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Static and Cyclic Flexural Behaviors of

Edge-Oxidized Graphene Oxide Cement Composites


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

Abstract: This paper investigates the flexural fatigue behavior of cement mortar mixed with edge-oxidized graphene oxide (EOGO), a
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carbon nanomaterial reinforcing cement hydration products. EOGO is produced by a mechanochemical process that enables dramatically
reduced costs, making it suitable for large-volume infrastructure construction. The compressive and flexural strengths of the EOGO cement
mortar mixtures are also compared with the results of fatigue tests. Test results indicate that the cement mortar containing 0.05% of EOGO by
weight of cement exhibits the best flexural fatigue performance as well as compressive and flexural strengths. It is also found that the EOGO
mixed specimens show a faster increase in flexural fatigue strains than the control specimens under sinusoidal loading. This implies
that EOGO helps to prevent or delay the propagation of internal damage (e.g., microcracks) in the cement composites in an early fatigue
phase, resulting in enhanced flexural ductility. Thus, it is concluded that the EOGO can be used as an additive, with cost competitiveness,
for improving the structural fatigue performance of cementitious composites. DOI: 10.1061/(ASCE)MT.1943-5533.0002914. © 2019
American Society of Civil Engineers.
Author keywords: Edge-oxidized graphene oxide (EOGO); Cement mortar; Flexural fatigue; Flexural ductility.

Introduction The mechanism identified is that the nanobridging effects in the


cementitious matrix control nanoscale cracks and prevent or delay
Carbon nanomaterials such as carbon nanotubes (CNTs), carbon the growth of microscale and mesoscale cracks in the cement com-
fibers (CFs), graphene, and graphene oxide (GO) have been exten- posites (Ahmed et al. 2018; Li et al. 2017a, b; Lu and Leung 2016;
sively studied in recent decades in research fields of applied science, Mohammed et al. 2015; Musso et al. 2009; Nadiv et al. 2016).
technologies, and engineering because of their unique properties GO has a single layer of carbon atoms functionalized with
and combination synergy including electronic, optical, thermal, oxygen groups (Gao 2015), and a typical manufacturing process
mechanical, and chemical characteristics (Ajayan 1999; Huang et al. is a chemical process of oxidizing graphite. The functionalized
2011; Kroto et al. 1985). surface of GO plays an important role in acting as seeding material
Many previous researchers have reported that carbon nanoma- for hydration products and accelerating the hydration process, thus
terials cause mechanical improvements in cement and concrete contributing to an increase in the amount of calcium-silicate-
(Dreyer et al. 2014; Kumar et al. 2011; Lavagna et al. 2018; Tyson hydrate (C-S-H) gel in the cementitious matrix (Chuah et al. 2014;
et al. 2011; Vipulanandan and Garas 2008; Zhao et al. 2017). It has Ghazizadeh et al. 2018; Lv et al. 2014). Previous research has
been known that nanomaterials could improve the mechanical shown the positive effects of GO in cement composites of increas-
properties of hardened cement composites by acting as bridging ing compressive and flexural strengths (Al-Muhit et al. 2015;
elements in nanosize or microsize structures due to their high ten- Devasena and Karthikeyan 2015; Li et al. 2017a, b, c; Lu and
sile strength and modulus, large surface area, and high aspect ratio. Ouyang 2017; Mohammed et al. 2017; Mokhtar et al. 2017;
Sharma and Kothiyal 2015; Yang et al. 2017). These studies have
1
Postdoctoral Researcher, Dept. of Civil, Environmental and Construc- reported that the compressive and flexural strength were improved
tion Engineering, Univ. of Central Florida, 12800 Pegasus Dr., Suite 211, by adding GO to cement paste, mortar, and concrete mixtures. For
Orlando, FL 32816. Email: byoungcho@ucf.edu the cement paste and mortar, 0.02%–0.08% of GO by weight of
2
Graduate Research Assistant, Dept. of Civil, Environmental and cement increased the compressive strength by 29%–46% and flexu-
Construction Engineering, Univ. of Central Florida, 12800 Pegasus Dr., ral strength by 26%–61%. For the concrete mixture, around 10% of
Suite 211, Orlando, FL 32816. Email: mkhawaji@knights.ucf.edu
3 improvement for both compressive and flexural strengths were ob-
Associate Professor, Dept. of Civil, Environmental and Construction
Engineering, Univ. of Central Florida, 12800 Pegasus Dr., Suite 211, served by mixing 0.1% of GO. The most dominant cause of this
Orlando, FL 32816. Email: boohyun.nam@ucf.edu improvement is considered to be nucleation effects by the reactive
4
Assistant Professor, Dept. of Civil Engineering, King Saud Univ., oxygen groups and the reinforcing (bridging) effect of GO (Al-
P.O. Box 800, Riyadh 11421, Saudi Arabia. Email: yrharbi@knights Muhit et al. 2015; Gong et al. 2014). One recent study presented
.ucf.edu effects from 0.02%, 0.04%, and 0.08% of GO in cement paste
5
Assistant Professor, Dept. of Engineering, Univ. of Mount Union, mixtures and postulated that the reinforcing effect of GO is not
1972 Clark Ave., Alliance, OH 44601 (corresponding author). Email: substantial (Ghazizadeh et al. 2018). Nonetheless, the reinforcing
jinwooan@knights.ucf.edu
effect is still commonly understood as one of the main benefits of
Note. This manuscript was submitted on October 10, 2018; approved
on May 29, 2019; published online on August 28, 2019. Discussion per- GO in cement mixtures.
iod open until January 28, 2020; separate discussions must be submitted Edge-oxidized graphene oxide (EOGO) used in this study is a
for individual papers. This paper is part of the Journal of Materials in new low-cost carbon nanomaterial produced with ball-milling pro-
Civil Engineering, © ASCE, ISSN 0899-1561. cess technology (Garmor 2015). EOGO has a flake shape composed

