Materials & Design 185 (2020) 108257

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Materials & Design

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

The reinforcing effect of oriented graphene on the interlaminar shear

strength of carbon fabric/epoxy composites
Xiao-Jun Shen a, b, *, Chen-Yang Dang a, c, Bo-Lin Tang a, Xiao-Hui Yang a, Hui-Jie Nie a, c,
Jing-Jing Lu a, Tong-Tong Zhang a, Klaus Friedrich b, **
a
Key Laboratory of Yarn Materials Forming and Composite Processing Technology of Zhejiang Province, Jiaxing University, Jiaxing, 314001, China
b
Institute for Composite Materials, Technical University of Kaiserslautern, Kaiserslautern, D-67663, Germany
c
School of Materials Science and Engineering, Changzhou University, Changzhou, 213164, China

h i g h l i g h t s g r a p h i c a l a b s t r a c t

The interlaminar shear strength

(ILSS) of a CF/EP composite can be
effectively improved by oriented
Fe3O4@GO.

The Fe3O4@GO can form an oriented
structure in the CF/EP composites by
magnetic field orientation.

The optimal content of oriented
Fe3O4@GO for enhancing the ILSS of
the CF/EP composite is 1 wt%.

The optimal molar ratio of Fe2þ and
Fe3þ for preparing Fe3O4@GO was
found to be 1:1.25.

a r t i c l e i n f o a b s t r a c t

Article history: In this study, nano Fe3O4 functionalized graphene oxide (Fe3O4@GO) was employed to enhance the
Received 5 August 2019 interlaminar shear strength (ILSS) of carbon fabric/epoxy (CF/EP) composites. The composite was
Received in revised form fabricated via a vacuum-assisted resin transfer molding process under a magnetic field. The micro-
5 October 2019
structure and reinforcement mechanism of the CF/EP composite was further investigated. The results
Accepted 5 October 2019
Available online 8 October 2019
indicate that the Fe3O4@GO can increase the ILSS of the CF/EP composite by 12.9%, and it can further
enhance it to 41% under the magnetic field orientation. Furthermore, it was observed that the oriented
Fe3O4@GO can also improve the flexural strength and tensile strength of the CF/EP composite by 29.7%
Keywords:
Carbon fiber
and 40.9%, respectively. The main reason is that the oriented GO arrangement is better ordered and thus
Polymer-matrix composites (PMCs) can withstand more lateral loads inside the composite.
Epoxy © 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND
Interlaminar shear strength license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Magnetic oriented graphene oxide

1. Introduction

Carbon fabric reinforced epoxy (CF/EP) composites have been

* Corresponding author. Key Laboratory of Yarn Materials Forming and Com-
widely used in many areas, including automobile, aerospace, mili-
posite Processing Technology of Zhejiang Province, Jiaxing University, Jiaxing,
314001, China.
tary, marine, etc., due to their unique properties, such as high
** Corresponding author. strength, lightweight and high modulus [1e4]. However, most of
E-mail addresses: sxj07@mail.ipc.ac.cn (X.-J. Shen), klaus.friedrich@ivw.uni-kl. the CF/EP composites are laminated plate structures. The strength
de (K. Friedrich).

