Nano-Structures & Nano-Objects 11 (2017) 102–111

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Nano-Structures & Nano-Objects

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

Nanostructured nickel oxide and its electrochemical behaviour

—A brief review
Rini Paulose, Raja Mohan *, Vandana Parihar
Centre for Advanced Materials Research, School of Engineering and Technology, Jagran Lakecity University, Mugaliyachap, Bhopal—462044, Madhya
Pradesh, India

graphical abstract

article info a b s t r a c t
Article history: This review article summarises few researches that took place on nickel oxide, which is an important
Received 11 May 2017 transition metal oxide in various applications significantly as energy storage material. Nickel oxide is a
Received in revised form 23 June 2017 promising metal oxide and is exhaustively investigated for its electrocapacitive property. Firstly, various
Accepted 4 July 2017
easy and widely used method to prepare or synthesise nickel oxide has been discussed which includes
wet chemical synthesis, sol–gel method, hydrothermal method, microwave assisted route and thermal
decomposition. Then physical properties are reviewed briefly including its structural, magnetic, electrical
Keywords:
Nanostructures and optical properties. Finally, the electrochemical behaviour of nickel oxide and nickel oxide based
Metal oxide composite has been discussed.
Nickel oxide © 2017 Elsevier B.V. All rights reserved.
Electrochemical behaviour
Energy storage

Contents

1. Introduction....................................................................................................................................................................................................................... 103
2. Synthesis methods of NiO nanoparticles......................................................................................................................................................................... 103
2.1. Sol–Gel method .................................................................................................................................................................................................... 103
2.2. Wet chemical synthesis ....................................................................................................................................................................................... 103
2.3. Hydrothermal method ......................................................................................................................................................................................... 103
2.4. Solid-state thermal decomposition..................................................................................................................................................................... 104
2.5. Microwave method .............................................................................................................................................................................................. 104
2.6. Other methods...................................................................................................................................................................................................... 104

* Corresponding author.
E-mail address: drmraja@jlu.edu.in (R. Mohan).

http://dx.doi.org/10.1016/j.nanoso.2017.07.003
2352-507X/© 2017 Elsevier B.V. All rights reserved.
 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111 103

3. Physical properties of nickel oxide .................................................................................................................................................................................. 104

3.1. Structural properties ............................................................................................................................................................................................ 104
3.2. Magnetic properties ............................................................................................................................................................................................. 105
3.3. Electrical properties ............................................................................................................................................................................................. 105
3.4. Optical properties................................................................................................................................................................................................. 105
4. Electrochemical behaviour of nanostructured nickel oxide and nickel oxide based composite................................................................................. 105
4.1. Nickel oxide .......................................................................................................................................................................................................... 105
4.1.1. Factors affecting electrochemical behaviour ...................................................................................................................................... 106
4.2. NiO based composite material ............................................................................................................................................................................ 107
5. Summary ........................................................................................................................................................................................................................... 109
Acknowledgement ............................................................................................................................................................................................................ 109
References ......................................................................................................................................................................................................................... 109

