i An update to this article is included at the end

Cement and Concrete Composites 130 (2022) 104508

Contents lists available at ScienceDirect

Cement and Concrete Composites

journal homepage: www.elsevier.com/locate/cemconcomp

Studies on mechanical properties and durability of steel fiber reinforced

concrete incorporating graphene oxide
Changjiang Liu a, 1, 2, *, Xiaochuan Hunag b, 1, 2, **, Yu-You Wu c, 1, 2, ***, Xiaowei Deng d, ****,
Zhoulian Zheng e, *****, Bo Yang e, ******
a
School of Civil Engineering, Guangzhou University, Guangzhou, 510006, China
b
College of Environment and Civil Engineering, Chengdu University of Technology, Chengdu, 610059, China
c
School of Transportation, Civil Engineering and Architecture, Foshan University, Foshan, Guangdong, 528000, China
d
Department of Civil Engineering, The University of Hong Kong, Pokfulam, 999077, Hong Kong, China
e
School of Civil Engineering, Chongqing University, Chongqing, 400045, China

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

Keywords: Steel fiber reinforced concrete (SFRC) is a kind of modified concrete that has attracted much attention at present.
Graphene oxide Compared with ordinary concrete, SFRC has superior physical and mechanical properties, so it is widely used in
Steel fiber railway sleeper prefabricated, highway pavement, and tunnel lining. However, the compressive strength,
Steel fiber reinforced concrete
impermeability, and frost resistance of SFRC are not prominent compared with ordinary concrete. To optimize
Mechanical properties
Durability
the performance of SFRC, different amounts of graphene oxide (GO) were added in this study. The results showed
that the excellent properties of GO have a significant improvement effect on the mechanical and durability of
SFRC. Among them, the compressive strength, flexural strength, and splitting tensile strength of the specimens
were increased by 20.1%, 29.5%, and 26.2% compared with the reference group after 28 days of curing. At the
same time, the penetration depth of chloride ion is reduced by 56.8% at most compared with the benchmark after
adding GO, the mass loss and relative dynamic modulus loss were 4.5% and 32.6% after 100 freeze-thaw cycles
respectively, which were much lower than those of the reference group. To explain this phenomenon, different
microstructure characterization techniques including XRD, MIP, and SEM were used to study the composition,
pore size distribution, and microstructure of concrete. The results showed that the main role of GO is to promote
the early hydration reaction, repair the micro defects of the matrix, improve the density of the matrix and
strengthen the bonding between steel fiber and the matrix. In this work, the strengthening mechanism of GO on
the SFRC matrix has been discussed in detail.

1. Introduction performance is also greatly concerned when exposed to aggressive en­

Concrete is a kind of heterogeneous composite material cemented by
cementitious materials and aggregates. It is widely used in civil engi­
neering due to its relatively low price and high compressive strength.
However, its toughness and tensile strength are low, and its durability
vironments, which may be associated with its micro-cracks and pores
within the matrix bulks, distribution of chaotic hydration products, and
insufficient density within interfacial zone [1–3]. Existing solutions
mainly consist of adding cementitious supplementary materials (e.g. fly
ash [4], slag powder [5], and silica fume [6]), reducing the ratio of

* Corresponding author.
** Corresponding author.
*** Corresponding author.
**** Corresponding author.
***** Corresponding author.
****** Corresponding author.
E-mail addresses: cjliu@gzhu.edu.cn (C. Liu), hxc313440155@163.com (X. Hunag), yuyou.wu@yahoo.com (Y.-Y. Wu), xwdeng@hku.hk (X. Deng), zhengzl@cqu.
edu.cn (Z. Zheng), yang0206@cqu.edu.cn (B. Yang).
1
Contributed equally to this work.
2
Co-first authors.

https://doi.org/10.1016/j.cemconcomp.2022.104508
Received 18 July 2021; Received in revised form 13 March 2022; Accepted 24 March 2022
Available online 26 March 2022
0958-9465/© 2022 Elsevier Ltd. All rights reserved.
C. Liu et al. Cement and Concrete Composites 130 (2022) 104508