https://doi.org/10.1016/j.matdes.2019.108257
0264-1275/© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
2 X.-J. Shen et al. / Materials & Design 185 (2020) 108257
in the through-thickness direction is relatively low due to the fact
that there are no fibers in the thickness direction. Furthermore, the
low strength in the through-thickness direction generally leads to
delaminations in the composites, which limits the application of
CF/EP composites [1,5,6].
The interlaminar shear strength (ILSS) of CF/EP composites de-
pends on the strength of EP and the interfacial adhesion between
CF and EP [5,7]. Thus to improve the ILSS of CF/EP composites, two
kinds of methods can be used. On the one hand, the surface of CF
should be treated. Wu et al. modified the CF surface by synergistic
modification of electrochemical oxidation and sizing treatment to
increase the surface activity of CF, which ultimately increased the
ILSS of the composite by 158% [8]. Qi et al. reported that grafting
rigid (p-phenylenediamine) and flexible structures (ethylenedi-
amine) to the CF surface could improve the interfacial properties of
composites. The rigid and flexible structures increased the ILSS of
the composite by 44.8% and 38.6%, respectively [9]. On the other
hand, the strength of EP can be reinforced by introducing some
nanofillers such as nano SiO2, nano TiO2, carbon nanotubes and
graphene and its derivatives into the EP matrix [10]. Among them,
graphene oxide (GO) is regarded as the ideal nanofiller for
enhancing epoxy resins because of its functional groups, such as
carboxyl and hydroxyl groups. The latter can react with EP to
achieve good interfacial adhesion between EP and GO [11e13].
Bhanuprakash et al. reported that GO can effectively improve the
interfacial properties between CF and EP, and increase the ILSS of
composites by 47% [2]. However, the disordered structure of the GO
is easier to agglomerate than the oriented GO, which is not
conducive to fully exerting the enhancement effect of the GO in the
composites.
This work was inspired by the honeycomb panel model: in the
honeycomb panel model, the honeycomb core material plays a
major role in bearing the lateral shear force [14]. The honeycomb
core layer can be simplified into a plurality of longitudinal support
faces. Therefore, in this work the GO platelets were oriented as
longitudinal support surfaces between the layers of the carbon
fabric. In this way, the oriented GO is supposed to carry the major
transverse shear force in the weakest area of the CF/EP composite
material (between the CF layers) and to prevent the lateral micro
cracks expanding between the composite layers.
2. Experimental section
2.1. Basic materials
Natural graphite powders were purchased from Qingdao Jinrilai
Shimo Co. Ltd, China. Carbon fabric (T300, 3 K) was bought from
Jiaxing Longshine Carbon Fiber Co. Ltd, China. FeCl3$6H2O and
FeSO4$7H2O were obtained from Lanxi Yongli Chemical Co. Ltd,
China. Concentrated sulfuric acid and hydrochloric acid were pur-
chased from Xiaoshan Chemical Reagent Co. Ltd, China. EP (digly-
cidyl ether of bisphenol A) resin and the curing agent (593) were
obtained from Haining Hailong Chemical Co. Ltd, China. Ethanol,
Sodium nitrate and potassium permanganate were purchased from
Xiaoshan Chemical Reagent Co. Ltd, China, and used as received.
2.2. Preparation of Fe3O4@GO
Graphene oxide (GO) was prepared according to our previous
work [15]. Under a nitrogen atmosphere, FeCl3$6H2O and FeS-
O4$7H2O were added to deionized water (60 ml), and the resultant
mixture was treated by ultrasonic technique (400 W) for 0.5 h. The
ratio of Fe2þ to Fe3þ was 1:1.25 and the total amount was 0.03 mol.