1. Introduction 2. Synthesis methods of NiO nanoparticles

Nanostructured metal oxides have gained considerable atten-
tion for electrochemical applications. Metallic nanoparticles with
optimum morphology, higher surface area, and specific optical,
magnetic, electrical and mechanical properties attracted several
researchers for attaining excellent electrochemical performance.
Electrochemical process involve physical interaction/chemical re-
action at the surface or interface, so specific surface area, surface
energy and surface chemistry play important role. Hence smaller
dimensions of nanoparticles offer large surface area for faradaic
reactions and small distance for mass, heat and charge transfer [1].
Transition metal oxide show a high theoretical and are inexpensive
with high abundance and low toxicity [2,3]. Several metal oxides
have been studied for electrochemical performance which includes
manganese oxide, ruthenium oxide, cobalt oxide, tin oxide, nickel
oxide and ferrous oxide.
Among other transition metal oxide, Nickel oxide (NiO) have
shown good electrochemical performance [4,5] and also have
gained considerable attention in past few years due to its mag-
netic, mechanical, electronic and optical properties and have been
used as smart windows, supercapacitor, electrode, catalyst and
electrochromic device [6,7]. Nickel oxide is a wide band stable
p-type semiconductor with band gap ranging from 3.6–4.0 eV [8].
It also exhibits electrochemical stability, anodic electrochromism,
large spin optical stability, excellent durability and various man-
ufacturing possibilities. Nickel oxide has high theoretical specific
capacitance of 2584 F/g in potential window of 0.5 V [9]. Liu
and Anderson prepared porous NiO and reported specific ca-
pacitance of 50–64 F/g for the first time in 1996 [10]. It pos-
sesses multiple oxidation state which favour fast redox reactions
— resulting in high specific capacitance. Practically nickel ox-
ide tend to have low electronic conductivity so they are com-
bined with other components that have increased its conductivity
such as CNT, graphene and metal oxides, reporting capacitance of
some NiO composite. At room temperature, NiO have resistivity
in the order of 1013  cm [11]. Its resistivity can be lowered
by doping with monovalent ions [12]. Nickel oxide have been
synthesised in various morphological structures like nanoflakes,
nanosheet, nanoflower, nanoball, nanowire, nanorod, nanotube,
nanoneedle and nanospheres by employing various synthesising
techniques like wet chemical synthesis, hydrothermal method,
sol–gel method, thermal decomposition method, microwave
method and many others. The basic synthesis techniques have
been briefly discussed in this review paper. Also, there is brief
summary of the physical properties of nickel oxide including its
structure, optical, magnetic, and electronic properties. The main
focus of this review paper is to study electrochemical behaviour
of nanostructured nickel oxide. Here we have provided with elec-
trochemical behaviour of pure NiO and NiO based composite, re-
porting few researchers work.
Nanoparticle applications do not depend only on properties
(size, morphology and structure) but also in the method of syn-
thesis employed. There are several methods to synthesise NiO
nanoparticles which determine its physiochemical properties and
which in turn determine its electrochemical property as well. Here
are given brief review on synthesis methods of NiO nanoparticles.
2.1. Sol–Gel method
Sol–Gel method involves preparation of sol, successive gela-
tion followed by removal of solvent. It is very useful and easy
method to produce nanostructures wherein precursors are ho-
mogeneously mixed in solvent to form an integrated continuous
network of liquid phase (gel) which are then heat treated to form
nanoparticles, controlling its morphology, shape and size. Yang
et al. synthesised NiO nanowire employing sol–gel method [13].
L. Gaik and K.D. Li [14] synthesised spherical NiO nanoparticle
using Sol–Gel method where nickel nitrate hexahydrate was added
to an ethanolic solution of non-ionic copolymer F108 and result-
ing sol solution was dried and calcined at various temperatures
Fig. 1a. Nurul et al. presented sol–gel method in which nickel oxide
nanoparticles were obtained using alcoholic solution of nickel
nitrate hexahydrate dissolved in polyethylene glycol [15]. In work
done by P. Jeevanandam and V.R.R. Pulimi [16], NiO nanocrystals
were synthesised by dropwise addition of alcoholic solution of
NaOH to nickel nitrate hexahydrate solution prepared in absolute
ethanol.
2.2. Wet chemical synthesis
Precipitation methods are easy to implement and useful to
synthesise nanomaterials in large scale. It requires precursors and
precipitating agents and the reaction is fast due to which con-
trolling of morphology of the nanoparticles of metal oxides is a
major challenge. Xu et al. [18] synthesised NiO nanowires by wet
chemical route. A. Rahdar et al. [19] employed co-precipitation
method for the synthesis of nanocrystalline NiO, using nickel
chloride hexahydrate and NaOH as starting material. A.J. Ahamed
et al. synthesised spherically grain shaped NiO using nickel nitrate
hexahydrate [20]. Fig. 1b shows FESEM image of nanocrystalline
NiO synthesised using wet chemical synthesis.
2.3. Hydrothermal method
Hydrothermal method is a heterogeneous reaction occurring in
presence of aqueous solvents under high temperature and pressure
conditions to synthesise or recrystallise nanomaterial [21]. It is
very useful method, here reaction temperature, pH, pressure can
be controlled to obtain high purity nanostructured NiO. Some
researchers demonstrated hydrothermal method for synthesising
104 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111

Fig. 1. (a) TEM image of Microstructure NiO via sol–gel method. (b) FESEM image porous nanocrystallineNiO prepared using homogeneous precipitation method. (a)
Reprinted with permission from Ref. [14], Copyright 2012, JIM; (b) reprinted with permission from Ref. [17], Copyright 2015, Elsevier.

Fig. 2. (a). SEM image of NiOnanoflakes prepared using hydrothermal route, (b). FESEM image of flower like NiO prepared via Microwave method, (c). SEM image of NiO
nanoparticles obtained via solid state decomposition. (a) Adapted with permission from Ref. [26] Copyright, 2008 Elsevier; (b) adapted with permission from Ref. [27]
Copyright, 2011 American Chemical Society; (c) adapted from Ref. [28].