Table 1 Table 2
Chemical composition and physical properties of cementitious materials. Performance parameters of steel fiber.
Materials OPC FA Model Length Diameter Shape Tensile Bending
strength performance
SiO2 (mass%) 20.08 52.5
Al2O3 (mass%) 5.09 15.1 TB-32 32 mm 1.2 mm Straight 732 MPa 100% without
Fe2O3 (mass%) 3.81 7.1 waveform fracture
CaO (mass%) 63.41 8.62
MgO (mass%) 2.06 1.2
SO3 (mass%) 2.33 0.7 experimental techniques, including scanning electron microscopy
K2O(mass%) – 1.3 (SEM), mercury intrusion porosimetry (MIP), and X-ray diffractometry
Na2O(mass%) 0.55 0.5
TiO2(mass%) – 1.0
(XRD).
P2O5(mass%) – –
Cl(mass%) 0.016 0.12 2. Materials and test methods
NiO(mass%) – –
Loss on ignition(g) 5.0 4.6
2.1. Materials
BET surface area(m2/kg) 346 1000
Specific gravity(g/cm3) 3.12 2.3
Setting time(min) Initial 96 – P⋅O.42.5 R cement complying with GB/T175-2007 and class F fly ash
Final 258 － (FA) was used as binder materials for all mixes of the concrete. Their
chemical compositions and properties are listed in Table 1. Fine aggre­
gate (FIA) was manufactured sand a fineness modulus of 2.67. And
water-binder, adding concrete admixtures, such as early strength agents
coarse aggregate (CA) was crushed limestone with a size range of 5–10
[7,8]and adding micro steel fibers to concrete, which is also named steel
mm and10-20mm. A polycarboxylate superplasticizer used in the test
fiber reinforced concrete (SFRC) [9–11]. Among these methods, the
was Sika 540P. Straight steel fiber with a 32 mm length and 1.2 mm
latter one is considered to be most effective in improving tensile
diameter and tensile strength of 732 MPa was produced by Taian Peer
strength, fracture toughness, and fatigue resistance of concrete.
Fiber Co., Ltd and its details are shown in Table 2 and Fig. 1. GO pro­
Studies such as Mansour Ghalehnovi et al. [9] showed that the
vided by Shenzhen Matterene Tech. Co. Ltd. The main parameters of the
lap-spliced length of steel fiber reinforced concrete beams can be
GO nanosheet are shown in Table 3 and Fig. 2.
reduced by at least 20% with the addition of 2% steel fiber, and the
Fig. 2 is the microscopic characterization results of GO. Fig.2 (a) and
ductility and bearing capacity are not affected. Rahmat Madandoust
Fig.2 (b) were used to characterize the structure, size, and thickness of
et al. [10] assessed the effect of steel and polypropylene fibers at various
GO sheets by SEM and AFM morphology. The results showed that GO
volume contents on concrete incorporating lightweight expanded clay
sheets had superb diameter distribution (0.5 ~ 3um) and the monolayer
aggregate. The results showed that when the steel fiber content is 1%
rate (91%). Fig. 2 (c) is the XRD diffraction pattern of GO, and it is found
and 3%, the compressive strength and splitting tensile strength of
that GO only has a diffraction peak at the diffraction angle of 2θ = 10.9◦ ,
lightweight concrete is the best. Liao et al. [11] studied the effect of steel
indicating that GO has a high oxidation degree and purity. Raman
fiber with different content and aspect ratio on the mechanical proper­
spectra in Fig. 2 (d) also confirmed that GO showed G peak (1580 cm− 1)
ties of concrete. The test results showed that with the increase of steel
and D peak (1350 cm− 1). The G peak corresponds to the in-plane
fiber content, the dynamic increase factor (DIF) of SFRC gradually de­
stretching vibration of sp2 hybrid C atom, while the D peak corre­
creases. In addition, under the same steel fiber content, SFRC with the
sponds to the structural defect. The D peak intensity of GO is very high
steel fiber length-diameter ratio of 50 exhibits maximum compressive
and the G peak is very wide, indicating that the original structure of
strength at different strain rates.
graphite has been greatly damaged due to the introduction of oxidation
It should be pointed out that these methods cannot improve the
functional groups, so GO has more active properties.
microstructure properties of cement matrix through nanoscale. As a
consequence, the inherent defects of cement-based composites remain
an issue. 2.2. Mix proportions and specimen preparation
Advancement in nanotechnology can offer opportunities to enhance
the properties and performance of cement-based composites by incor­ Five concrete mixes, designated as SFRC, GOSFRC-1, GOSFRC-3,
porating nanomaterials [12–18]. Previous work has confirmed that GO GOSFRC-5, and GOSFRC-7, were prepared containing 0.00 wt%, 0.01 wt
plays a significant role in improving the microstructure of cement-based %, 0.03 wt%, 0.05 wt%, and 0.07 wt% of GO by weight of cement,
materials, thus greatly enhancing its mechanical properties and dura­ respectively. Their mix proportions are shown in Table 4.
bility [18–23] as the addition of GO can promote cement hydration,
refines capillary pore structure, reduces pore content, and improves the 2.3. Test methods
density of the cement matrix [18–23].
Although GO has excellent properties, due to the large surface energy 2.3.1. Stirring and curing of SFRC
of GO, it is prone to particle agglomeration in its preparation and use. The mixing process of SFRC is as follows: firstly, the cementitious
Another disadvantage is that the oxygen-containing groups of GO are materials and aggregate were stirred for 2 min. Secondly, the steel fibers
easy to cross-link with Ca2+ in the cement matrix, resulting in granu­ were poured into the mixture and stirred for 2 min. Finally, GO
lation and aggregation, which greatly limits the role of GO. To solve this dispersion and additional water were poured into the mixer for 2 min.
problem, a variety of methods have been proposed to improve GO The specimens (after molding) were cured with mold for 1 day at room
dispersion, including ultrasonic dispersion [24,25] and adding surfac­ temperature of 20 ◦ C, and the plastic film was covered to prevent water
tants [26–34]. Based on the previous studies, a GO dispersion with stable loss. After that, the specimen was moved into the standard curing room
performance was successfully prepared [35] to prepare for subsequent to maintain until the specified age.
experiments.
In this study, the specimen with different GO content in terms of their 2.3.2. Workability test
workability, mechanical properties, durability, change of pore structure, The workability of SFRC was referred to the “Standard for perfor­
matrix composition, and microstructure have been discussed. Efforts mance test method of ordinary concrete mixture” (GB/T 50080–2002).
have been made to reveal the fundamental mechanisms of GO using The specific operation steps are to take 15 L of the mixed SFRC mixture
and put it into the tube evenly by three layers with a small shovel, so that

