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DOI 10.1007/s11581-015-1482-3

ORIGINAL PAPER

Flexible carbon nanostructures with electrospun nickel oxide


as a lithium-ion battery anode
Boor Singh Lalia 1 & Abdullah Khalil 1 & Tushar Shah 2 & Raed Hashaikeh 1

Received: 14 April 2015 / Revised: 26 May 2015 / Accepted: 27 May 2015


# Springer-Verlag Berlin Heidelberg 2015

Abstract Carbon nanostructures (CNS) with high electrical


conductivity and unique branched structure of carbon nanotubes combined with NiO nanofibers (NFs) were used as anode for lithium-ion batteries. CNS works as a framework substrate for the anodic conversion reaction of nickel oxide
(NiO). Electrochemical performance and behavior of CNS/
NiO anodes is compared with the conventional carbon (C)/
NiO anodes. CNS/NiO NF-based anode retains high specific
capacity under different current densities compared to C/NiO
anode. Moreover, specific capacity as high as 450 mAh/g for
CNS/NiO NF anode is observed compared to only 90 mAh/g
for C/NiO NFs using a current density of 500 mA/g after
500 cycles. This improved performance is attributed to the
highly conductive network of CNS leading to efficient charge
transfer. The high porosity, electrical conductivity as well as
the branched and networked nature of CNS reveal to be of
critical importance to allow the electrochemical conversion
reactions.

Keywords Electrochemical . Conversion reaction . Nickel


oxide nanofibers . Carbon nanostructures . Electrical
conductivity

* Raed Hashaikeh
rhashaikeh@masdar.ac.ae
1

Institute Center for Water and Environment (iWATER), Department


of Mechanical and Materials Engineering, Masdar Institute of
Science and Technology, Masdar, Abu Dhabi -54224, United Arab
Emirates

Applied Nanostructures Solutions, LLC, 2323 Eastern Boulevard,


Baltimore, MD 21220, USA

Introduction
Lithium-ion battery (LIB) is currently considered the most
practical energy storage device at various scales because of
its high energy density, minimum self-discharge, prolonged
consistent performance, and economy. Since its commercialization by Sony in 1991 [1], LIBs have become the primary
source of power for almost all the portable electronics such
as mobile phones, laptops, and tablets. Improvements in
their architecture have extended the hopes for their commercial usage in automobiles. Tremendous amount of research
has been done to optimize the design and composition of
cathode and anode as well as the electrolyte between them
so as to obtain the highest charge output in a consistent
manner [24].
The anode material must possess low reduction potential
and high specific capacity for high energy density batteries.
Lithium metal is at the top of the list in this regard; however,
very high reactivity with electrolyte and dendrite formation
during repeated cycling makes its usage impractical [5].
Thus, lithium was initially employed with carbon-based insertion compounds, however, at the cost of low energy density
[6]. In order to achieve higher energy density, lithium metal
can be employed in an alloyed form with other elements such
as tin (Li4.4Sn), antimony (Li3Sb), and silicon (Li4.4Si).
However, significant volume expansion and contraction of
these Li alloys during the chargedischarge cycles make them
impractical, though their energy density is much higher than
conventional carbon-based materials [7]. In order to tackle the
volumetric instability problem, various kinds of chemically
active intermetallic materials such as InSb [8] and Cu2Sb [9]
have been used as anode materials and they have shown excellent volumetric stability. However, low gravimetric energy
density and significant capacity fading with repeated cycling
are the major drawbacks of these intermetallics.

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Similar to plenty of engineering applications,


nanomaterials have shown remarkable potential as electrodes
for LIBs. The unique advantages of high surface area, short
diffusion length, enhanced ionic/electronic conductivity, and
good mechanical stability make the nanomaterials as ideal
choice for LIB electrodes. Moreover, their unique ability to
form hierarchical framework allows us to develop the electrode with desired configuration for specific performance parameters. Variety of materials in different nanostructured
forms such as nanoparticles, nanorods, and nanofibers have
been tested as anode material for LIBs, and the reported results
have been remarkably encouraging. Interested readers may
refer to the review articles [2, 10, 11] for a detailed description
of various nanomaterials such as Si and Ge nanofibers and
carbon nanotubes which have been used so far as LIB anodes.
It has been reported that if conventional bulk carbon is replaced with its nanostructured counterparts as anode material,
the capacity of LIBs can be increased by several folds [12, 13].
Recently, our group reported the use of high-performance carbon nanostructures (CNS) for the fabrication of LiFePO4based cathodes in LIBs [14]. Thus, there has been a growing
interest to produce carbon nanostructures in an economical
way so that their usage can be commercialized in LIBs.
Because of their low-cost and environment friendly nature,
metal oxides have also gained significant attention as anode
materials for LIBs [15]. In the bulk form, they are not active
enough to provide high energy density. However, at the nanoscale, their high surface greatly enhances their reactivity. In
case of metal oxides, the reaction pathway is changed from Li
insertion or alloying to the formation and decomposition of
Li2O as follows [16]:

(SEI) [19]. Reversible capacities above 300 mAh/g have been


reported for hydrothermally grown NiO NFs acting as LIB
anodes [20, 21]. Recently, NiO NFs, synthesized via
electrospinning technique, have shown reversible capacity
above 700 mAh/g [22]. This result is very encouraging from
a commercial point of view as the electrospinning is an economical and an industrially scalable technique for producing
metal oxide NFs [23].
Herein, we report the electrochemical performance of
electrospun NiO NFs impregnated in the three-dimensional
network of CNS. This composite anode system, employed in
LIBs, was found to be very efficient in terms of capacity
retention and cyclability which are the two key desired characteristics for any LIB. After several cycles, consistent capacity output was observed from this newly developed CNS/NiO
NF anode. The performance of NiO NFs when employed with
conventional amorphous carbon (C) was also studied for
comparison.

Mx Oy 2ye 2yLi xM yLi2 O

Fabrication of nickel oxide nanofibers

where BM^ represents the transition metal such as Co, Fe, Ni,
etc. This reaction is highly reversible leading to improved
capacity retention after several cycles. The reaction pathway
could be different based on the type of metal oxide used.
Plenty of nanostructured metal oxides embedded in carbon matrix have been tested as LIB anode, and remarkable improvement in capacity and energy density has been
obtained [17].
Among various nanostructured forms, Bnanofibers^ (NFs)
have gained significant attention because of their ease of synthesis, efficient electron transport, and ability to integrate with
carbon-based anode. Moreover, their strain relaxation ability
minimizes the volumetric expansion which contributes to the
stability of anode during repeated cycling. Various metal oxide NFs such as Fe2O3, Co3O4, and SnO2 have been reported
as potential candidate material for LIB anodes because of
significant enhancement in performance [18]. In this regard,
nickel oxide (NiO) NFs carry unique significance because of
their tendency towards reversible lithiation and sustained Li
diffusion after the formation of solid-electrolyte interface

Experimental methods
Materials
Nickel II acetate (Aldrich), poly(vinylalcohol) (Mw = 61,000,
Aldrich), conductive carbon Super C65 (Timrex, TIMCAL),
lithium bis(trifluoromethanesulfone) imide (LiTFSI)
(Aldrich), ethylene carbonate (EC) (Aldrich), and diethyl carbonate (DEC) (Aldrich) were used as received.

The NiO NFs were fabricated via electrospinning technique.


The details of the synthesis procedure can be found in our
previous work where we reported the fabrication of NiO
NFs with varying diameter and surface roughness via
electrospinning technique [24]. In this study, we employed
the NiO NFs with minimum diameter and maximum roughness so as to insure maximum surface area which is a highly
desirable characteristic for the LIB electrode material.
CNS synthesis
Applied NanoStructured Solutions, LLC (ANS) synthesized
CNS by the cavity CVD method using glass fiber substrate.
The detailed procedure can be found elsewhere [25]. Glass
substrate loaded with metal oxide nanoparticles acts as a catalyst for CNS growth. A high-pressure gas used to separate
the CNS from the growth substrate and contaminants from the
growth substrate were separated from CNS by using density
separation technique.