After that, the above mixture was added to a GO suspension
(200 ml, 0.2 mg/ml) drop by drop with mechanical stirring. Then,
the resultant mixture was heated up to 60  C and the pH value of
the mixture was tuned to 9e10 by quickly adding ammonium hy-
droxide. After that, the mixture was stirred for 2 h with constant
temperature. Then, the resultant mixture was washed by deionized
water several times till the pH value closed to 7.
2.3. Preparation of Fe3O4@GO/carbon fabric/epoxy composites
The schematic of the preparing process of CF/EP composites is
displayed in Fig. 1. The as-prepared Fe3O4@GO was dispersed in
ethanol to form a 0.2 mg/ml suspension. Then, the above suspen-
sion was treated by ultrasonication (400 W) for 0.5 h. After that, the
epoxy resin was mixed with the Fe3O4@GO suspension. The
resulting mixture was mechanically stirred for 0.5 h, and treated by
ultrasonication for another 0.5 h. It was heated in an oven at 80  C
for 24 h to remove the ethanol. Afterwards, the curing agent (593)
was added to the mixture with a ratio of 30e100 (593: EP). The
resultant suspension was degassed with a vacuum pump to elimi-
nate air bubbles and residual ethanol. The as-prepared mixture was
then transferred to the CF fabric preform to fabricate CF/EP com-
posites by a vacuum assisted resin transfer molding process
(VARTM). At the same time, two magnets were arranged on both
sides of the CF/EP composites. Curing of the CF/EP composites took
place at room temperature for 24 h under the magnetic fields. The
volume fraction of CF in the composites was characterized ac-
cording to the methods described in our previous work [16]. The
volume fraction of the CF in this work was 52 vol%.
2.4. Characterization
The phase purity of Fe3O4@GO was characterized by X-ray
diffraction (XRD), using an X-ray diffractometer with a Cu Ka ra-
diation (l ¼ 1.5418 Å). The interlaminar shear specimens were
prepared according to the standard of ASTM D2344 [17]. The
mechanical properties of the composites were measured on a
Shimadzu AG-X plus Mechanical Tester using a 50 kN load cell with
a crosshead speed of 1 mm/min. At least five specimens were
measured for each composition. Scanning electron microscope
(SEM) images were obtained by a Hitachi S-4800 microscope
(Japan). In particular, the fracture surfaces of the specimens after
interlaminar shear testing were examined. Before examination, the
fracture surfaces were cleaned using alcohol and then coated with a
thin evaporated platinum layer to improve the electrical conduc-
tivity. Transmission electron microscope (TEM) images were
created on a JEOL JEM-2010 instrument in bright field with an
accelerating voltage of 10 kV. Acetone solution containing
Fe3O4@GO was dropped onto a copper grid. After drying, it was
used to take the TEM images of the Fe3O4@GO. The distribution of
Fe3O4@GO in pure EP was observed by inverted phase contrast
microscopy (Motic, AE2000). The content of Fe3O4 in Fe3O4@GO
was analyzed using a thermogravimetric analyzer (TGA, NETZSCH
TG, 209F1), The sample was heated from ambient temperature to
800  C in air atmosphere at a heating rate of 10  C/min.
3. Results and discussion
3.1. Characterization of Fe3O4@GO
The SEM images of the as-prepared GO and Fe3O4@GO are dis-
played in Fig. 2a and b. The TEM images of the as-prepared GO and
Fe3O4@GO are displayed in Fig. 2c and d, respectively. As shown in
Fig. 2, the in-plane size of GO is about 5 mm and Fe3O4 particles are
decorated on the GO surfaces. As shown in Fig. 3, the particle size
distribution of Fe3O4 on GO was statistically analyzed, and the re-
sults showed that the average particle diameter was about 260 nm.
 X.-J. Shen et al. / Materials & Design 185 (2020) 108257 3