2
C. Liu et al.
Fig. 1. (a) Fly ash and (b) Steel fiber.
Table 3
Main properties of GO.
Diameter Odour C/ Solvent Concentration pH Single-
O layer
rate
0.5～3 Odorlessness 1.7 Water 8 mg/mL 4.56 91%
μm
the height of each layer after tamping is about 1/3 of the tube height.
Then the slump value of the SFRC mixture was measured. It should be
noted that the entire test process should be completed within 150 s.
2.3.3. Mechanical properties
The test method of mechanical properties was based on the “Stan­
dard for test methods of concrete physical and mechanical properties”
(GB/T 50081–2019). The mechanical properties of specimens were
tested by the testing machine. The specimen size of the compression test
and splitting tensile test is 100 mm × 100 mm × 100 mm, and the
specimen size of the flexural test is 400 mm × 100 mm × 100 mm.
2.3.4. Accelerated chloride penetration
The test method of chloride ions penetration resistance was based on
the “Standard for test methods of long-term performance and durability
of ordinary concrete” (GB/T 50082–2009). The specimen size of the
chloride ions penetration test is Ф 100 mm × 50 mm. The test uses the
silver nitrate chromogenic method to measure the penetration depth of
free chloride ions in concrete. The principle of the silver nitrate chro­
mogenic method is: in the area where the chloride ions concentration is
higher than a certain value, it is mainly the reaction between the chlo­
ride ions and the silver ion to form a silvery-white silver chloride pre­
cipitation, and the whole area is silvery white. In the region where the
chloride ions concentration is lower than a certain value, mainly hy­
droxide ions react with silver ions to form brown silver oxide pre­
cipitates. The basis for judging the penetration depth of chloride ions is
based on the height of the white area (silver chloride).
2.3.5. Freeze-thaw resistance of concrete
The test method of frost resistance was based on the “Standard for
test methods of long-term performance and durability of ordinary con­
crete” (GB/T 50082–2009). The specimen size of the frost resistance test
is 400 mm × 100 mm × 100 mm.
2.3.6. X-ray powder diffraction (XRD)
The ground powder samples that meet the requirements were loaded
into the groove, and the powder was compacted with clean glass, and
then put into the sample room for testing. The sample was analyzed by
X-ray diffraction, and the composition information of the materials was
obtained.
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Cement and Concrete Composites 130 (2022) 104508
2.3.7. Pore structure characterization
The test method of pore size distribution was based on “Pore size
distribution and porosity of solid materials by mercury porosimetry and
gas adsorption” (GB/T 21650.1–2008). The porosity measurement
principle of mercury intrusion porosimetry (MIP for short): vacuum the
gas in through holes inside the porous material, and then fill the pores
with mercury under the action of external pressure. The amount of
mercury pressed into the material is related to the size and distribution
of the pore size, and the mercury intrusion pressure is related to the size
of the pore size. Qualitatively, the smaller the hole, the higher the
mercury intrusion pressure required, and vice versa. According to the
functional relationship between the applied pressure, the amount of
mercury intrusion, and the pore size, the pore structure of the concrete is
obtained.
2.3.8. Microstructure characterization
Due to the scanning electron microscope (SEM for short) imaging is
obtained by the detector secondary electrons and backscattered electron
signals. If the sample is not conductive or has poor conductivity, it will
eventually affect the transmission of electronic signals, resulting in
image distortion, deformation, sloshing, and other phenomena. In order
to enhance the conductivity of the sample surface, the samples with a
thickness of only 5 mm were prepared, and sprayed with gold.
3. Results and discussion
3.1. Workability
For concrete slurry (Fig. 3 (a)), whether it has excellent fluidity is
very important for pumping and construction. However, past studies
have shown that GO is not conducive to the fluidity of cement-based
materials [36–38]. To eliminate the negative impact of GO on the per­
formance of concrete, the method adopted in this study is to change the
PC content according to the GO content. Through many tests, find the
appropriate PC content for each group of concrete (Table 4), and the
slump of the specimens is shown in Fig. 3 (b).
It is not difficult to find from the figure that by adjusting the PC
content, the slump of each group of specimens is approximately the
same. The reason for controlling the same liquidity is that GO adsorbs
free water in the system, and the higher the GO content is, the more free
water it will adsorb. In this case, the amount of water that can partici­
pate in the reaction is different in different groups of concrete. In
addition, disunity fluidity will result in different compactness of spec­
imen after molding. It will bring additional interference factors to the
test, resulting in unclear conclusions. Therefore, controlling the same
liquidity is necessary to eliminate these interfering factors.
C. Liu et al. Cement and Concrete Composites 130 (2022) 104508

Fig. 2. Physical properties of GO.