© ASCE 04019273-1 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(11): 04019273


of several layers of carbon graphene sheets, with the reactive oxygen in addition to the cement mortar mixture to determine the optimum
groups attached along the periphery of the flakes. The amount of percentage of EOGO producing the best performance for the three
reactive oxygen groups in the EOGO is normally less than that of tests. Fatigue life of the designed EOGO cement mortar mixtures
the conventional GO sheets produced by chemical processing. How- was evaluated under different stress levels. Moreover, the flexural
ever, the direct milling process offers the capacity to dramatically damage process of EOGO cement mortar under repeated loading
reduce the cost to manufacture EOGO by eliminating hazardous- cycles is suggested based on incremental characteristics of flexural
waste disposal (Blair et al. 2014). Therefore, EOGO can be an alter- strain. The relationship between flexural fatigue strain and loading
nate additive for cementitious composites with positive effects on cycles is reported, and the flexural fatigue strain at failure of the
performance as well as important economic advantages for high- specimens is also discussed.
volume construction use.
In recent years, several researches have exhibited the effects of
EOGO on the compressive and flexural performance improvement Experimental Program
for both cement paste and mortar mixtures, utilizing petrographic
analyses to identify microstructure and chemical compositions of
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Materials
the resulting cement composites (Alharbi et al. 2018; An et al.
2018a, b).
Cement-based and concrete-based structures including bridges, Edge-Oxidized Graphene Oxide
pavements, and buildings, among others, are designed to withstand Whereas conventional GOs are manufactured through a chemical
repeated stresses of various loads throughout their expected service process known as the Hummers method, involving strong oxidizing
life. Fatigue is caused by cumulative damage resulting from re- agents and acids such as KMnO4 , H2 SO4 , and H2 O2 (Hummers and
peated loads stressing the structural material, which over time leads Offeman 1958), EOGOs are produced by a ball-milling process of
to cracks or fractures. Structural fatigue is a reduction in structural graphite powder with an oxidizing agent under optimized shear and
capacity and an overall degradation of the durability and longevity minimized collision forces. The ball-milling process produces gra-
(Soroushian and Elzafraney 2004; Zhang 1998). A previous study phene oxide nanoflakes, which have functionalized oxygen groups
investigated the benefits to counteracting flexural fatigue produced along the edges of the graphene nanoflake layers (Garmor 2015).
by concrete reinforced with CF (Deng 2005). Additional studies This EOGO production process not only minimizes waste-disposal
have shown that CNT and CF produce high tensile ductility in ce- costs but also dramatically reduces the unit price to less than 1/100
mentitious materials, resulting in overall structural improvement compared with conventional GO sheets produced by the Hummers
(Stynoski et al. 2015). In particular, tensile ductility is dominated method.
by crack opening and spacing, which depends on the level of stress Table 1 presents the chemical composition and physical proper-
transfer between the fibers (herein, carbon-based nanomaterial) ties of the EOGO used in this study (Garmor 2015). EOGO con-
and cement matrix (Lu et al. 2016). Consequently, EOGO can be tains oxygen ranging from 5% to 10%, which is a relatively small
expected to have similar beneficial effects on the fatigue perfor- amount of the oxygen content compared with conventional GO
mance of cementitious composites, although this has yet to be fully (40%–50%) manufactured through a chemical process (Chuah
understood. et al. 2014; Nováček et al. 2017). EOGO has a thin flake form with
In this study, the compressive strength, flexural strength, and an average particle size of 500 nm in diameter and less than 10
flexural fatigue performance of cement mortar containing EOGO layers of single graphene sheets. A single graphene sheet is around
were experimentally investigated. Different amounts of EOGO 0.7–1.0 nm (Müller et al. 2010). Scanning electronic microscopy
ranging from 0.01% to 0.1% (by weight of cement) were designed (SEM) and transmission electron microscopy (TEM) images of
EOGO are illustrated in Fig. 1 (Garmor 2015). The TEM image
by scale of 40 nm clearly shows the presence of multilayer struc-
Table 1. Chemical composition and physical properties of EOGO tures with overlapping areas of EOGO.
Property Value Cement Mortar
Carbon (%) 90–95 Conventional cement mortar was used in this study for preparing
Oxygen (%) 5–10 specimens, which is composed of Type I ordinary portland cement
Nominal particle size (nm) 500 (OPC) and standard sand as a fine aggregate, satisfying the re-
Surface area (m2 =g) 200–300 quirements of ASTM C33 (ASTM 2018a) and ASTM C150
Density (g=cm3 ) ∼1.0
(ASTM 2018b). The chemical composition of OPC used in this
Thickness (layers, nm) ∼10
study is listed in Table 2. The gradation curve of fine aggregate

