Composite Structures 134 (2015) 106113

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Composite Structures
journal homepage: www.elsevier.com/locate/compstruct

Durability of graphite coated carbon composite bipolar plates for

vanadium redox flow batteries
Jaeheon Choe a, Jun Woo Lim b, Minkook Kim a, Jinwhan Kim a, Dai Gil Lee a,
a
b

School of Mechanical, Aerospace and Systems Engineering, KAIST (Korea Advanced Institute of Science and Technology), 291, Daehak-ro, Yuseong-gu, Daejeon, Republic of Korea
LANL-CBNU Engineering Institute Korea, Chonbuk National University, 567, Baekje-daero, Deokjin-gu, Jeonju-si, Jeollabuk-do, Republic of Korea

a r t i c l e

i n f o

Article history:
Available online 11 August 2015
Keywords:
Vanadium redox flow battery (VRFB)
Graphite coated composite bipolar plate
Electro-chemical corrosion

a b s t r a c t
Composite bipolar plates for vanadium redox flow batteries (VRFBs) and fuel cells are coated with
expanded graphite to decrease the interfacial contact resistance of the carbon composite. The bipolar
plates of vanadium redox flow batteries are exposed to electro-chemical corrosion, which might degrade
the graphite coating layer. From two types of graphite foil, i.e., pyrolytic graphite and expanded flaketype graphite, the former has higher durability because its graphene sheets are crystallized in a planar
direction with a highly oriented structure, which has a stronger van der Waals bonding.
In this study, the characteristics of the pyrolytic graphite and expanded flake-type graphite are investigated with respect to the porosity of graphite. The durability of the graphite coating of the carbon/epoxy
composite bipolar plate during the electrochemical reaction in vanadium electrolytes, based on highly
concentrated sulfuric acid, is investigated. The areal specific resistances (ASRs) of the bipolar plates
coated with pyrolytic graphite are measured, from which the ASR is expressed in terms of modulus of
the graphite based on the Hertzian contact model. A single cell test is performed to evaluate the performance of the developed bipolar plate.
2015 Elsevier Ltd. All rights reserved.

1. Introduction

vanadium ions in the electrolytes based on sulfuric acid. The cathodic reaction is as follows:

Recently, electric power management has become an important

issue as power consumption has been increased, but the construction of new power plants is restricted because of environmental
problems and the NIMBY attitude. In addition, because the power
supply from renewable energy sources, such as solar and wind
power, is unstable, the use of a power stabilization system is necessary. Therefore, the needs for energy storage systems (ESSs) are
increasing, which enable the storage of excess electricity during
non-peak time and release of it when the electricity demand
increases [1,2].
In the past, lithium ion batteries were commonly used for ESSs;
however, due to their explosiveness, such batteries have been
replaced by vanadium redox flow batteries (VRFBs). The VRFB
has no explosive character, as it uses a liquid electrolyte based
on sulfuric acid, and the energy capacity of VRFBs is easily controlled by the amount of electrolyte. Basically, the charge and discharge of VRFBs occur through the reduction and oxidation of

VO2 2H e $ VO2 H2 O

Corresponding author. Tel.: +82 42 350 3221; fax: +82 42 350 5221.
E-mail address: dglee@kaist.ac.kr (D.G. Lee).
http://dx.doi.org/10.1016/j.compstruct.2015.08.030
0263-8223/ 2015 Elsevier Ltd. All rights reserved.

In an anode, the reaction is as follows:

2

$ V3 e

These reactions occur simultaneously in the electrodes [3].

A VRFB system generally consists of a stack, two liquid electrolyte tanks, and two pumps, as shown in Fig. 1(a) [4]. A cell
is composed of a proton exchange membrane, two electrodes,
two flow frames, and two bipolar plates, as shown in Fig. 1(b).
For the electrodes, carbon felt is used, which provides a large
reactive surface and an electrolyte path. The flow frame is generally made of polymer, and it supports other components. The
bipolar plate which separates each cell is generally made of graphite because it is highly conductive and resistant to sulfuric acid
[5]. However, the graphite bipolar plate is very brittle and has
low mechanical properties, which is not adequate for the VRFB
as it has a large reactive area to compensate the low energy density less than 100 mA/cm2 [6]. To overcome this issue, Kim et al.
have developed a carbon/epoxy composite bipolar plate that has