Table 4
Mix proportions of concrete.
Number GO Cement (Kg/m3) FA (Kg/m3) Steel fiber (Kg/m3) Water (Kg/m3) Aggregate (Kg/m3) Sand (Kg/m3) W/C PC (Kg/m3)

SFRC-0 0 294.3 73.6 78.5 172.9 1154.3 677.9 0.47 0.77

GOSFRC-1 0.01% 294.3 73.6 78.5 172.9 1154.3 677.9 0.47 0.79
GOSFRC-3 0.03% 294.3 73.6 78.5 172.9 1154.3 677.9 0.47 0.81
GOSFRC-5 0.05% 294.3 73.6 78.5 172.9 1154.3 677.9 0.47 0.83
GOSFRC-7 0.07% 294.3 73.6 78.5 172.9 1154.3 677.9 0.47 0.86

Note: SFRC represents the reference specimen, GOSFRC-1 represents the addition of 0.01 wt % GO on the basis of SFRC. To control the fluidity of each group, the
amount of PC in different groups is different.

3.2. Mechanical properties
As shown in Fig. 4, the mechanical properties of SFRC at various ages
have different degrees of improvement, and within a certain range,
showed a trend of first increased and then decreased after adding GO
[35,39–41]. When the GO content was 0.05 wt%, the compressive
strength of the specimen was the highest, reaching 53.3 MPa after 28
days of curing, which was 20.1% higher than that of the reference
specimen. When the GO content is 0.03 wt%, the flexural strength and
splitting tensile strength of the specimens are improved most signifi­
cantly, reaching 7.6 MPa and 4.63 MPa respectively after 28 days of
curing, which are 29.8% and 26.2% higher than those of the reference

4
C. Liu et al. Cement and Concrete Composites 130 (2022) 104508

Fig. 3. The workability of specimens.

Fig. 4. Mechanical properties of GO modified SFRC.

specimens. When the GO content reaches 0.07 wt%, the strength of the
specimens decreases to a certain extent. The possible reason is that more
water is attached to the large surface area of GO, so there is less free
water in the system, resulting in incomplete hydration of cement [40]. In
addition, when GO content is higher, it tends to agglomerate together,
which is also not conducive to its role [41–43]. However, the test results
still show that an appropriate amount of GO has an excellent
improvement effect on the mechanical properties of SFRC, which is of
great significance for the potential application of concrete structures.
3.3. Resistance to chloride ions penetration
In this study, the resistance of concrete to chloride ions penetration
was determined by measuring the migration coefficient of chloride ions

5
C. Liu et al.
Fig. 5. The chloride ion resistance of GO modified SFRC.
in concrete under unsteady migration. After the average penetration
depth of each group of specimens was measured, the migration coeffi­
cient of chloride ions was calculated according to the specification. It
can be found from Fig. 5 that with the increase of curing time, the
resistance to chloride ions penetration of concrete specimen gradually
improves, and at the same age, different contents of GO also lead to
different resistance to chloride ions penetration of each group of speci­
mens. In contrast, when the dosage of GO was 0.03 wt% and 0.05 wt%,
the penetration depth of chloride ions was shallower and the corre­
sponding chloride migration coefficient was smaller. Among them,
when the GO content was 0.03 wt% after curing for 28 days, the resis­
tance to chloride ions of the SFRC specimens was the best, and the
chloride ions penetration depth was 4.8 mm, which was 53.8% lower
than that of the reference group. When the GO content was 0.05 wt%
after curing for 56 days, the chloride ions resistance of the concrete
specimen was the best, and the chloride ions penetration depth was 3.8
mm, which was 56.8% lower than that of the reference group. This is
because the incorporation of GO improves the pore structure of the
cement matrix. At the same time, under the action of the GO template,
the hydration products tend to be regular and dense, the compactness of
the matrix is improved, and the barrier effect on chloride ions is stron­
ger. However, when the amount of GO is too large (0.07 wt%), the larger
surface energy makes it more likely to agglomerate. The role of GO is
weakened to some extent, and the promotion effect on the hydration
6
Cement and Concrete Composites 130 (2022) 104508
reaction of cement is limited, resulting in some defects in the matrix.
Therefore, the resistance of SFRC to chloride ions penetration decreases.
3.4. Freeze-thaw resistance
The operation of the freeze-thaw cycle test is shown in Fig. 6 (a).
From Fig. 6 (b)–(f), it can be seen that after 100 freeze-thaw cycles, each
group of specimens showed different degrees of spalling. Among them,
the matrix of SFRC was peeled off in a large area, and the size of the
specimen had changed significantly. In contrast, the specimens with GO
showed better frost resistance. Although there was a large number of
matrix exfoliation on the surface of GOSFRC-1, the amount of exfoliation
was significantly less than that of the reference specimen. Then, with the
gradual increase of GO content, the frost resistance of GOSFRC-3 and
GOSFRC-5 was better and better. Compared with other groups, the
integrity of GOSFRC-5 specimen was very superior. There was only a
small amount of matrix exfoliation on the surface of the specimen, and
the mass loss was far less than that of other groups. It can be judged that
when the GO content was 0.05 wt%, the improvement of the frost
resistance of the specimen was the most significant. When the GO con­
tent is 0.07 wt%, the damage of the specimen is more serious than 0.05
wt%, which shows that excessive GO is also not conducive to the frost
resistance of the specimen.
It can be seen from Fig. 7 that as the freeze-thaw cycle test goes to the
C. Liu et al. Cement and Concrete Composites 130 (2022) 104508

