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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.
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
100
Test Method
Percent passing by mass (%)
Gradation of sand
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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)
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
1.0
0.5
0.0
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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]
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]
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.
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]
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.
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
although the extent of effects is relatively lower than conven- West Conshohocken, PA: ASTM.
tional GO. ASTM. 2018b. Standard specification for portland cement. ASTM C150.
• The optimum content of EOGO is 0.05% by weight of cement in West Conshohocken, PA: ASTM.
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