NiO including Changyu Li and Shouxin Liu [22], they have prepared
mesoporous nanosheets nickel oxide by the addition of NaOH in
the mixture of nickel nitrate hexahydrate and SDBS, carried out in
autoclave at 140 ◦ C for 24 h. The obtained β -Ni(OH)2 was calcined
at 400 ◦ C to obtain NiO in form of nanosheet. Employing same
method, L. Wang and co-workers [23] produced NiO microspheres
using nickel chloride hexahydrate and ammonia with glucose;
also NiO nanoplates were obtained for same method, without
glucose. Various other synthesis using hydrothermal method were
reported which includes NiOnanobelts [24], NiOnanorods and
nanoworms [25]. Fig. 2a depicts the SEM image of NiOnanoflakes
synthesised using hydrothermal method.
2.4. Solid-state thermal decomposition
Thermal decomposition is easy method for synthesising
nanoparticles by oxidising the solid material in an optimum
temperature. M.S. Niasaria obtained single phase NiO nanoparti-
cles by the solid state decomposition of nickel-o-phthalate com-
plexes [29]. Utilising this method, A. Barakat and co-workers [28]
prepared spherical NiO nanoparticle by thermal decomposing (2,9-
dimethyl-1,10-phenanthroline)NiCl2 complex precursor at 400 ◦ C
Fig. 2c. In similar work done by Zhang and co-workers [30] pre-
pared grain sized NiO from heating the mixture of nickel acetate
tetra hydrate and oxalic acid at 500 ◦ C for 1 h.
other methods such as higher efficiency, nanoparticle rapid forma-
tion, and narrow crystalline size distribution and agglomeration
diminution [31]. Employing this method Meher et al. [27] syn-
thesised porous ball like NiO nanostructure depicted in Fig. 2b,
NiO nanoflakes obtained by S. Vijay kumar et al. [32], and X. Song
and L. Gao [33] synthesised NiO nanorods. NiO nanoparticles were
easily synthesised using microwave assisted route by microwave
irradiation of nickel hydroxide prepared from nickel precursor and
hydroxide solution [34].
2.6. Other methods
Apart from easy approach like sol–gel method, precipitation
method, microwave method, hydrothermal synthesis, and ther-
mal decomposition, there are several other methods to syn-
thesise nanocrystalline NiO which includes anodic arc plasma
method [35], reduction method [36], electro-deposition method
[37], template method [38], solvothermal method [39] and so on.
Yet new facile route of synthesis are authors concern to obtain
smaller dimension of particle size with higher surface area.
Widely used synthesis methods for nanostructured NiO with
varying particle size has been summarised in Table 1.
3. Physical properties of nickel oxide

2.5. Microwave method 3.1. Structural properties

Microwave method provides extremely rapid kinetics of syn- Morphology and particle size have significant effect on the
thesis. Microwave heating method has various advantages over capacitance. Smaller the size of particle more will be the
 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111 105

Table 1
Pure NiO obtained via various methods and their particle sizes.
Synthesis method Morphology Particle size (nm) Surface area Ref.
(m2 /g)
Sol–gel Nanoflake 20–30 7 [14]
Sol–Gel Nanoparticle ∼19 322 [16]
Sol–Gel Nanoparticle 18 – [40]
Sol–Gel Nanoparticle 33 – [15]
Chemical precipitation Nanosheet ∼2 377 [16]
Chemical precipitation Nanoparticle 25–65 – [41]
Chemical precipitation Nanoparticle 24 – [19]
Chemical precipitation Nanosheet 16 108 [17]
Solid state thermal decomposition Nanoparticle 8 – [42]
Solid state thermal decomposition Nanosphere 16 – [28]
Solid state thermal decomposition Nanoparticle 5–15 – [43]
Solid state thermal decomposition Nanoflake 76 – [30]
Reduction Nanoflake 12 – [44]
Microwave Nanoparticle 19 – [34]
Microwave Nanoparticle 20 – [45]
Microwave Nanoflower 5 125 [27]
Microwave Nanocrystal 35 – [30]
Hydrothermal Nanoparticle 96 – [46]
Hydrothermal Nanoflake 50–80 – [26]

other, successive planes having ordered moments are antiparallel

which is type II antiferromagnetism. Ni-O–Ni bonds are antiferro-
magnetic in this way. Above the Neel temperature, in paramagnetic
phase, NiO has a rock-salt crystal cubic structure [59].