Fig. 6. Freeze-thaw cycle test and appearance changes of specimens after 100 tests.

Fig. 7. Freeze-thaw loss rate of each group of specimens.

7
C. Liu et al.
Fig. 8. XRD patterns of the matrix at different curing ages.
later stage, the increase of the loss rate of concrete specimens is faster,
which indicates that the effect of the freeze-thaw cycle on concrete has a
“snowballing effect”. When a part of the specimen appears spalling
damage under the action of freeze-thaw, this spalling place will become
a weak point, after that, it gradually became larger under the damage of
multiple freeze-thaw cycles, and finally destroyed the entire specimen.
As mentioned above, the freeze-thaw loss of the reference group was
larger than that of the other four groups of specimens with GO. After 100
freeze-thaw cycles, the mass loss of SFRC was as high as 20.7%, and the
relative dynamic elastic modulus loss was 58.9%. The relative dynamic
elastic modulus loss and mass loss rate of SFRC with GO were lower than
those of SFRC, and the freeze-thaw loss of GOSFRC-5 was the lowest.
After 100 freeze-thaw cycles, the mass loss and relative dynamic elastic
modulus loss were 4.5% and 32.6%, respectively. The performance
degradation of concrete is inevitable after freeze-thaw because the
concrete is a porous and heterogeneous medium, and the micropores are
difficult to resist the intrusion of water. The external water and the
original pore water freeze under the action of freezing, resulting in the
expansion of the concrete matrix. Then, in the process of heating, ice
gradually melts into water, which is a complete freeze-thaw cycle pro­
cess. When this cycle process is repeated frequently, the accumulated
expansion stress will lead to the cracking and spalling of the concrete
surface, the exposed concrete will continue to be subjected to freeze-
thaw damage, and finally, the concrete structure will be completely
damaged.
The reason why GO improves the frost resistance of concrete is its
unique nano-filling effect, crystal nucleus effect, and template regula­
tion. The nano-size effect of GO has a significant effect on infilling a
large number of harmful pores and micro-cracks in the matrix. At the
same time, GO has a promoting effect on the hydration reaction of
cement. Its two-dimensional lamellar structure is used as a template, and
the adsorbed hydration products are gathered on its surface to grow.
Finally, a regular and dense hydration crystal is formed. These two as­
pects greatly improve the compactness of the matrix, greatly reduce the
content of pore water, and have a certain blocking effect on the moisture
in the external environment. When the internal density of concrete is
high, the destruction of freeze-thaw on it will be greatly reduced.
However, the content of GO also has a significant impact on its role in
concrete. As shown in Fig. 6, with the increase of GO content, the frost
resistance of the specimen shows a trend of first strengthening and then
weakening. This is due to the poor dispersion of GO when the content of
GO is too much, and it is easier to combine with free calcium ions in the
cement matrix, which affects the improvement of frost resistance of
8
Cement and Concrete Composites 130 (2022) 104508
concrete.
3.5. Matrix composition
The XRD patterns of each group after 3 and 28 days of curing are
shown in Fig. 8. It can be found from Fig. 8 (a) that a large amount of
dicalcium silicate (C2S), tricalcium silicate (C3S), and SiO2 were still
retained in each group of samples. Among them, the C2S and C3S in the
sample were due to the incomplete hydration of cement at this time, and
a large number of cement clinkers were not reacted. SiO2 is due to the
late hydration reaction time of fly ash in the sample. By observing the
diffraction pattern for 3 days, it can be seen that the diffraction peaks
corresponding to C2S and C3S in the sample doped with GO are also
lower than those in the reference sample, and the diffraction peaks of
calcium hydroxide (CH) and calcium silicate hydrate (C–S–H) are
generally stronger than those in the reference sample. This is because
GO promotes the early hydration of cement, making the contents of C2S
and C3S in the paste gradually decrease and the hydration products
gradually increase. Fig. 8 (b) shows that after 28 days of curing, the
diffraction peaks of C2S and C3S in the sample have disappeared, with
only a small amount of residue. The diffraction peak of SiO2 has dis­
appeared, indicating that the hydration reaction of the sample at the age
of 28 days is relatively complete, and the raw materials are completely
hydrated. Fig. 8 (b) also shows that the diffraction peak intensity of
hydration products in the sample is not much different from that of the
reference sample at 28 days of curing. This indicates that GO mainly
plays a role in the early hydration reaction of cement, which is also the
reason why the early strength growth rate of SFRC is higher than that of
the latter. It can also be seen in the diagram that the effect of GO content
on the hydration reaction is also significantly different. Compared with
the reference sample SFRC, when the GO content is 0.05 wt%, the
diffraction peaks of CH and C–S–H also gradually increase, which also
explains why GOSFRC-5 group has the best mechanical properties. It is
worth mentioning that the diffraction peak of CaCO3 in Fig. 8 (b) may be
the carbonation of the sample in the maintenance and treatment process.
By analyzing the XRD patterns of the samples at different ages, it can be
seen that GO did not react in the cement matrix, nor did it change the
type of hydration products. Its working mechanism is mainly to promote
the early hydration process. In a certain range, this effect gradually in­
creases with the increase of the dosage, but the effect on hydration is
weakened when it is overused.
C. Liu et al. Cement and Concrete Composites 130 (2022) 104508