Fig. 1. Microscopic images of EOGO: (a) SEM; and (b) TEM.

© ASCE 04019273-2 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(11): 04019273


Table 2. Chemical composition of OPC from a single batch of the mortar at one time to maximize uniformity
Component Amount (%) of the mixtures. The mechanical testing was performed on separate
samples 7 and 28 days after initial casting. All cast specimens were
CaO 64.90
stored under normal laboratory temperature and humidity condi-
SiO2 21.49
Al2 O3 4.21
tions for 1 day. After that, the samples were demolded and cured in
Fe2 O3 3.50 a water bath (relative humidity of 100% and 23°C temperature) for
SO3 0.70 5 and 26 days. All specimens were then taken out from the water bath
IR 1.10 and dried in the normal laboratory environmental condition for 1
LOI — additional day. In this way, the 7- and 28-day cured specimens were
Note: LOI = loss on ignition.
prepared for the compressive and flexural strength tests, and the
flexural fatigue test was conducted on the 28-day cured samples.

100
Test Method
Percent passing by mass (%)

Gradation of sand
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80 Upper gradation limit


Lower gradation limit Compressive Strength Test
60 Compressive strength tests were carried out on the cube specimens
cured for both 7 and 28 days in accordance with ASTM C109
40
(ASTM 2016a). A static hydraulic loading system with the loading
20 capacity of 1,000 kN was used for this test. A cross-sectional area
was measured for each specimen, and testing was conducted at the
0 loading rate of 900 N=s. The loading history was recorded until the
0.01 0.1 1 10
specimens failed, and the compressive strength was calculated by
Sieve sizes (mm)
dividing the maximum load by the measured cross-sectional area.
Fig. 2. Gradation curve of fine aggregate and ASTM C33
Flexural Strength Test
requirements.
A three-point bending test was performed on the prismatic cement
mortar specimens with a loading span of 300 mm. A servocontrolled
hydraulic actuator with maximum loading capacity of 100 kN was
Table 3. Mix proportion and IDs used. The static flexural strength test, in accordance with ASTM
Cement Water to Fine aggregate EOGO C293 (ASTM 2016b), was conducted on each of the three prismatic
Mix ID (kg=m3 ) cement ratio (kg=m3 ) (kg=m3 ) samples cured for 7 and 28 days. The tests were carried out by dis-
placement control at a rate of 0.005 mm=min. The load and dis-
CTRL 580 0.5 1,450 —
placement values were recorded automatically at a sampling rate
EOGO 0.01 580 0.5 1,450 0.058
EOGO 0.05 580 0.5 1,450 0.290
of 10 Hz. Here, displacement refers to the relative deflection be-
EOGO 0.1 580 0.5 1,450 0.580 tween the average of the two supports and the center of the beam
specimen, measured by LVDT. The dimensions of the fractured sur-
face were measured in order to calculate the flexural strength
(modulus of rupture, f r ) after testing. The collected load and dis-
is illustrated in Fig. 2 along with the upper and lower limits required placement data were converted to flexural stress (σ) and strain (ε)
by ASTM C33. using the following Eqs. (1) and (2), respectively:
σ ¼ 3PL=2bd2 ð1Þ
Mix Design and Specimen Preparation
The mix proportions of EOGO-mixed cement mortar are summa- where σ = flexural stress (MPa); P = applied load (N); L = span
rized in Table 3. The ratio of cement to fine aggregate was 1:2.5, length (mm); b = average width of specimen at the fracture
and the water to cement (w/c) ratio was 0.5 for all cases. A different (mm); and d = average depth of specimen at the fracture (mm), and
percentage of EOGO as dry powder was used with 0% (control), ε ¼ 6dδ=L2 ð2Þ
0.01%, 0.05%, and 0.1% by weight of cement for the mixture
specimens. The EOGO powder was mixed in a dry condition. where ε = flexural strain; d = average depth of specimen at the frac-
A shear mixer was used for the uniform distribution. This is ac- ture (mm); δ = deflection at center of beam (mm); and L = span
cording to a previous study that dry- and wet-mixing methods of length (mm).
EOGO exhibit minor differences regarding mechanical properties
(e.g., compressive and flexural strength) for identifying the carbon Flexural Fatigue Test
component of EOGO in the cement composite analyzed by SEM Flexural fatigue tests were conducted on the beam specimens cured
and energy dispersive spectroscopy (EDS) (Alharbi et al. 2018). for 28 days to evaluate the influence of EOGO on the long-term
The control mix design with no EOGO (0%) is denoted as CTRL, performance of cement mortars under a repetitive bending load
and other EOGO mixtures are referred as EOGO 0.01, EOGO 0.05, environment. As shown in Fig. 3, the simple-supported prismatic
and EOGO 0.1 based on different portions of EOGO (Table 3). specimens were subjected to a sinusoidal cyclic loading in the three-
Specimens were prepared for mechanical testing such as com- point bending mode with the constant frequency (f) of 10 Hz.
pressive strength, flexural strength, and flexural fatigue performance Specific stress levels (Smax ) were computed for each mixture
tests. Cube specimens with dimension of 50 × 50 × 50 mm were Smax ¼ σmax =f r ð3Þ
selected for the compressive strength test, and beam samples were
designed for the flexural strength and fatigue tests with dimensions where fr = measured static flexural strength; and σmax = desired
of 65 × 65 × 350 mm. The test specimens of each mix ID were cast maximum fatigue stress.

© ASCE 04019273-3 J. Mater. Civ. Eng.

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Stress
Sinusoidal loading at 10 Hz

fmax
f amp
f mid

f min
Loading cycle Time
Cyclic Loading Cyclic Loading
Initial delay

65mm
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300mm 65mm

25mm 25mm

Fig. 3. Sinusoidal loading configuration and specimen dimension for flexural fatigue test.