J. Choe et al. / Composite Structures 134 (2015) 106113

107

Fig. 1. Schematic diagrams of the VRFB: (a) a whole system; (b) a single cell.

an expanded flake-type graphite coating layer; this bipolar plate

achieved both high electrical conductivity and good mechanical
properties [7].
In VRFBs, all the components are exposed to the highly concentrated sulfuric acid which is a main ingredient of the electrolyte. In
addition, the cell voltage can be higher than the necessary potential for water electrolysis, and water might be decomposed into
oxygen and hydrogen during operation [8]. This phenomenon

occurs mainly near the surface of bipolar plates, especially the graphite coating layer. If the water penetrated into the graphite is
electrolyzed, then the generated gas may delaminate the graphite
layer. Furthermore, oxygen molecules may combine with the graphite because the sulfuric acid in the electrolyte is a very strong
oxidizing agent [9]. The oxidized graphite has weaker bonds
between the graphene layer, which causes the intercalation and
exfoliation of graphite eventually [10].

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J. Choe et al. / Composite Structures 134 (2015) 106113

Table 1
Properties of the graphite foils.
Type

Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Expanded flake-type

Porosity,

Table 2
Measured permeability of the graphite foils.

Thickness
(lm)

Density
(kg/m3)

Electrical
conductivity
(S/cm)

0.15
0.20
0.24
0.46
0.62
0.42

25
40
50
70
100
100

1900
1800
1700
1210
850
940

>10,000 S/cm

There are two types of graphite foil: pyrolytic graphite and

expanded flake-type graphite. Conventionally, the expanded
flake-type graphite was used as the coating material for bipolar
plates [11]. Since the graphite particles in expanded flake-type graphite are aligned randomly due to the fabrication process, which
means that its mechanical properties are very poor. On the other
hand, the pyrolytic graphite is produced by heating a hydrocarbon,
and its graphene sheets are crystallized in a planar direction.
Therefore, the pyrolytic graphite has a highly oriented structure,
and the van der Waals bonding in the pyrolytic graphite is much
stronger. In addition, covalent bonding occurs between the graphene sheets because some of the hydrocarbons remain during
production, which makes the pyrolytic graphite have higher
mechanical properties than the expanded flake-type graphite.
Regarding electro-chemical corrosion, the pyrolytic graphite may
have higher durability because water will penetrate less into the
graphene layer, and the stronger bonding between graphene layers
will prevent delamination. If the pyrolytic graphite is adopted as
the coating material for the composite bipolar plate for VRFBs,
the chemical and electro-chemical durability of the composite
bipolar plate might be improved substantially.
In this study, a carbon/epoxy composite bipolar plate coated
with pyrolytic graphite is developed. The electro-chemical corrosion on the bipolar plate is investigated with respect to the porosity of the graphite coating. The properties that may affect the
corrosion aspect are measured and analyzed. After the fabrication
process for the bipolar plate is optimized, the performance of the
developed bipolar plate is evaluated.
2. Electro-chemical corrosion of graphite coating
In a VRFB cell, the potential difference is approximately 1.4 V,
which may electrolyze water in the electrolyte into oxygen and
hydrogen during operation because the required potential for the
electrolysis of water is around 1.3 V. In some circumstances, electric
current passes through an abnormal path, such as the electrolyte
flow path, which generates a potential difference higher than
1.4 V on the bipolar plate of VRFBs. In that case, the generated oxygen from electrolysis becomes very active, and it can be easily combined with graphite. In addition, sulfuric acid in the electrolyte is a
very strong oxidizing agent, which may accelerate this reaction.
Eventually, this will weaken the van der Waals force between the
graphene layers, and the graphite is then exfoliated electrochemically [9]. The degradation of the graphite coating increases
the resistance of the bipolar plate, which decreases the efficiency
of the batteries. In addition, the delaminated graphite pollutes the
electrolyte and fills the pores of the carbon felt electrodes, which
will increase the pumping loss. Therefore, the aspects of electrochemical corrosion of graphite should be investigated based on
the properties of graphite, such as porosity, permeability, and types.
2.1. Permeability measurement
The permeability of various graphite foils with respect to porosity (U) and types was measured to verify the relation to the