3.3. Electrical properties

The electrical conductivity of NiO depends on microstructural

defects such as nickel vacancies and interstitial [60]. Electrical
properties are influenced by the size of nanoparticle. Bigger grain
results in less grain boundaries which effect electrical conductivity
as scattering effect at grain boundary is reduced.

Fig. 3. XRD pattern of NiO nanoparticles. 3.4. Optical properties

Source: adapted from Ref. [35]
conductance. Porosity and surface area is closely related to the
morphology. High surface area and porosity leads to the easy
diffusion of ions which in turn leads to high capacitance. NiO are
obtained in various structural forms which includes nanoparticle
[47], nanoflakes [48], nanowire and nanodisks [49], nanoflower
[50], nanosheet [51], nanoball [52], nanorolls [53], nanowalls [54],
nanorods [55], nanobelt [56] and so on.
Crystallinity plays a crucial role in pseudocapacitance of elec-
trode material. It has been reported that electrode materials with
low crystallinity exhibit large capacitance as it provides more
diffusion channels for electrolyte ions [57]. The phase crystallinity
and purity of NiO are examined using X-ray diffraction technique
which gives peaks indexed at (111), (200), (220), (311), and (222)
crystal planes and all these peaks are indexed to face-centred cubic
crystalline structure where its peak position and intensity should
be in accordance with standard spectrum (JCPDS No. 04-0835).
Fig. 3 shows the typical XRD pattern for NiO nanoparticles.
3.2. Magnetic properties
Magnetic nanoparticles are widely used in rechargeable batter-
ies, conducting paints, optoelectronics, chemical catalyst, magnetic
recording media, magnetic resonance imaging, drug delivery and
ferro-fluids. There is a difference between physical properties of
bulk and nanoparticles [58]. Nickel oxide exhibit magnetism as
bulk material. It particular undergoes antiferromagnetic ordering
transition at Neel temperature T N = 523 K, here Ni-ions planes
perpendicular to (1,1,1) align its magnetic moment parallel to each
The band gap for NiO is 3.6–4.0 eV [61]. The energy gap of semi-
conductor decreases with the increase of grain size of nanoparti-
cle. This was demonstrated by various authors. S. Sriram and A.
Thayumanavan [62] obtained optical band gap for the NiO film
sample as 3.6 eV which got decreased for aged sample due to
the increase in grain size. Similar work done by S.A. Mahmoud
and co-workers [63] reported that on increasing the calcination
temperature of NiO thin films from 225 to 350 ◦ C, the band gap
decreases from 3.84 and 3.14 eV.
4. Electrochemical behaviour of nanostructured nickel oxide
and nickel oxide based composite
4.1. Nickel oxide
The pseudocapacitance of nickel oxide nanoparticle has been
investigated by many researchers using cyclic voltammetry (CV)
technique. Cyclic voltammetry is method in electrochemistry
which measures current as function of potential. CVs involve re-
sponse of nanomaterial to varying voltage at various scan rates.
It determines electrode reaction mechanisms, standard electron
transfer rate constants, and also diffusion coefficients [64]. CVs are
recorded using three electrodes, one is working electrode prepared
with electroactive material, second is reference electrode and
third is counter electrode. The working electrode provides surface
for redox or faradaic reaction to take place, reference electrode
provides calibration for applied potential and counter electrode
which is generally Pt wire that conduct electricity from source.
Working electrode play vital role in supercapacitors, so increasing
106 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111
Fig. 4. (a) CV voltammogram for NiOnanoflakes, (b) Charge–discharge cycle for same sample, (c) Discharge curves for NiO prepared via microwave method and (d) reflux
method at different current densities, (e) Specific capacitance v/s potential for NiO prepared via solvothermal method, (f) CV voltammogram for NiO prepared via template
method. (a&b) adapted from Ref. [72]. (c&d) adapted with permission from Ref. [27]. Copyright 2011, American Chemical Society, (e) Adapted with permission from Ref. [73].