Fig. 1. The schematic of the preparing process of Fe3O4@GO/CF/EP composites.

Fig. 2. The SEM images of the (a) as-prepared GO and (b) Fe3O4@GO, the TEM images of (c) as-prepared GO and (d) Fe3O4@GO.

However, from Fig. 2d, it can be seen that many small spheres form
a Fe3O4 ball. This may be due to pH values in the range 9e10, so that
Fe3O4 surface charges decrease significantly, resulting in an
extensive aggregation i.e. the formation of large aggregates [18].
The TGA curve of the as-prepared Fe3O4@GO fillers is shown in
Fig. 4. It implies that the weight loss of 2.6% between room tem-
perature and 120  C can be attributed to the loss of adsorbed water.
The weight increasing between 120 and 200  C was caused by the
oxidation of Fe3O4 to Fe2O3. The drop to 93.8% over 200  C can be
attributed to the decomposition of GO. This means, the residual
sample should be Fe2O3. Therefore, the original Fe3O4 should be
90.7% in the sample. Thus, after excluding the water, a mass loading
of Fe3O4 in the Fe3O4@GO can be calculated as 93.1%.
The X-ray diffraction (XRD) patterns of Fe3O4 and Fe3O4@GO are
displayed in Fig. 5. Six sharp peaks at 2q ¼ 30.3 , 35.6 , 43.3 , 53.6 ,
57.1 and 62.9 can be distinguished for Fe3O4, which are assigned
to the diffraction of (220), (311), (400), (422), (511) and (440) planes
of Fe3O4, respectively [19,20]. In our previous work, the XRD
pattern of GO was reported, in which a broad peak appeared around
2q ¼ 10.2 , corresponding to the (002) plane [21]. Nevertheless,
there is no obvious diffraction peak of GO in the XRD pattern of
Fe3O4@GO. It can be explained by the fact that the diffraction
4 X.-J. Shen et al. / Materials & Design 185 (2020) 108257
Fig. 3. The particle size distribution of Fe3O4 on GO.
Fig. 4. TGA curve of Fe3O4@GO.
signals of Fe3O4 are significantly stronger than GO, and the weight
content of GO is relatively low in Fe3O4@GO [22]. This is consistent
with the values in the standard card (JCPDS card No. 65e3107).
The influence of the molar ratio of Fe2þ and Fe3þ on the for-
mation of Fe3O4 was analyzed by XRD, and the results are shown in
Fig. 6. The grain size of Fe3O4 particle was determined according to
Scherrer formula [23]:
Kl
D¼
b cos q
where D is the average grain size of the crystal (nm), l the ray
wavelength (nm), k the peak shape factor (value is 0.81), b the
corrected half width, and q the diffraction angle. The average grain
diameter of the Fe3O4 was calculated, and the results are shown in
Table 1.
The average grain size of Fe3O4 increased as the ratio of Fe2þ was
increased. This is consistent with the results reported in the liter-
ature [23]. Although the average grain size of Fe3O4 obtained from
the SEM data is much larger than the XRD data, this is mainly
Fig. 5. XRD patterns of the Fe3O4 and Fe3O4@GO composites.
because the Scherrer formula calculates the average grain diameter
of the Fe3O4, whereas the results observed by SEM and TEM refer to
agglomerates of Fe3O4 [18].
The as-prepared GO, Fe3O4 and Fe3O4@GO was also character-
ized by FTIR to determine its surface functional groups. The results
are shown in Fig. 7. It can be observed from the FTIR spectrum that
the GO surface is rich in oxygen-containing functional groups, and
the peaks at 3392 and 1070 cm1 can be ascribed to the stretching
vibration of eOH and alkoxy [24,25]. Fe3O4 and Fe3O4@GO showed
the FeeO stretching vibration adsorption peak at 544 and 582 cm1
[26]. In addition, Fe3O4@GO exhibits a stretching vibration peak of
alkoxy at 1053 cm1, but in comparison with GO, the spectrum of
Fe3O4@GO showed a dramatic decrease in the intensity of the
adsorption peaks of oxygen-containing functional groups, which
indicated that GO has been partially reduced due to heating [27].
3.2. Magnetic properties of Fe3O4@GO
The magnetic hysteresis measurement of the as-prepared
Fe3O4@GO was carried out at room temperature in an applied
magnetic field, sweeping from 796 to 796 kA/m. The room tem-
perature magnetic hysteresis curves are displayed in Figs. 8 and 9.
Different Fe3O4 modified GO samples were prepared by adjusting
the molar ratio of Fe2þ and Fe3þ at a GO content of 2 mg/ml, and
their magnetic properties were characterized as shown in Fig. 8.
The results show that, when the molar ratio of Fe2þ and Fe3þ is
1:1.25, the Fe3O4@GO has the best magnetic properties. The satu-