Table 5 pores further enhances the compactness of the matrix, and the me­
Effect of GO on concrete pore structure. chanical properties and durability of concrete are improved.
Number Porosity (%) median pore-size (nm) average pore-size (nm) Fig. 9 shows that the pore size range of GO-doped specimens is
mainly concentrated in the range of 10 nm–100 nm, which indicates that
SFRC 11.3587 39.41 29.81
GOSFRC-1 13.5549 33.15 25.74 the regulation of GO on pore structure is mainly reflected in the elimi­
GOSFRC-3 12.9372 27.36 21.24 nation of large micropores and the increase of small micropores. As
GOSFRC-5 15.9093 25.39 18.75 shown in Fig. 9 (b), compared with other groups of specimens, the
GOSFRC-7 16.3147 34.47 27.08 macropores of GOSFRC-5 were significantly reduced, which showed that
when the GO content was 0.05 wt%, the pore repair effect was the best.
3.6. Pore structure At this time, the hydration products became denser than the reference
specimens, and the defects in the matrix were significantly repaired.
According to the results of Table 5, the incorporation of GO leads to When the GO content was further increased to 0.07 wt%, the large mi­
the increase of porosity of concrete, but the pore size of concrete has cropores of the matrix began to increase again, indicating that too much
decreased to varying degrees at the same time. This change is due to the GO is not conducive to the improvement of the pore structure. The
nano-filling effect and nucleation effect of GO. The hydration products fundamental reason is that when the dosage of GO is too much, it is
are often intertwined and overlapped irregularly, and eventually form a easier to adsorb between layers, which is not conducive to its role. In
porous, disorderly, and amorphous gel state. There are a lot of defects in addition, the free calcium ions in the matrix are easier to complex with
this microstructure, and many micro-cracks and micropores will GO, resulting in the granulation and aggregation of GO into clusters,
continue to penetrate and extend after the force, resulting in a signifi­ resulting in a significant weakening of its reinforcement.
cant decline in the performance of concrete structures. However, the
incorporation of GO promotes the early process of cement hydration
3.7. Microstructure
reaction. GO acts as a crystal nucleus to adsorb the hydration products
onto the surface. Under the control of GO, the originally disordered
As shown in Fig. 10, steel fiber and concrete matrix formed a good
hydration products grow densely and aggregate into a regular poly­
occlusion, there is no too obvious interface transition zone between fiber
hedron crystal structure. A large number of large micropores in the
and slurry. The reason is that the corrugated surface of the steel fiber
matrix are eliminated, and small micropores begin to increase. The de­
increases the water holding capacity of the fiber surface, making the
fects in the microstructure are repaired, and the compactness of concrete
water-binder ratio in the interface area larger than that of the cement
is improved. In summary, the increase of small pores in the matrix leads
matrix, and the water film thickness increases. In this case, the growth of
to the increase of porosity of concrete, but the disappearance of large
hydration products is no longer subject to any constraints, thus forming

Fig. 9. MIP results.

Fig. 10. Interface area between steel fiber and concrete matrix.