Copyright 2007, Springer, (f) Adapted with permission from Ref. [52] Copyright 2004, Elsevier.
the surface area of the working electrode, increases the capaci-
tance and the availability of pores allow easy flow of electrolyte
through it. Porous electrode material which matches with the size
of electrolyte ion improves the capacitance [65]. Capacitance of the
electrode material is calculated from cyclic voltammogram using
formula:
i
C =
Sm
where, C is the capacity of the working electrode, i is the average
current of anode and cathode curves at zero potential on the x-axis,
S is the scan rate and m is the mass of electroactive material [66].
The electrochemical properties of any electrode material rely on
its morphology and particle size owing to larger surface area, pore
size distribution, ion permeability and electrolyte wetting.
4.1.1. Factors affecting electrochemical behaviour
Surface area and pore size. Surface area is analysed by Brunauer–
Emmett–Teller method. Capacitance according to Eq. (1) is propor-
tional to electrode/electrolyte surface.
εS
C =
d
where ε is dielectric constant and d is thickness of the electric
double layer. Hence, increasing the surface area increases the ca-
pacitance value. And the pores which are larger in size compared
to ions increase storage efficiency and capacitance. The pores of
electrode matching the size of electrolyte ions improve the ca-
pacitance. Porous electrode material have significant effect on the
capacitance as it provides feasible accessibility of electrolyte ion for
faradaic or redox reactions in energy storage application. Porosity
distribution in the sample is analysed by Barrett–Joyner–Halenda
method. The capacitance behaviour can be improved with the pore
size in the range of 2–5 nm as it provides unhindered diffusion of
ions in inner matrix [67].
Electrolyte. Performance of capacitor strongly depends on type of
electrolyte used. Aqueous electrolytes in its concentrated solution
have higher conductivity and low viscosity and it tend to produce
faster charge and discharge rate and is most commonly used for
the NiO based electrode [68]. The most common electrolyte used
NiO based capacitor is KOH. Also, the cost and manufacturing of
aqueous electrolyte is lower compared to other electrolytes.
Electrical conductivity. The pseudocapacitance strongly depends
on the charge–discharge rates and resistance. At high charge–
discharge rate, material with low conductivity have more pro-
nounced resistance to electron conductance as charge–discharge
process will take place in a finite volume near current collector,
decreasing its capacitance (Cs) value and making it inefficient for
high power systems [69,70].
Mass of electrode material. Electroactive material loaded on sub-
strate should be low; as capacitance value decrease on increasing
the loading mass. With thicker mass loading, electrolyte finds
it difficult to access all inner active surface areas of electrode,
consequently capacitance value decreases.
The reaction involved in the redox process of nickel oxide in
alkaline solution, NiO + OH− →NiOOH + e− , and then the oxyhy-
(1) droxide participates in the following reversible redox process [71].
Various researches carried out for studying electrochemical be-
haviour of nickel oxide.
Wang et al. [72] prepared wave like NiO flakes via immersion
method and carried out charge – discharge process and cyclic
voltammetry at different scan rates. It was found that lower current
enhances the capacitance of nickel oxide and the specific capaci-
tance calculated from discharge curves are 525, 455 and 380 F/g
at current 5, 10 and 20 mA. Cyclic voltammetry results showed
capacitance of 628 and 586 at scan rate of 1 mV/s and 2 mV/s
respectively shown in Fig. 4a&b slow scan rate and lower were
attributed for the excellent capacitance of nickel oxide. Meher
et al. [27], synthesised porous ball like NiO via microwave method
using Ni(NO3 )2 .6H2 O as precursor and flower like NiO via reflux
 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111 107