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Cell fabrication and testing


Electrode slurry was prepared by dispersing 70 wt% NiO NFs,
20 wt% CNS (or Super C65 carbon), and 10 wt% PVDF in Nmethyl-2-pyrrolidone for 24 h to obtain a homogeneous suspension. The resulting suspension was coated on the copper
current collector using doctor blade and dried in vacuum oven
for 12 h at 80 C. Specific capacities of the cells were calculated by using weight of the NiO NFs, i.e., 70 wt%. Dried
electrode were transfered to argon-filled glove box (Mbraun,
Germany) having moisture and oxygen level below 0.1 ppm.
CR2032-type coin cells were assembled inside the in glove
box using NiO NF-based electrode as a working electrode and
lithium foil as a reference and counter electrode. Glass fiber
filter (Aldrich) was used as a separator. One molar of LiTFSI
solution in binary mixture of EC:DEC (2:1 v/v) was used as an
electrolyte.
Cyclic voltammetry and electrochemical impedance spectroscopy studies of the half cells were performaed on
Autolab302N potentiostat/galvanostat. Impedance measurements were taken in a frequency range of 100 kHz10 mHz
at AC amplitude of 10 mV. Chargedischarge cycling tests
were conducted on an Arbin battery tester (USA) using a
CR2036 coin-type two-electrode cell, and the curves were
measured in the voltage range of 0.013.0 V (vs. Li+/Li).
Morphological analysis
The morphology of C, CNS, and NiO NFs and the composite
anodes was examined through transmission electron microscope (TEM) (Tecnai F20, FEI) and scanning electron microscope (NovaNano, FEI).

Results and discussion


The morphology and crystalline structure of CNS and C is
presented in Fig. 1a, b, respectively. These TEM images clearly reveal the amorphous nature of C and CNS, confirmed via
fast Fourier transform (FFT) shown in the inset. The NiO NFs,
shown in Fig. 1c, are polycrystalline, composed of tiny crystalline domains attached together in a linear one-dimensional
Fig. 1 TEM images of a CNS, b
C, and c NiO NF. Insets show the
corresponding FFT (a, b) and
selected area diffraction
pattern (c)

pattern to give the NF shape. This unique morphology imparts


the NFs very high roughness and hence high surface area,
which make them suitable as an anode material.
Figure 2 shows the TEM images of CNS/NiO NFs and
C/NiO NFs composites. In case of CNS/NiO NFs (Fig. 2a),
the NiO NFs were found to be impregnated across the threedimensional network of CNS without any noticeable covering
of NiO NFs by CNS. The HRTEM image shown in Fig. 2b
clearly reveals the impregnation of NiO crystalline domains
across the amorphous CNS. In case of C/NiO NFs (Fig. 2b),
the NiO NFs were found to be loosely connected with amorphous C particles. However, some adhesion of C particles was
observed on NiO NFs causing covering of crystalline NiO
domains, as shown in the upper inset of Fig. 2d where the
FFT consists of diffused background combined with bright
spots. The lower inset shows the FFT of the exposed crystalline domain of NiO.
Figure 3 shows the electrochemical behavior of the C/NiO,
and CNS/NiO anode was characterized by the cyclic voltammetry (CV) measurements under the voltage range of
0.013.0 V vs. Li+/Li using a scan voltage of 0.1 mV/s.
During the first scan, broad irreversible peaks were observed
around 0.36 and 0.26 V for NiO/C and NiO/CNS electrodes,
respectively. These are due to the formation of solid electrolyte interphase (SEI) layer formation on the surface of the
electrodes [26]. During the second cycle, a peak at 0.8 V is
associated with reaction of NiO and Li+ ions [16]. Redox
peaks at 1.6 and 2.2 V for both the C/NiO and CNS/NiO are
related to the conversion reaction between NiO and lithium
[27]. For NiO/C electrode, the intensity of peaks at 1.6 and
2.2 V decreases for the second and the fifth cycles which may
be attributed to the poor conversion of NiO and lithium.
However for CNS/NiO electrode, these peaks retain their intensity which represents a consistent reversible reaction between NiO and lithium.
CV results suggest that the CNS provide highly conductive
pathways between the NiO NFs and current collector which
improves the reversible conversion reaction between NiO and
lithium and thus the overall electrochemical performance.
Figure 4 shows the chargedischarge characteristics of
C/NiO and CNS/NiO anode materials under the current density of 200 mA/g. As shown in Fig. 4a, during the first