9
C. Liu et al.
Fig. 11. Micromorphology of the matrix after curing for 3 days.
a crystal enrichment layer, and the mechanical bite force and interfacial
friction between the matrix and the steel fiber are greatly enhanced.
Through the enlarged image, it is not difficult to find that the surface of
the steel fiber is covered with rich and dense gel hydration products,
which greatly improves the cementing force between the slurry and the
steel fiber. The reason is that GO is orderly arranged under the action of
ultrasonic dispersion, and can be more evenly distributed in the matrix
and steel fiber surface. At the same time, the size of GO is mainly
concentrated below 3um, and its specific surface area is relatively large,
which creates a large number of nucleation sites and is easy to provide
conditions for the growth of hydration products. The continuous
stacking cross-linking between hydration products makes the bond be­
tween steel fiber and matrix closer, and improves the overall density of
SFRC.
10
Cement and Concrete Composites 130 (2022) 104508
Fig. 11 shows the microstructure of concrete specimens after curing
for 3 days. From Fig. 11 (a), it can be found that there are a large number
of obvious holes and cracks in the microstructure of cement matrix
composites without GO, and the microstructure is very loose and un­
even. From Fig. 11 (b)–(e), it is not difficult to find that with the increase
of GO content, the microstructure of the specimen is improved. The
matrix density of GOSFRC-1 is slightly better than that of the reference,
the crack becomes narrow, and there are rich acicular and lamellar
hydration products, but there are still unreacted FA particles and holes
in the matrix. GOSFRC-3 (Fig. 11 (c)) has no large pores, and can see gel-
like C–S–H and a large number of flake calcium hydroxide crystals. The
distribution of hydration products is more regular than the previous two
groups of specimens. GOSFRC-5 (Fig. 11 (d)) basically had the best
performance in all the performance tests, and by observing its
C. Liu et al.
Fig. 12. Micromorphology of the matrix after curing for 28 days.
microstructure, it could be found that the hydration products were
intertwined and aggregated on the GO surface, and finally developed
into a regular cluster hydration crystal. This reflects the template effect
and regulation of GO. These “flowers” grow on the surface or interlayer
of flake products, which improves the uniformity and compactness of
microstructure. Although a large number of needle-like ettringite (AFt)
can be seen in GOSFRC-7 (Fig. 11 (e)), which is initially intertwined, and
it does not reach the regular flower morphology as GOSFRC-5, indi­
cating that the excessive incorporation of GO weakens the micro-
regulation range of concrete. In summary, the hydration products of
the reference specimens have no regular and orderly morphology and
distribution, and a large number of pores and micro-cracks are distrib­
uted in the matrix. The hydration products of samples doped with GO
tend to crystallize, the pores and cracks are significantly reduced, and
the effect of GO content in a certain range will gradually strengthen. But
as the content of GO is too high, the crystal product distribution of hy­
dration products is uneven and irregular. At the same time, because the
hydration reaction only lasted for 3 days, although the microstructure of
each group of specimens was different, the overall compactness was
poor, and there were more or less some pores and cracks.
Fig. 12 shows the microstructure of the specimen after 28 days of
11
Cement and Concrete Composites 130 (2022) 104508
curing. As shown in the figure, the density of the matrix has been
significantly improved after 28 days of curing. The hydration products
of SFRC (Fig. 12(a)) have been roughly contiguous, but still do not have
regular morphology, accompanied by pores and cracks, and there are
still obvious defects in the microstructure. The hydration products of
GOSFRC-1 (Fig. 12 (b)) have certain morphological characteristics
compared with the reference parts, and most of them are cluster parti­
cles. However, because the combination between particles is not close,
there are still many small pores, and the microstructure is not uniform
and closely. Fig. 12 (c) shows that the hydration products of GOSFRC-3
have a trend of interlaced aggregation, and regular flower-like crystals
can be observed. The integrity of the microstructure of GOSFRC-3 is
higher than SFRC and GOSFRC-1. Fig. 12 (d) shows that there are a large
number of flower-like crystals in the matrix of GOSFRC-5. The micro­
structure is dense and regular, and the cracks and holes almost disap­
pear. Under the role of GO, a large number of hydration products are
interwoven and aggregated into a crystal structure with flower-like
morphology. The flower-like crystals are connected to form a large
area of the dense structure, and the continuity of the overall compact­
ness of the matrix is significantly improved. The microstructure of
GOSFRC-7 (Fig. 12 (e)) is similar to that of GOSFRC-1, the hydration
C. Liu et al.
products are mostly agglomerated particles with relatively low
compactness and uneven distribution of hydration products. By studying
the microstructure development process of the samples after curing for 3
days and 28 days, it can be seen that the matrix is formed by the needle,
rod, and so on through mutual embedding and interweaving. Within a
certain range, with the increase of GO content, the distribution and
aggregation state of hydration products are significantly improved. This
is due to the large surface energy and many active groups of GO, which
can adsorb hydration products on the surface to make it grow dense and
eventually form regular crystal morphology. These SEM images proves
that a small amount of GO nanosheets have an obvious strengthening
effect on cement and concrete. With the increase of GO content, it is
easier to form aggregates with free calcium ions in the matrix, resulting
in poor distribution of GO. Therefore, the size effect and crystal nucleus
effect of GO are affected, which cannot provide the growth point for the
hydration crystal, and eventually leads to the disorderly growth of hy­
dration products, and there are many micro defects in the matrix.
4. Conclusion
In this study, the effects of GO on the mechanical properties and
durability of SFRC were mainly studied by experiments. The following
conclusions can be drawn：
(1) GO has significantly improved the mechanical properties of
SFRC, and the early strength growth rate is more obvious. The
experimental data show that the strength of SFRC increases first
and then decreases with the increase of GO content. Among them,
when the GO content is 0.05 wt%, SFRC has the best compressive
performance. The compressive strength is 53.3 MPa after curing
for 28 days and the growth rate is 20.1%. When the GO content
was 0.03 wt%, the flexural strength and splitting tensile strength
of SFRC reach the highest, and the strength is 7.6 MPa and 4.63
MPa after curing for 28 days. The growth rates were 29.8% and
26.2%, respectively.
(2) GO has significantly improved the durability of SFRC. When the
GO content was 0.03 wt%, the chloride ions resistance of the
specimen was the best after 28 days of curing. The chloride ions
penetration depth was 4.8 mm, which was 53.8% lower than that
of the reference group. The sample with 0.05 wt% GO has the best
chloride ions resistance after 56 days of curing. The chloride ions
penetration depth was 3.8 mm, which was 56.8% lower than the
reference group. The results of the freeze-thaw test show that the
mass loss of the reference group after the freeze-thaw cycle test is
as high as 20.7%, and the relative dynamic elastic modulus de­
creases by 58.9%. The frost resistance of SFRC was significantly
improved after adding GO. The freeze-thaw loss was the smallest
when GO was 0.05 wt%, and the mass loss and relative dynamic
modulus loss after the freeze-thaw cycle test were 4.5% and
32.6%, respectively.
(3) The effects of GO on the phase composition, microstructure, and
pore structure of SFRC were investigated by SEM, XRD, and MIP.
XRD patterns showed that GO accelerated the early hydration
and promoted the conversion of cement clinker such as C2S and
C3S to hydration products. In the later stage of hydration, the
influence of GO is relatively limited. MIP results showed that the
incorporation of GO reduced the average pore size of SFRC and
promoted the transformation of large micropores to small mi­
cropores. The SEM images showed that the incorporation of GO
repairs the micro-cracks inside the matrix, regulates the aggre­
gation morphology of hydration products, makes them more
regular and dense. In addition, GO has strengthened the bonding
between steel fiber and the matrix. All the changes at the micro-
level have greatly enhanced the macro performance of SFRC.
These findings lay solid theoretical support and practical guid­
ance for the preparation of high-performance concrete materials.
12
Cement and Concrete Composites 130 (2022) 104508
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgment
This research was supported by Chongqing Technology Innovation
and Application Development Special General Project (cstc2020jscx-
msxmX0084), the Natural Science Foundation of China (52078079),
Chongqing Construction Science and technology project (Urban S&T
2021 No. 1-8) and Guangzhou Science and Technology Project
(202102010455).
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 Update
Cement and Concrete Composites
Volume 131, Issue , August 2022, Page