The testing was started by 0.8 of the stress level and carried out 50
within ranging from 0.6 to 0.95. The minimum loading ratio, de-
Compressive strength (Mpa)
7day 28day
fined by Smin ¼ σmin =fr, was set as 0.1 through the fatigue testing
program. The required fatigue stresses, σmax and σmin , were con- 40
verted into the corresponding loads based on the cross-sectional
dimensions of the specimens, and the converted load was entered
to the control software of the testing machine as input values. A 30
history of actual applied loads and displacements at the center of
the beam specimen was recorded at a sampling rate of 80 Hz until
the testing specimen broke. The number of loading cycles to fail- 20
ure, defined as N, was recorded for each specimen. The flexural CTRL EOGO 0.01 EOGO 0.05 EOGO 0.1
fatigue stresses and strains of the specimens were computed from (a) Mix ID
the collected load and displacement data by considering the dimen-
10
sion of fractured cross-sectional area.
7day 28day
Flexural strength (Mpa)

Results and Discussion 8

Static Compressive and Flexural Strength Tests 6


Figs. 4(a and b) show the average compressive strength (fc ) and
flexural strength (fr ), respectively, for the cement mortar specimens
cured for 7 and 28 days. Compared with the control mixture, the 4
EOGO 0.05 exhibits an increase of compressive strength of about CTRL EOGO 0.01 EOGO 0.05 EOGO 0.1
22% and 23% for the curing ages of 7 and 28 days, respectively. The (b) Mix ID
flexural strengths of EOGO 0.05 increased by 24% and 23% for
Fig. 4. Results of mechanical strength test for EOGO cement mortar:
7 and 28 days of curing, respectively, compared to the control. It is
(a) compressive strength for 7 and 28 days; and (b) flexural strength for
shown that EOGO contributes beneficial effects to the compressive
7 and 28 days.
and flexural strength with the maximum value at 0.05%. Thereafter,
the strengths at 0.1% show a slight reduction but are still higher
values than the control specimens. Thus, it is presumed that there
is an optimum ratio exhibiting the best performance, which is con- strength gain by EOGO is not as high as the conventional GO for
sidered to be 0.05% in this study. the cement mortar. Three possible reasons are presented. First, the
The test results indicate that EOGO produces less improvement amount of oxygen functional groups in EOGO (5%–10%) is less
in strength compared with the conventional GO nanosheet pro- than that in the conventional GO (40%–50%). The amount of
duced by chemical processing (e.g., Hummers method). Previous oxygen functional groups enhances performance of cementitious
studies on GO-cement mortar have reported an increase of com- composites (Lv et al. 2014). Therefore, the different amount of
pressive strength up to 40%, and flexural strength is enhanced up the functionalized oxygen groups between EOGO and GO would
to 60% (Li et al. 2015; Lv et al. 2013; Wang et al. 2015). The likely be a main cause of the strength difference.

© ASCE 04019273-4 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(11): 04019273