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Fig. 2 TEM images of
composites. a CNS/NiO NFs and
c C/NiO NFs. b, d Highresolution TEM images of a and
c, respectively. In b and d, insets
show the FFT of the indicated
regions

undergo significant volume change, and due to less flexibility,


the ultimate result is the formation of cracks within the electrode leading to drastic decrease in capacity. On the other
hand, the nanostructured one-dimensional materials, such as
CNS in the current case, are capable of retaining the volumetric strains due to their flexible network architecture. Thus,
they undergo minimum cracking leading to higher and more
consistent capacity output from the Li-ion battery [28].
On the other hand, capacity loss during the first discharge
charge cycle of CNS/NiO anode (Fig. 4b) was similar to that
of C/NiO. However, during second, fifth, and tenth cycle, a

discharge and charge cycle, the capacity was found to be 1414


and 926 mAh/g, respectively, for the NiO/C anode. The capacity loss during the first cycle is attributed to the formation
of SEI and irreversible reduction of NiO [16]. During the
subsequent second, fifth, and tenth chargedischarge cycle,
the capacity loss may have been due to the significant volumetric expansioncontraction leading to the pulverization and
degradation of the C/NiO electrode. In Li-ion batteries, a minimum volumetric change during successive cycling is one of
the key required characteristics for consistent chemical and
physical performance. Conventional carbon-based electrodes
0.1

1.0

b
0.5
0.0

Current (mA)

Current (mA)

0.0

-0.1

-0.2

-0.3

cycle 1
cycle 2
cycle 5

-0.4

-0.5
-1.0
-1.5
cycle 1
cycle 2
cycle 5

-2.0
-2.5

0.0

0.5

1.0

1.5

2.0

Potential ( V vs. Li/Li+)

2.5

3.0

0.0

0.5

1.0

1.5

2.0

Potential ( V vs. Li/Li+)

2.5

3.0

Fig. 3 Cyclic voltammograms of a C/NiO and b CNS/NiO as working electrode and lithium metal as counter and reference electrode in 0.013.0 V
potential range using 1 M LiTFSI/EC:DEC (2:1) electrolyte

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1D
1C
2D
2C
5D
5C
10D
10C

Potential (V)

2.5
2.0
1.5

2.0
1.5
1.0

0.5

0.5

0.0

0.0
0

200

400

600

800

1000

1200

1400

1D
1C
2D
2C
5D
5C
10D
10C

2.5

1.0

-200

3.0

Potential (V)

3.0

-200

1600

200

400

600

800

1000

1200

1400

1600

Specific capacity (mAh/g)

Specific capacity (mAh/g)

Fig. 4 Chargedischarge profile of a C/NiO and b CNS/NiO as working electrode and lithium metal as counter and reference electrode

minor capacity loss was observed. This capacity retention


during the repeated cycling is attributed to the highly conductive and nanoporous three-dimensional structure of CNS
which helps in retaining the anode structure during volumetric
expansion/contraction, occurring due to charging and
discharging processes.
Chargedischarge cycling performance of the CNS/NiO
and C/NiO electrode at different current rates is shown in

1600

100 mA/g
200 mA/g
300 mA/g
500 mA/g

Specific capacity (mAh/g)

1400
1200
1000
800
600
400

Specific capacity (mAh/g)

1600

Fig. 5. For C/NiO anode, a large irreversible capacity loss


observed during the first few cycles and after 50 cycles, specific discharge capacities were found to be 275, 247, 131, and
60 mAh/g at rated current densities of 100, 200, 300, and
500 mA/g, respectively. For CNS/NiO anode, capacity retention after cycling was much better as shown in Fig. 5b. After
50 cycles, specific discharge capacities were observed to be
902, 759, 482, and 464 mAh/g at current densities of 100, 200,

200

100 mA/g
200 mA/g
300 mA/g
500 mA/g

1400
1200
1000
800
600
400
200
0

0
0

10

20

30

40

50

10

C/NiO
CNS/NiO

1000

40

50

C/NiO
CNS/NiO

400

900
800
700

Z'' (ohm)

Discharge capacity (mAh/g)

30

500

1200
1100

20

Cycle number

Cycle number

600
500
400

300

200

300

100

200
100
0

0.1

0.2

0.3

0.4

C-rate

0.5

0.6

0.7

100

200

300

400

500

Z' (ohm)

Fig. 5 Cycling performance of a C/NiO, b CNS/NiO at different current densities using 1 M LiTFSI/EC:DEC (2:1; v/v) electrolyte, c variation of
discharge capacity with c-rate, and d EIS results of CNS/NiO and C/NiO after 50 cycles at OCV

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Specific capacity (mAh/g)

1400
C/NiO
CNS/NiO

1200
1000
800
600
400
200
0
0

100

200

300

400

500

Cycle number
Fig. 6 Cycling performance of C/NiO and CNS/NiO electrodes at
500 mA/g using 1 M LiTFSI/EC:DEC (2:1; v/v) electrolyte