DOI: https://doi.org/10.1016/j.cemconcomp.2022.104567
 Cement and Concrete Composites 131 (2022) 104567

Contents lists available at ScienceDirect

Cement and Concrete Composites

journal homepage: www.elsevier.com/locate/cemconcomp

Corrigendum to “Studies on mechanical properties and durability of steel

fiber reinforced concrete incorporating graphene oxide” [Cem. Concr.
Compos. 130 (2022) 104508]
Changjiang Liu a, *, 1, 2, Xiaochuan Huang b, **, 1, 2, Yu-You Wu c, ***, 1, 2, Xiaowei Deng d, ****,
Zhoulian Zheng e, *****, Bo Yang e, ******
a
School of Civil Engineering, Guangzhou University, Guangzhou, 510006, China
b
College of Environment and Civil Engineering, Chengdu University of Technology, Chengdu, 610059, China
c
School of Transportation, Civil Engineering and Architecture, Foshan University, Foshan, Guangdong, 528000, China
d
Department of Civil Engineering, The University of Hong Kong, Pokfulam, 999077, Hong Kong, China
e
School of Civil Engineering, Chongqing University, Chongqing, 400045, China

The authors regret The authors would like to apologise for any inconvenience caused.
The author’s name is corrected as follows: Xiaochuan Huang.

DOI of original article: https://doi.org/10.1016/j.cemconcomp.2022.104508.

* Corresponding author.
** Corresponding author.
*** Corresponding author.
**** Corresponding author.
***** Corresponding author.
***** Corresponding author.
E-mail addresses: cjliu@gzhu.edu.cn (C. Liu), hxc313440155@163.com (X. Huang), yuyou.wu@yahoo.com (Y.-Y. Wu), xwdeng@hku.hk (X. Deng), zhengzl@cqu.
edu.cn (Z. Zheng), yang0206@cqu.edu.cn (B. Yang).
1
Contributed equally to this work.
2
Co-first authors.

https://doi.org/10.1016/j.cemconcomp.2022.104567

Available online 11 May 2022

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