ration magnetization (Ms) is 11.2 emu/g, the coercivity (Hc) is
0.69 G, and the remanence (Mr) is 0.045 emu/g (Fig. 8). It is indi-
cated that the Fe3O4@GO exhibits soft magnetic properties. The
effect of GO concentration on the magnetic properties of Fe3O4@GO
(1) was also investigated (Fig. 9). It demonstrates that the Ms of
Fe3O4@GO increases with decreasing GO concentration. Because
the Ms is caused by Fe3O4 in the Fe3O4@GO nanocomposites [28],
the relative content of Fe3O4 increases with decreasing GO con-
centration. When the concentration of GO is 0.2 mg/ml, the Ms of
Fe3O4@GO is 30.3 emu/g, the Hc is 1.22 G, and the Mr is 0.043 emu/g
(Fig. 9).
3.3. Mechanical properties of Fe3O4@GO/CF/EP composites
The aligned GO structure cannot be seen from the side-view
 X.-J. Shen et al. / Materials & Design 185 (2020) 108257
Fig. 6. XRD patterns of Fe3O4 prepared in different molar ratios.
Table 1
The effect of the molar ratio of Fe2þ and Fe3þ on the average grain size of Fe3O4.
Molar ratio of Fe2þ and Fe3þ Average grain size of Fe3O4 (nm)
1:1 13.1
1:1.25 12.2
1:1.55 11.8
1:1.75 11.3
Fig. 7. FTIR spectrum of the as-prepared GO, Fe3O4 and Fe3O4@GO.
pictures of the CF/EP composites due to the opaqueness of the
composites. Therefore, in order to identify the orientation structure
of Fe3O4@GO in the EP layer clearly, the difference between the
oriented and non-oriented structures of Fe3O4@GO in a pure EP
composite was observed by microscopy. As shown in Fig. 10, the
non-oriented Fe3O4@GO fillers have a disordered distribution in the
resin (Fig. 10a and c). On the other hand, the oriented Fe3O4@GO
fillers are more ordered along the direction of the magnetic field
(Fig. 10b and d). The EDAX analysis of Fe3O4@GO modified epoxy
composite (Fig. 10e) also confirmed the existence of Fe3O4 in the
composite.
5
Fig. 8. Hysteresis loops of Fe3O4@GO obtained by different Fe2þ and Fe3þ molar ratios
at a GO content of 2 mg/ml.
Fig. 9. Hysteresis loops of Fe3O4@GO obtained by different GO concentrations with
constant molar ratio of Fe2þ and Fe3þ at 1:1.25.
To investigate the effect of the oriented Fe3O4@GO on the ILSS of
the CF/EP composites, the non-oriented Fe3O4@GO reinforced CF/
EP composites were also studied for comparison. The ILSS of the
specimens was calculated according to the following equation (2)
[17]:
P
F ¼ 0:75  (2)
bh
where F is the short beam shear strength (MPa), P the maximum
load (N), b the measured width (mm), and h the measured thick-
ness (mm) of the sample. The results of the ILSS of the composites
are displayed in Fig. 11.
It indicates that the ILSS of the Fe3O4@GO/CF/EP composites
prepared under a magnetic field is much higher than the com-
posites prepared without a magnetic field. When the Fe3O4@GO
content is less than 0.3 wt%, the ILSS of the CF/EP composite is
improved as increasing the Fe3O4@GO content. It could be due to
the enhancement effect of Fe3O4@GO on the EP [29,30]. Further-
more, the magnetic orientation showed an obvious improvement
to the ILSS of the CF/EP composites at the same content of
Fe3O4@GO. This could be attributed to the ordered Fe3O4@GO
6 X.-J. Shen et al. / Materials & Design 185 (2020) 108257
Fig. 10. Microscope image of an epoxy composites containing 1 wt% Fe3O4@GO: (a) top-view image of composite without magnetic orientation, (b) top-view image of composite
with magnetic orientation, (c) side-view image of composite without magnetic orientation, (d) side-view image of composite with magnetic orientation and (e) the SEM image and
EDAX analysis of the composite with magnetic orientation.
Fig. 11. Effect of orientation and contents of Fe3O4@GO relative to EP on the ILSS of CF/
EP composites.
which can bear the major transverse shear force. The cross-
sectional SEM images of the composites after the short beam
shear testing are shown in Fig. 12. It can be seen that the CF/EP
composite without Fe3O4@GO was dramatically damaged and the
delamination is obvious as shown in Fig. 12a. The cracks grow along
the interface between the CF and the EP. For the composites with
1.0 wt% non-oriented Fe3O4@GO, there are also small cracks at the
interface between the fibers and the resin, but the crack propaga-
tion path of the fracture surface is clearly dispersed and the
delamination is not as obvious (Fig. 12b). Moreover, there are no
obvious cracks in the composites with 1.0 wt% oriented Fe3O4@GO,