300, and 500 mA/g, respectively. C-rate performance of the


C/NiO and CNS/NiO is shown in Fig. 5c. Specific discharge
capacities of CNS/NiO anode observed to be higher than the
theoretical capacity of NiO (i.e., 718 mAh/g) at 100 and
200 mA/g current densities. This additional capacity is due
to the lithium storage contributed by CNS. Electrochemical
impedance spectrum (EIS) results of the CNS/NiO and C/NiO
half cells after 50 chargedischarge cycles are shown in
Fig. 5d. Typical two diffused semicircles were observed as
discussed in the previous studies [29], one located in the high
frequency range assigned to the surface film resistance and the
other in medium frequency range corresponding to the charge
transfer resistance. Clearly, the diameter of the semicircle in
Fig. 7 SEM images of a C/NiO
electrode of fresh electrode, b
C/NiO electrode after 50 charge
discharge cycles, c CNS/NiO
electrode of fresh electrode, and
ds CNS/NiO electrode after 50
chargedischarge cycles

medium frequency range for CNS/NiO was found to be smaller than C/NiO. These results indicate that electrical conductivity of the NiO electrode was improved with CNS as compared to the conventional carbon.
Long cycle life was also assessed for the two anodes at
500 mA/g discharging current density, and the results are
shown in Fig. 6. It was found that during the long charge
discharge cycles, discharge capacity varies from 741 mAh/g
for the 2nd cycle to 449 mAh/g for the 500th cycle with
decrease between 50 to 100 cycles and again rising in capacity
after the 100th cycle. This behavior is due to the different
expansion/contraction during the chargedischarge process.
Similar behavior was observed for C/NiO anode, but with
much lower specific capacity values.
SEM analysis of the CNS/NiO and C/NiO anodes after
cycling was carried out to analyze the effect of cycling on
the microstructure of the electrode. SEM results of the CNS/
NiO and C/NiO anodes after 50 cycles are presented in Fig. 7.
SEM samples of the fresh electrode without chargedischarge
cycling were also included for comparison. Figure 7a, b shows
SEM images of fresh and cycled C/NiO electrode. It was
found that after cycling, morphology of the electrode totally
changed and no individual NiO NFs were observed. SEM
micrograms revealed that during cycling, NiO starts
alloying/dealloying around the conductive carbon and forms
interconnected clusters of NiO/C. On the other hand, for CNS/
NiO electrodes, the NiO forms around the highly conductive
interconnected network of CNS and provides excellent lithium alloying/dealloying reaction with NiO and thus retains
high specific capacity. Electrical conductive pathways seem

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volumetric changes. The results also show that the electrical


conductivity of the conductive additives can have a significant effect on the performance of NiO-based anode material.
CNS proves its potential as an efficient framework for reversible electrochemical conversion reactions in anode materials that include volumetric changes.

References
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Fig. 8 Schematics showing the microstructural changes of a C/NiO and


b CNS/NiO electrode after several chargedischarge cycles

to remain more effective in CNS/NiO electrode which leads to


their large specific capacity as compared to C/NiO anode.
A possible schematic of the mechanism of the lithium
conversion reaction in CNS/NiO and C/NiO anode is presented in Fig. 8. After multiple chargedischarge cycles,
NiO NFs lose their shape and morphology and form
microclusters of C/NiO composite as shown in Fig. 8a.
These microclusters keep changing their shape during the
conversion of NiO to Ni and vice versa during the charge
discharge process. This reduces the efficiency of interconnection with the C electrode and each other so that efficient
charge transfer does not occur. This seems to be the most
likely reason for low discharge capacity of C/NiO anode. On
the other hand, CNS/NiO are capable of forming a wellconnected network of CNS and NiO composite which provides efficient charge transfer during the chargedischarge
process and thus shows improved specific discharge capacity compared to traditional C/NiO anode.

Conclusions
The results obtained in this study show the importance of
highly entangled and three-dimensional interconnected network of the CNS as anode material in LIBs. CNS/NiO exhibit improved specific discharge capacity of 450 mAh/g
compared to only 90 mAh/g for conventional C/NiO anode
after 500 cycles. This improved capacity and its retention
after repeated cycling may be attributed to high electrical
conductivity and surface area of CNS. In addition to providing high electrically conductive pathways due to the covalent branching of carbon nanotubes, CNS provide flexible
framework with enhanced electrode stability during the

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