Type

Porosity, U

Permeability coefficient (1020 s)

Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Expanded flake-type

0.15
0.20
0.24
0.46
0.62
0.42

1.83
3.07
3.75
5.00
8.54
296,000

5 cm
Graphite foil

Al plate

5 cm
0.1M Sulfuric acid solution
Fig. 2. Schematic illustration of the experimental setup for the electro-chemical
aging test.

electro-chemical corrosion. Five pyrolytic graphite foils (PGS, Panasonic, Japan) with different porosities and an expanded flake-type
graphite (BD-100, Samjung CNG, Republic of Korea) were tested.
The properties of the graphite are listed in Table 1. The water vapor
transmission rate (WVTR) was measured at 40 C and 90% relative
humidity based on the ASTM standard. To normalize the result,
permeability coefficient was calculated as follows [12]:

Permeability coefficient

WVTR
b
Pw

where, Pw is the pressure difference across the specimen (6700 Pa in

this work), and b is the thickness of the specimen. The calculated
result is presented in Table 2. The permeability coefficient of pyrolytic graphite increased when the porosity U was increased as
expected. The pyrolytic graphite with the U of 0.15 was least permeable, and its permeability coefficient was 1.83  1020 s. In addition, the value increased up to 8.54  1020 s when the U of
pyrolytic graphite was increased to 0.62. The increase of permeability was due to the increase of the pore space. However, the
expanded flake-type graphite showed different results compared
to the pyrolytic one. The measured permeability coefficient was
2.96  1015 s when the U was 0.42, which was approximately
105 times higher than that of pyrolytic graphite. This was due to
the difference of microstructure in the two types of graphite.
Because the pyrolytic graphite has a highly ordered structure in
the planar direction, the water vapor cannot penetrate easily. How-

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J. Choe et al. / Composite Structures 134 (2015) 106113

aging, from which the mass loss per unit area was calculated.
The graph in Fig. 3 shows the mass loss per unit area for the various
graphite samples, and the average mass loss rate per unit area of
each graphite is presented in Table 3.
According to the results, the mass per unit area decreased linearly with time. The permeability difference did not show any
obvious trend in the case of pyrolytic graphite. Although, the pyrolytic graphite with U of 0.62 had approximately 5 times higher
permeability than that with U of 0.15, but the mass loss rate
increased only 9% because the electro-chemical corrosion occurred
mainly on the surface of graphite. Although the porosities of the
pyrolytic graphites were different, the van der Waals force
between the graphene layers did not change substantially due to
the similar structure.
In addition, the pyrolytic graphite showed much higher durability compared to the expanded flake-type graphite because it had
stronger bonding between the graphene layers, as mentioned previously. The slope of the mass loss of the pyrolytic graphite was
much flatter than that of the expanded flake-type graphite, which
means that the degradation of the pyrolytic graphite occurred
more slowly. Fig. 4 shows the SEM images of both the pyrolytic
graphite and expanded flake-type graphite before and after aging.
Little change was observed in the case of pyrolytic graphite. However, the surface of the expanded flake-type graphite was significantly changed, and some evident traces of exfoliation of
graphite were observed. Therefore, it can be concluded that the
durability of pyrolytic graphite against electro-chemical corrosion
is much higher than the durability of expanded flake-type graphite.

Mass loss (kg/m2)

Time (s)

= 0.15
= 0.20
= 0.24
= 0.46
= 0.62
= 0.42 (Flake-type)

(a)

Mass loss (kg/m2)

Time (s)

= 0.15
= 0.20
= 0.24
= 0.46
= 0.62

3. Electrical properties of the bipolar plates

(b)

3.1. Fabrication of the bipolar plate specimens

Fig. 3. Mass loss per unit area with respect to time: (a) various graphite samples;
(b) pyrolytic graphite.