Second, the particle shapes of EOGO and GO are different, Fig. 5 illustrates the S-N relationship for EOGO-cement mortar
showing different aspect ratios (ratio of length to thickness). EOGO specimens. For all mixtures, N increases as Smax decreases, which
shows a flake form consisting of several layers, which has a lower exhibits a negative linear relationship and is normally observed in
aspect ratio. On the other hand, conventional GO nanosheets have the fatigue behavior of cementitious materials. It can also be seen
thin plate shape with a single layer, which leads to a higher aspect that 0.05% of EOGO provides the most pronounced effect on the
ratio. The increased aspect ratios are beneficial for improving flexural fatigue life, showing the best fatigue performance among
mechanical properties by providing strong interaction between the specimens. Meanwhile, 0.01% and 0.1% of EOGO show
cracks and GO sheets in the cementitious composites (Pan et al. slightly improved performance in fatigue life compared to the con-
2015). Lastly, the size of GO particle is smaller than a single trol mixture. It is interesting that these results are consistent with
EOGO; thus, for a given weight, the number of GO nanosheet the static compressive and flexural strengths shown in Fig. 4, sup-
particles is greater than that of EOGO. It is reported that a smaller porting the conclusion that 0.05% EOGO is the optimum for both
size of nanomaterial is more effective in reducing the amount of strength and fatigue performance. It is known that internal micro-
fine pores, leading to the reduction of the capillary stresses and cracks in the cementitious composites grow to macrocracks as the
densifying microstructures in the cementitious composites (Konsta- number of loading repetitions increases, which results in larger con-
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Gdoutos et al. 2010). centration of stress in those cracks and failure as well (Lee and Barr
2004). It is apparent that EOGO helps to prevent or delay crack
growth in nanoscales or microscales.
Flexural Fatigue Test
Cycle-Strain Behavior
S-N Relationships The changes in flexural strain at the bottom of EOGO mortar spec-
The results of flexural fatigue test [i.e., relationship between stress imens were investigated. The history of flexural strain was recorded
level (Smax ) and number of loading cycles to failure (N), referred to as the number of load repetition increases. Fig. 6 illustrates a typical
as S-N relationship] for all EOGO mortar prismatic specimens are strain history when the prismatic specimen is exposed to sinusoidal
summarized in Table 4. Although seven samples for each mix de- loading for flexural fatigue testing. In this graph, the strain values
sign were prepared and tested, some of them were broken at the first corresponding to maximum stress level (Smax ) and minimum stress
level (Smin ) are defined as total strain (εt ) and plastic strain (εp ),
loading step by accident. Accordingly, five samples were recorded
respectively. The plastic strain at the first loading cycle was set
successfully for the cases of EOGO 0.01, EOGO 0.05, and EOGO
to zero; thus, the plastic strain represents a permanent deformation
