flexural performance of the SFRC and EOGO-SFRC
Fig. 12(b). The results show a trend that the EOGO slightly enhan-
mixtures were further investigated using the energy-absorption re-
ces the flexural strength of SFRC in comparison with the normal
lated parameters derived from the load-deflection curve (shown in
concrete. About 13% enhancement of the flexural strength of SFRC
Fig. 13) in accordance with ASTM C1609 (ASTM 2005). Toughness
was recorded by mixing with EOGO for 28-day cured specimens.
was determined by calculating the area under the load-deflection
Flexural Behavior of EOGO-SFRC curve. Table 8 summarizes the parameters related to the energy-
The effect of EOGO in the flexural behavior of concrete was absorption capacity of SFRC and EOGO-SFRC, and the parameters
further investigated based on the load-displacement curves of are P1 = first-peak load (kN); d1 = deflection at first-peak load (mm);
the four (4) mixtures (Fig. 13). Distinguishable behaviors are PP = Peak load (kN); dP = deflection at peak load (mm); T D d1 = area
observed in the EOGO-SFRC mixture associated with ductility under the load-deflection curve 0 to d1 (J); PD 600 = residual load at
and/or brittleness, while these behaviors are hardly identified in the deflection of L=600 (kN); T D 600 = area under the load-deflection
EOGO-concrete. The load-displacement curve of the EOGO-SFRC curve 0 to L=600 (J); PD 150 = residual load at deflection of L=150
specimen shows one peak at a maximum loading point, whereas (kN); T D150 = area under the load-deflection curve 0 to L=150 (J);
multiple peaks are shown in the curve of the SFRC specimen that and L = span length (mm).
is well known (Abbass et al. 2018; Hu et al. 2018; Lim et al. 2018; The capability of energy absorption in the range of elastic
Yoo et al. 2015). The single peak trend on the curve could be lim- behavior (T D d1 ) improved by more than 30% by EOGOs in the
ited since the EOGO of only 0.1% was adopted in this experiment, SFRC mixture. EOGO-SFRC also shows about 13% higher tough-
and there are possibilities to change the trend in accordance with ness value than SFRC at the deflection of 0.5 mm (¼ L=600).
different amounts of EOGO. Nonetheless, the trend could be iden- However, the results show that the absorbed energy is rapidly dis-
tified that the roof of the EOGO-SFRC curve almost covers the top sipated in EOGO-SFRC than SFRC after the deflection of L=600.
of the SFRC curve. This infers that the EOGO-SFRC could absorb It could be postulated that the rapid energy dissipation of EOGO-
more energy during the loading stage and extend the elastic range SFRC is related to the fact that more energy was absorbed in
in the mixture. The flexural tests were repeatedly performed with EOGO-SFRC than in the SFRC composite. As more energy is
three (3) samples per mixture ID, and an identical trend was ob- stored, more energy should be dissipated, which could be expressed
served in all cases. The peaks of the load-displacement curves by a phenomenon in which the energy dissipates rapidly at a thresh-
are highly correlated with cracks generation and their propagation. old value of displacement. In this respect, it could be presumed that
The presence of multiple peaks in the SFRC indicates that the steel there is a combination effect of EOGO and SF to play a pivotal role
fibers transfer and redistribute flexural stress after initial cracking in in preventing and delaying initial cracks in the mixture, resulting in

© ASCE 04020028-9 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2020, 32(4): 04020028

 storing more energy. Finally, at the deflection of L=150, SFRC strength, 0.05% EOGO shows the best performance of about an
presents a higher residual load (PD D
150 ) and toughness (T 150 ) than increase of 16%; afterward, the effect of EOGO then decreases.
EOGO-SFRC. • For the BFRC mixture, the effects of EOGO could not be sig-
nificantly observed on both fresh and hardened properties. This
Discussion might be because of the high-water absorption ratio of BFs and
Discussions are presented with respect to the three performance its balling effect inside the concrete matrix.
criteria of workability, mechanical strength, and flexural behavior. • For the SFRC mixture, the workability is significantly enhanced
First, regarding the workability, the effect of EOGO is more sig- by more than 100% by mixing 0.10% of EOGO by weight of
nificant in the SFRC than normal PCC. It could be assumed that cement, and it was observed that EOGO delays the slump loss of
EOGOs interact at the interface between the coarse aggregate and EOGO-SFRC mixture compared with SFRC.
cement matrix and between the SFs and cement matrix. The mobil- • Although a minor improvement of flexural strength was re-
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ity of the cement paste at those interfaces seems increased by the corded for 28-day cured EOGO-SFRC samples than SFRC,
presence of EOGO, thus resulting in improved workability. Second, it could be hardly concluded that EOGO provides beneficial
a slight improvement of flexural strength was observed for 28-day effects for the mechanical strengths of SFRC mixture.
cured EOGO-SFRC samples. However, it is barely recognized that • EOGO-SFRC exhibits a 30% higher energy-absorption capabil-
EOGOs significantly improve the overall mechanical properties of ity in the range of elastic behavior under the flexural loading
concrete mixtures for both normal PCC and SFRC. Conventional condition than the SFRC matrix. This can infer that EOGO
GO nanosheets show beneficial effects on the mechanical strength plays a role in delaying the initial crack generation and propa-
of cement paste and mortar mixtures alone not for concrete gation in the nanostructure or microstructure in the SFRC
(Al-Muhit et al. 2015; Chuah et al. 2018; Gong et al. 2015; Li et al. matrix.
2017b; Lu and Ouyang 2017; Lv et al. 2014; Mohammed et al. In conclusion, the beneficial effects of EOGO on the concept of
2016; Mokhtar et al. 2017; Pan et al. 2015; Wang et al. 2015). workability for different types of concrete mixtures are clearly
One of the reasons can be the decreased concentration of function- identified in this study, and this is quite the opposite phenomenon
alized oxygen groups in EOGO (5%–10%) compared with conven- onto cement paste or mortar composites. However, the advantage of
tional GOs (30%) by the Hummers method. It is reported that EOGO on mechanical properties are still controversial and need
oxygen groups promote the process of cement hydration (Li et al. more verification. Nevertheless, considering EOGO’s economic
2017a; Yang et al. 2017). However, the interaction at those inter- competitiveness, it seems to have an important potential as an
faces of GO and other ingredients can be a critical factor in strength additive to improve the workability of cement concrete or low-
development. Lastly, the enhanced resistance of crack generation workable concrete mixtures in the construction industry.
and propagation by EOGOs is an encouraging finding because
the benefit of GOs can be extended to FRC. EOGOs are beneficial
in the SFRC with two mechanisms: (1) to delay the initiation of
cracks, resulting in the extended range of elastic behavior and
Data Availability Statement
(2) to resist slippage of SF from the concrete matrix, increasing the Some or all data, models, or code generated or used during the
maximum loading of the EOGO-SFRC. According to the results of study are available from the corresponding author by request.
the tests, the EOGO contributes to the flexural behavior of concrete
composites, particularly in the range of elastic behavior and in the
range of small deflection after the first crack of the specimen. Acknowledgments
The existing study focused on the effect of EOGO in normal
PCC and FRCs but with a limited scope to workability, strength, The authors gratefully acknowledge Garmor, Inc. for their supply
and flexural behavior. Broader characterizations of EOGO- of EOGO to this research.
reinforced concretes such as durability and long-term performance
are necessary. In addition, further investigation is necessary in the
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