ever, the graphite structures in the expanded flake-type graphite

are randomly aligned, which enables the water vapor transmission
more likely to occur.
2.2. Electro-chemical aging test
The electro-chemical aging tests were performed to investigate
the durability with respect to graphite type and U. The experimental setup is shown in Fig. 2. The test conditions were determined
based on the operational conditions of the VRFBs. The porosity of
pyrolytic graphite was varied from 0.15 to 0.62, while that of
expanded flake-type graphite was fixed to be 0.42. A graphite foil
of 50 mm by 50 mm and an aluminum plate of the same size were
submerged into 0.1 M sulfuric acid solution, and the voltage of 10 V
and current density of 1200 A/m2 were applied to the two plates.
The graphite foil was connected to the anode, where oxygen was
generated, while the aluminum plate was connected to the cathode
where hydrogen was generated. The aging time was varied from
60 s up to 600 s. The mass change was measured before and after

The bipolar plate specimens coated with pyrolytic graphite

were fabricated via compression molding using a hot press. A plain
weave carbon/epoxy prepreg (WSN 1k, SK Chemicals, Republic of
Korea) and commercial pyrolytic graphite foils of different porosities and thickness were used. The properties of the plain weave
carbon/epoxy prepreg are presented in Table 4.
Fig. 5 shows the schematic illustration of the fabrication process
[13]. First, 2 plies of prepregs were stacked, and the pyrolytic graphite was attached to both sides. Next, the specimen was placed in
a steel compression mold and cured at 125 C for 1 h. The curing
pressure was 20 MPa during the process.
3.2. Electrical resistance measurement
Because the resistance of a bipolar plate affects the ohmic loss
in a stack, it is an important factor that determines the efficiency
of VRFBs. To measure the total resistance of the fabricated bipolar
plate specimens, the four-point probe method with the experimental setup shown in Fig. 6 was used. A specimen of 100 mm by
100 mm was placed between two carbon felt electrodes, the properties of which are presented in Table 5. In addition, these electrodes were mounted between two gold-coated copper plates,

Table 3
Average mass loss rate per unit area of the graphite foils.
Type

Porosity, U

Mass loss rate (105 kg/(m2 s))

R-squared

Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Pyrolytic
Expanded flake-type

0.15
0.20
0.24
0.46
0.62
0.42

4.81
5.05
5.32
5.09
5.23
17.5

0.998
0.997
0.998
0.998
0.999
0.999

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J. Choe et al. / Composite Structures 134 (2015) 106113

Fig. 4. SEM images: (a) pyrolytic graphite before aging and (b) after aging; (c) expanded flake-type graphite before aging and (d) after aging.

Table 4
Properties of the plain weave carbon/epoxy prepreg (WSN 1 k, SK Chemicals, Republic
of Korea).
Property

Value
2

Fiber area density (kg/m )

Thickness b (mm)
Fiber volume fraction (%)
Compressive modulus in the thickness direction (GPa)

0.119
0.133
71.6
10

Fig. 6. Schematic illustration of the experimental setup for the resistance

measurement.

Fig. 5. Schematic illustration of the fabrication of a bipolar plate.

which were connected to a power supply (DP30-05CF, TOYOTECH,

Republic of Korea). Next, an electrical current of 1.0 A was applied
to the setup, and then, the voltage was measured using a multimeter (3457A, HewlettPackard, USA) to calculate the resistance. The
voltage was measured with respect to the compaction pressure
from 0.01 to 0.10 MPa using a universal testing machine (INSTRON
4469, Instron Corp., MA, USA) at a temperature of 25 1 C with
the crosshead speed of 1 mm/min. The total resistances of a composite bipolar plate and graphite and the system resistance are
as follows:

RTotalComposite 2RAuCF 2RCFGr 2RCF RGr RComposite

RTotalGr 2RAuCF 2RCFGr 2RCF RGr

RSystem 2RAuCF 2RCF

where:
RTotalComposite : Total resistance of the graphite-coated composite
bipolar plate
RTotalGr : Total resistance of the graphite.
RAuCF : Interfacial contact resistance between the gold-coated
copper plate and the carbon felt electrode.
RCFGr : Interfacial contact resistance between the carbon felt
electrode and the graphite.
RCF : Bulk resistance of the carbon felt electrode.
RGr : Bulk resistance of the graphite.
RComposite : Bulk resistance of the composite bipolar plate.
The areal specific resistance (ASR) can be defined by subtracting
the system resistance from the total resistance. The ASRs of the