0.1. Thus, a limited number of samples were tested, focusing on the
by the repetitive loading. Furthermore, the values of the maximum
effect of EOGO on the cyclic flexural behavior of cement mortar.
total strain and plastic strain at the failure moment, i.e., at the last
Therefore, a complete study on the development of the S-N model,
cycle of the repetitive loading, were separately recorded.
including reliability analyses, was not considered in this study.
A stress ratio from 0.75 to 0.9, which successfully provides all
the fatigue life testing results for the four mixtures, was used in this
analysis. Table 5 presents the recorded data corresponding to the
Table 4. Flexural fatigue testing results of number of cycles to failure (N) selected parameters including number of cycles to failure (N),
Stress level, maximum total strain at failure (εt·f ), and maximum plastic strain
Smax CTRL EOGO 0.01 EOGO 0.05 EOGO 0.1 at failure (εp·f ).
Fig. 7 shows the history of the plastic fatigue strain at the mini-
0.95 — 20 16 —
mum stress level (Smin ) as the number of loading cycles increases.
0.90 6 34 41 124
0.85 271 148 16,929 345 The number of load repetitions (n) is normalized by the number of
0.80 9,249 2,613 64,074 1,785 loading to failure, n=N, referred to as the cycle ratio. Variation of
0.75 46,325 79,405 1,085,304 15,960 the plastic strain through the entire loading repetition shows a dis-
0.70 1,898 — — 251,623 tinct three phases for all cases. In Phase 1, the plastic deformation
0.65 819,891 — — — increases rapidly in the early phase of the load repetition and is
0.60 203,556 — — — commonly known to be the result of the creep effect of the speci-
men. In Phase 2, the plastic strain is increased continuously accord-
ing to combined effects of periodic creep and fatigue cracks in the
specimen, but the rate is very low. Finally, in Phase 3, the plastic
1.0
deformation increases rapidly again by expanding and connecting
the fatigue cracks. These three phases are known as the cyclic creep
0.9 phase, creep-to-fatigue coupling phase, and fatigue phase, respec-
Stress level (S max )

R² = 0.93
tively (Gao and Hsu 1998; Mun et al. 2016; Xiao et al. 2013). The
0.8 amounts and rates of the strain increment of EOGO mixed cement
R² = 0.89
mortars in Phase 1 are mostly larger and faster than specimens of
0.7
CTRL EOGO 0.01
the control mixture, respectively, except for the case of Smax ¼ 0.9.
R² = 0.94
EOGO 0.05 EOGO 0.1 R² = 0.84 It is also shown that the EOGO mixed cement mortar yielded
0.6 CTRL EOGO 0.01
faster incremental rates of plastic strain than the control mixture in
EOGO 0.05 EOGO 0.1
Phase 2. In addition, the length of Phase 1 was computed for CTRL
0.5 and EOGO 0.05 cases. The transition between Phases 1 and 2 was
0 1 2 3 4 5 6 graphically determined by drawing tangential lines first on Phase 1
Number of cycles to failure (log N) and Phase 2, and then the cross point is set to the transition point.
In this way, the lengths of Phase 1 by cycle ratio were determined,
Fig. 5. S-N relationship for the EOGO cement mortars in flexural
and the results show that EOGO allow for a longer length of
behavior.
Phase 1 than the control sample. These phenomena become more