as displayed in Fig. 12c. It became evident that the optimal content
of oriented Fe3O4@GO to improve the ILSS of the CF/EP composite is
1.0 wt% (Fig. 11). The ILSS of the CF/EP composite reinforced by non-
oriented Fe3O4@GO reached a peak value of 48.05 MPa at 0.3 wt%
Fe3O4@GO. While the ILSS of the CF/EP composite reinforced by
oriented Fe3O4@GO reaches peak value of 59.99 MPa at 1.0 wt% of
Fe3O4@GO. However, the ILSS of the CF/EP composites reinforced by
oriented or non-oriented Fe3O4@GO decreased with a further in-
crease in the Fe3O4@GO content above the optimal content. The
declining tendency seems to be caused by a reaction of the func-
tional group of Fe3O4@GO with the epoxy groups, which influences
the curing degree of the EP resin [13]. In addition, defects or ag-
gregation of Fe3O4@GO generated as the content of Fe3O4@GO
exceeded the optimal value might also be the reason for the
decreasing ILSS of the CF/EP composites [31].
In addition, the flexural and tensile properties of the CF/EP
composites were investigated; the results are shown in Figs. 13 and
 X.-J. Shen et al. / Materials & Design 185 (2020) 108257
Fig. 12. SEM images of the CF/EP composites: (a) pure CF/EP composites; (b) CF/EP composites with 1.0 wt% non-oriented Fe3O4@GO; (c) cross section of CF/EP composites with
1.0 wt% oriented Fe3O4@GO.
Fig. 13. The effect of orientation and content of Fe3O4@GO on the flexural strength of
CF/EP composites.
Fig. 14. The effect of orientation and content of Fe3O4@GO on the tensile strength of
CF/EP composites.
14, respectively. The effects of orientated Fe3O4@GO on the flexural
and tensile properties of the CF/EP composite are similar to that of
the ILSS. The flexural strength of the composites without orienta-
tion was only increased by 4.6% at a 0.5 wt% Fe3O4@GO content.
However, the flexural strength of the composite was increased by
29.7% at a content of 0.3 wt% oriented Fe3O4@GO. Moreover, the
non-oriented Fe3O4@GO can increase the tensile strength of the
7
composite by 25%. While the tensile strength of the oriented
Fe3O4@GO/CF/EP composite can be increased by 40.9%. Further-
more, the flexural and tensile strength of the magnetic oriented
composites are much higher than the composites without magnetic
orientation at the same content of Fe3O4@GO. It can be concluded
that the orientation of the Fe3O4@GO has not only an excellent
reinforcing effect on the ILSS of the CF/EP composites but can also
greatly improves the flexural and tensile strength of the CF/EP
composites. This should be attributed to the oriented Fe3O4@GO
which can bear the major transverse shear force.
4. Conclusions
Fe3O4 magnetic particles can be decorated onto the surface of
GO. The optimal molar ratio of Fe2þ and Fe3þ was 1:1.25 for pre-
paring the Fe3O4@GO fillers. The Ms of Fe3O4@GO increased with
decreasing GO concentration. With increasing the Fe3O4@GO con-
tent, the ILSS, flexural and tensile strength of the CF/EP composite
firstly increased and then decreased. In addition, the oriented
Fe3O4@GO can improve the mechanical properties of the CF/EP
composite much more effectively than the non-oriented
Fe3O4@GO. This indicates that the orientation of GO can be a po-
tential method to improve the mechanical properties of CF/EP
composites.
Credit authorship contribution statement
Xiao-Jun Shen: Conceptualization, Data curation, Investigation,
Methodology, Writing - original draft, Writing - review & editing,
Funding acquisition, Project administration, Supervision. Chen-
Yang Dang: Data curation, Investigation, Methodology, Validation,
Writing - original draft. Bo-Lin Tang: Data curation, Formal anal-
ysis, Validation. Xiao-Hui Yang: Data curation, Investigation. Hui-
Jie Nie: Data curation, Methodology. Jing-Jing Lu: Data curation.
Tong-Tong Zhang: Data curation. Klaus Friedrich: Methodology,
Supervision, Writing - review & Editing.
Acknowledgements
This work was financially supported by the National Natural
Science Foundation of China (No. 11502096); the program of China
Scholarship Council (No. 201408330128); the Open Project Pro-
gram of Key Laboratory of Yarn Materials Forming and Composite
Processing Technology of Zhejiang Province (Nos. MTC 2019-04 and
MTC 2019e12) and the Student Research Training of Jiaxing Uni-
versity (Nos. CD8517193243 and CD8517193244).
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