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J. Choe et al. / Composite Structures 134 (2015) 106113

Table 5
Properties of the carbon felt electrode.
Value

Thickness (mm)
Fiber volume fraction (%)
Diameter (lm)
Compressive modulus in the thickness direction (kPa)
Carbonization temperature (C)
Precursor type

3
3.3
7
150
>2000
PAN

ASR (m cm2)

Property

300

ASR of graphite (m cm2)

ASR of bipolar plate at 0.05 MPa

ASR of graphite at 0.05 MPa

120
90
60
30
0

0.15,t =
b=
m
==0.15,
2525
m
==0.20,
0.20,t =
b=
4040
m
m
==0.24,
0.24,t =
b=
5050
m
m
==0.46,
7070
m
0.46,t =
b=
m
==0.62,
100
m
0.62,t =
b=
100
m

200

==0.15
== 0.20
== 0.24
= 0.46
0.62
0.15
0.20
0.24
== 0.62
25 m
m bt = 40 m
m bt = 50 m
m bt = 70 m
m tb==100
m
bt == 25
100 m
Fig. 8. ASR of graphite and the bipolar plate at the compaction pressure of
0.05 MPa.

Therefore, the bipolar plate coated with the most porous pyrolytic
graphite, U of 0.62, showed the lowest ASR.

100

3.3. Contact resistance model of the bipolar plates coated with

pyrolytic graphite

0
0

0.02

0.04

0.06

0.08

0.1

Compaction pressure (MPa)

(a)

ASR of BP (m cm2)

300
0.15,t b= =2525m
m
==0.15,
0.20,t b= =4040m
m
==0.20,
0.24,t b= =5050m
m
==0.24,
0.46,t b= =7070m
m
==0.46,
0.62,t b= =100
100m
m
==0.62,

200

100

When the bipolar plate is fabricated, the carbon fiber deforms

the graphite, which increases the contact area. Because the contact
resistance is a function of the contact area [14], both the contact
resistance and the ASR can be predicted by the numerical calculation of the contact area based on a Hertzian contact model, as
shown in Fig. 9. The width of contact area b is derived as follows
[15]:

b

0.02

0.04

0.06

0.08

0.1

Compaction pressure (MPa)

(b)
Fig. 7. Measured ASR of (a) graphite and (b) the bipolar plate.

graphite and fabricated bipolar plate with respect to the compaction pressure are shown in Fig. 7. The ASRs at the compaction
pressure of 0.05 MPa, which is the typical compaction pressure of
VRFBs, are compared in Fig. 8. All the graphite specimens have
almost identical ASRs, although they have different values of
porosity U and thickness b. As a result, the bulk resistance of graphite is negligible, and the ASR of graphite is mainly determined by
the interfacial contact resistance with the carbon felt electrode.
However, the ASR of the bipolar plate decreases as the porosity
and thickness of the pyrolytic graphite increase. This change is
due to the difference of the interfacial contact resistance between
the graphite and composite, which might be a function of mechanical properties of graphite and the fabrication parameters during
the compression molding. The graphite that has a higher U has a
lower stiffness, which makes it deform more during fabrication.

1=2
7

where, EGr is the Youngs modulus for graphite, ECF is the Youngs
modulus for carbon fiber, and mGr and mCF are the Poissons ratio of
graphite and carbon fiber, respectively. Eq. (7) can be approximated
as follows because ECF is much higher than EGr.

2F 1  m2CF =ECF 1  m2Gr =EGr

pl
1=d

2F 1  m2Gr =EGr
pl
1=d

1=2
8

According to Eq. (8), the contact resistance has a linear relationp

ship to EGr because it is inversely proportional to b [14]. Therefore, the ASR that includes the contact resistance is a function of
EG as follows.

p
ASR a EG b

To assess the validity of Eq. (9), the measured results were used.
The Youngs modulus of graphite was measured based on the
ASTM standard [16], whose data are presented in Table 6. A graph
p
of the ASR with respect to EG is shown in Fig. 10, and the formula
of the linear trend line was derived as follows:

p
ASR 21:3 EG 87:1

10
2

where, the unit of the ASR is mO cm , and the unit of Eg is GPa.