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J. Mater. Civ. Eng., 2019, 31(11): 04019273


2.5

: Plastic strain at n th cycle of loading


2.0 : Total strain at n th cycle of loading
: Maximum plastic strain at failure

Flexural strain ( ) [10-3 ]


: Maximum total strain at failure
1.5

1.0

0.5

0.0
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0 2 4 … 40000 40002 40004 40006 … 79400 79402 79404 79406


Number of cycles (n)

Fig. 6. Typical cycle-strain history for flexural fatigue test.

Table 5. Summary of flexural fatigue test results for EOGO cement mortar beams
Stress level, Smax
Item Specimen ID 0.90 0.85 0.80 0.75
Number of cycles to failure, N CTRL 6 271 9,249 46,325
EOGO 0.01 34 148 2,613 79,405
EOGO 0.05 41 16,929 64,074 1,085,304
EOGO 0.1 124 345 1,785 15,960
Maximum total strain at failure, εt·f (×10−3 ) CTRL 1.16 1.18 1.21 1.35
EOGO 0.01 1.27 1.30 1.47 1.76
EOGO 0.05 1.41 1.43 1.72 1.96
EOGO 0.1 1.40 1.34 1.60 1.57
Maximum plastic strain at failure, εp·f (×10−3 ) CTRL 0.46 0.56 0.49 0.56
EOGO 0.01 0.41 0.52 0.62 1.00
EOGO 0.05 0.49 0.60 0.81 1.19
EOGO 0.1 0.48 0.56 0.87 0.77

1.5 1.5
CTRL EOGO 0.01 CTRL EOGO 0.01
Flexural strain [10 -3]

Flexural strain [10 -3]

EOGO 0.05 EOGO 0.1 EOGO 0.05 EOGO 0.1


1.0 1.0

0.5 0.5

0.0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
(a) Cycle ratio (b) Cycle ratio
1.5 1.5
CTRL EOGO 0.01 CTRL EOGO 0.01
Flexural strain [10 -3]

Flexural strain [10 -3]

EOGO 0.05 EOGO 0.1 EOGO 0.05 EOGO 0.1


1.0 1.0

0.5 0.5

0.0 0.0
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
(c) Cycle ratio (d) Cycle ratio

Fig. 7. History of plastic flexural strains by cycle ratio for four different stress levels (Smax ): (a) 0.90; (b) 0.85; (c) 0.80; and (d) 0.75.

© ASCE 04019273-6 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(11): 04019273


2.0 2.0
CTRL EOGO 0.01 CTRL EOGO 0.01

Flexural strain [10-3]


Flexural strain [10-3]
EOGO 0.05 EOGO 0.1 EOGO 0.05 EOGO 0.1
1.5 1.5

1.0 1.0

0.5 0.5
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
(a) Cycle ratio (b) Cycle ratio
2.0 2.0
CTRL EOGO 0.01 CTRL EOGO 0.01
Flexural strain [10-3]

Flexural strain [10-3]


EOGO 0.05 EOGO 0.1 EOGO 0.05 EOGO 0.1
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1.5 1.5

1.0 1.0

0.5 0.5
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
(c) Cycle ratio (d) Cycle ratio

Fig. 8. History of total flexural strains by cycle ratio for four different stress levels (Smax ): (a) 0.90; (b) 0.85; (c) 0.80; and (d) 0.75.