Because the coefficient of determination (R-squared) of this equation was 0.997, it accurately predicted the ASR of the bipolar plates.
Therefore, a linear relationship between the ASR of the bipolar
plates and the Youngs modulus of graphite was revealed.
4. Single cell test of the bipolar plate
To investigate the performance of the bipolar plate, charge/discharge tests were performed using single cell test equipment

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J. Choe et al. / Composite Structures 134 (2015) 106113

Carbon fiber

F : curing force

Graphite
d

2b (contact zone)

Fig. 9. Schematic illustration of the Hertzian contact model of the composite bipolar plate.

Table 6
Youngs modulus of the pyrolytic graphite foils with different porosities.
Youngs modulus, EG (GPa)

0.15
0.20
0.24
0.46
0.62

2.51
1.20
0.55
0.36
0.20

Voltage (V)

Porosity, U

(Standard Cell BLUE, Standard Energy Co., Ltd., Republic of

Korea). Because the bipolar plate coated with pyrolytic graphite
with U of 0.62 showed the lowest ASR, it was tested and compared
with a conventional bipolar plate coated with expanded flake-type
graphite with U of 0.42. The vanadium ion concentration of the
vanadium electrolyte was 4M, and the amount of each electrolyte
was 50 ml. The charge/discharge voltage was in the range of 1.0 V
to 1.8 V, and the reactive area of the cell was 49 cm2. Fig. 11 shows
a representative charge/discharge curve from the test, and the
average energy efficiencies of 5 cycles were obtained and compared. The formula of the energy efficiency gEnergy is defined as
follows:

P
tdt
gEnergy R Discharge

11

P Charge tdt

ASR of bipolar plate (m cm2)

where PDischarge is the power output during the discharge cycle, and
PCharge is the power input during the charge cycle.
The developed bipolar plate achieved 80% energy efficiency,
which is similar to the conventional bipolar plates energy efficiency of 81%. This similarity was observed because the developed
bipolar plates ASR was as low as that of the conventional bipolar
plate. Furthermore, no degradation on the developed bipolar plate

140

ASR = 21.3 EG0.5 + 87.1

120

100

80

Pyrolytic
Flake-type expanded

Time (s)
Fig. 11. Representative charge/discharge curve of the single cell test.

occurred after 20 h of the test, while the conventional one had partial delamination of graphite. Therefore, it might be concluded that
the bipolar plate coated with pyrolytic graphite is more suitable for
the VRFB application than the conventional expanded bipolar
plate.
5. Conclusion
In this study, the durability of graphite coating of a carbon/
epoxy composite bipolar plate for vanadium redox flow batteries
(VRFBs) against the electro-chemical corrosion during the operation in the highly acidic electrolyte was investigated. The mass loss
of graphite with respect to time under electro-chemical corrosion
was measured to obtain the effects of the types of graphite and
their porosities. The pyrolytic graphite showed much higher durability than the conventional expanded flake-type graphite because
the pyrolytic graphite had much lower permeability. The durability
of the pyrolytic graphite was little sensitive to the porosity of graphite while its permeability was dependent on its porosity. Therefore, it can be concluded that the type of graphite has a stronger
effect than the porosity, and the pyrolytic graphite is more suitable
for the VRFB application. Since the areal specific resistance (ASR) of
the pyrolytic graphite decreased as its porosity was increased, the
model of ASR was derived as a function of Youngs modulus of graphite using the Hertzian contact model.
From the single VRFB cell tests with the developed bipolar plate,
an energy efficiency of 80% was achieved, which was a similar
result to that of the conventional expanded bipolar plate.
Acknowledgments

0.5

1.5

EG0.5 (GPa0.5)
Fig. 10. ASR of the bipolar plate with respect to the modulus of graphite EG with the
linear trend line.

This research was supported by the Climate Change Research

Hub of KAIST (Grant No. N01150036) and the KAIST Institute
Research Fund (Grant Nos. N10150022, N10150023). Their support
is greatly appreciated.

J. Choe et al. / Composite Structures 134 (2015) 106113

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