noticeable as the stress ratio decreases [apparent in Fig. 7(d)]. On 1.5


CTRL EOGO 0.01
Max. plastic strain at failure [10-3]
the other hand, in Phase 3, it is shown that the strain increment rate
EOGO 0.05 EOGO 0.1
of the EOGO mixtures is smaller than that of the control specimens. CTRL EOGO 0.01
Fig. 8 presents the history of total strain corresponding to the EOGO 0.05 EOGO 0.1
1.0
maximum stress level (Smax ), which includes the stress levels of
0.9, 0.85, 0.8, and 0.75. The general trend of total strain history
is similar to that of plastic strain. The EOGO mixed specimens pro-
duce faster and larger initial strain increments in the early stage of 0.5
cyclic loading, regardless of the stress level. The lengths of Phase 1
were quantified by the same way as plastic strain, and the results
indicate that EOGO seems to allow for almost a twice as long 0.0
length of Phase 1 than the control, like in the case of plastic strain. 0 1 2 3 4 5 6 7
In the second phase, the EOGO mixed specimens show higher (a) Number of cycles to failure (log N)
incremental rates of total flexural fatigue strain than the control
2.5
samples, particularly when the stress level is small [Fig. 8(d)]. In CTRL EOGO 0.01
Max. total strain at failure [10-3]

the last phase, however, the incremental rate of total strain for the EOGO 0.05 EOGO 0.1
control specimens is steeper than that of EOGO mixed specimens, CTRL EOGO 0.01
similar to the results of plastic strain. The results show that the 2.0 EOGO 0.05 EOGO 0.1

EOGO cement mortars yield larger permanent flexural deformation


and maximum deflection at the failure of fatigue than the control
mixture. Particularly, the cement mortar mixture with 0.05% of 1.5
EOGO gives the greatest values in both the plastic and total strains.
It could be understood that the EOGO flakes play a role in prevent-
ing and delaying the growth and propagation of fatigue cracks from
nanoscales to microscales. This conclusion is supported by Deng 1.0
0 1 2 3 4 5 6 7
(2005), who presented the beneficial effects of the carbon nano- (b) Number of cycles to failure (log N)
materials on the improvement of mechanical behavior of cement
composites. Fig. 9. Cycles’ maximum strain relationship at failure of the EOGO
Figs. 9(a and b) present the relationships between N and εp·f cement mortar beams: (a) maximum plastic flexural fatigue strain at
and N and εt·f , respectively. The logarithmic regression lines for the failure (εp·f ); and (b) maximum total flexural fatigue strain at failure
four mix designs indicate that the maximum plastic strain and (εt·f ).
maximum total strain at failure increase with increasing the number
of cycles to specimen failure. Interestingly, the strain increment
rates of EOGO mixed cement mortars show a steeper increase than
the control mixture as the number of load repetitions increases. cement composites more ductile in the flexural fatigue bending. In
On the other hand, it is hard to find a distinguishable relationship other words, EOGO can help to improve the transfer level of tensile
between the maximum plastic and total strains at failure and the stress by bridging nanoeffects in the cementitious composites, re-
EOGO content. It is likely that the addition of EOGO makes the sulting in enhancement of the flexural ductility.

© ASCE 04019273-7 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(11): 04019273


Conclusions composite.” In Proc., Transportation Research Board 94th Annual
Meeting. Washington, DC: Transportation Research Board.
In this study, the effects of EOGO on cement mortar were exper- An, J., B. H. Cho, Y. Alharbi, M. Khawaji, M. McInnis, and B. H. Nam.
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An, J., M. McInnis, W. Chung, and B. Nam. 2018b. “Feasibility of using
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plastic and total strains during the fatigue life were discussed in ASTM. 2016a. Standard test method for compressive strength of hydraulic
terms of internal damage process and structural performance. The cement mortars. ASTM C109. West Conshohocken, PA: ASTM.
following conclusions can be drawn from this study: ASTM. 2016b. Standard test method for flexural strength of concrete
• EOGO can be used as an alternative additive. A small dosage of (using simple beam with center-point loading). ASTM C293. West
EOGO has beneficial effects on mechanical properties of a ce- Conshohocken, PA: ASTM.
ment mortar mixture. EOGO has economical competitiveness, ASTM. 2018a. Standard specification for concrete aggregates. ASTM C33.
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although the extent of effects is relatively lower than conven- West Conshohocken, PA: ASTM.
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• The optimum content of EOGO is 0.05% by weight of cement in West Conshohocken, PA: ASTM.
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syntheses of edge functionalized graphene materials and biomass-
7 and 28 days, respectively, and the flexural strength up to 24% derived chemicals.” Faraday Discuss. 170: 223–233. https://doi.org/10
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