Table 2
Structural parameters with synthesis and capacitance of some published results of NiO.
Morphology Synthesis Particle Pore Surface area Electrolyte Specific No. of Retention Ref.
method size (nm) size (nm) concentration capacitance cycles capacity (%)
NiO nanoflakes Immersion – – – 3 M KOH 525, 485, 380 200 91.2% [72]
method F/g at 5, 10, 20
mV/s
NiO porous a. Microwave 5 1.9, 3, 3.7 125.2, 1 M KOH 598, 576, 541 400 97.27% at [27]
ball-like method 167 m2 /g F/g at 5, 10, 20 4.0 Ag−1
mV/s
NiO-flower like b. Reflux 4 ∼1.8, 14.9 0.22, 0.23 cm2 /g 1 KOH 388, 313, 400 60% at
method 247 F/g 4.0 Ag−1

NiO Solvo thermal 7–15 – – 1 M KOH 200 F/g – – [73]

nanospheres process
2
NiO nanoballs Precipitation 300 5.0 477.7 m /g 3% wt KOH 124 F/g – – [52]
NiOnanoflakes Hydrothermal 50–80 – – 2 M KOH 137.7 F/g 1000 91.6% [26]
method
NiO nanoparticles a. Microwave 35 – – 6 M KOH 186 F/g 1000 91.4% [75]
method 76 6 M KOH 97 F/g 1000 76.7%
b. HTSS
NiO Liquid phase 20 – – 6 M KOH 300 F/g – – [74]
nanoparticles process
2
NiOnanospheres Phase reaction 60 – 27 m /g 1 M KOH 22.20 F/g at 50 – – [66]
mV/s
17.29 F/g at 100
mV/s
NiO nanotube Ni-precursor- 450–550 2–10 98 m2 /g 2M KOH 960 F/g 1000 98.8% [76]
nanosheet polymeric
nanotubes
composite was
Calcinated
Hierarchical Dispersing ∼100 2–4 62 m2 /g 2M KOH 415 F/g 1000 91% [51]
NiO nanosheet sPSHSs with
Ni(NO3 )2 .6H2 O
and urea
followed by
heating
NiO nanowires Electrospinning 10–20 11.5 14 m2 /g 6M KOH 746 F/g at 1 3000 85% [77]
mV/s
NiOnanosheets Solvothermal 30–40 23 24 cm2 /g 1M LiPF6 400 mAh g−1 100 98% [78]
and thermolysis
NiO films Chemical spray – – – 2M KOH 405 F/g 1000 92.1% [79]
pyrolysis
NiOnanowalls Electrochemical 20 – – 1M LiPF6 721 mAh g−1 – – [80]
corrosion

method. The obtained NiO sample from microwave method and
reflux method showed specific capacitance of 598, 576, 541 F/g
and 388, 313, 247 F/ g respectively at same scan rate 5, 10 and
20 mV/s shown in Fig. 4c&d. They demonstrated that the loss of
only 9.5% in specific capacitance took place at 20 mV/s, thus having
higher current response. They also reported that the low scan rate
improves the specific capacitance as both outer and inner pore
surfaces are utilised for OH− propagation. Also, NiO exhibit longer
discharge time with specific capacitance of 420, 399, 372, and
337 F/g at scan rate 0.5, 1.0, 2.0, and 4.0 mV/s respectively. Wang
et al. [23] synthesised NiO microspheres by hydrothermal method.
The electrode prepared using this NiO sample showed a linear
potential variation v/s time for charge–discharge curve making it
ideal for energy storage devices. Nathan et al. [73] prepared single
phase nanostructured nickel oxide via solvothermal method. The
cyclic voltammetry conducted gave maximum capacitance of 200
F/g shown in Fig. 4e. Xing et al. [52] prepared mesoporous nanoball
NiO using template method using NiCl2 .6H2 O as precursor and
sodium dodecyl sulphate as template. The capacitance obtained
for samples obtained at 250, 300 and 350 ◦ C is 124, 106 and 68
F g−1 1, respectively shown in Fig. 4f. They concluded that with
the increase in calcination temperature increases the capacitive
behaviour. Zhang et al. [74] reported specific capacitance of 300
F/g at sweep rate 5 mV/s. Zheng et al. [26] utilising hydrothermal
method for NiO nanoflakes synthesis have attained capacitance of
137.7 F/g with retention of 91.6% over 1000 cycles. Zhang et al. [75]
employed solid state decomposition and microwave method to
obtain nanocrystalline NiO with capacitance of 97 and 186 F/g. Xu
et al. [76] prepared NiO nanotube with thin nanosheet had capac-
itance 960 F/g at end of 1000 cycles with 98% capacity retention.
NiO nanosheet hollow spheres prepared by Ding et al. showed
capacitance of 415 F/g with 91% retention [51].
Table 2 reports the data about the morphology of NiO and its
synthesis, its structural parameter, electrolyte used, capacitance
obtained and its retention capacity.
4.2. NiO based composite material
Nanocrystalline nickel oxide have high theoretical capaci-
tance of 2584 F/g but its electrical conductivity is less than
10−13 −1 cm−1 [81], limiting its charge–discharge rates and
power performance of electrode material for high power applica-
tions [82,83]. Pure NiO, however have relatively poor conductivity
and low accessible area and so it delivers poor rate capability and
reversibility during the charge/discharge process [84]. The com-
posite have benefits of both pseudocapacitive behaviour of metal
oxide and also carbon material. NiOcomposite material synergis-
tic effects have shown impressive electrochemical performance
108 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111

Fig. 5. (a) SEM image of nickel–cobalt oxides/CNTs/graphite electrodes. (b) Cyclic stability of nickel–cobalt oxide/CNTs/graphite electrode. (c) FESEM image of pure
NiCo2 O4 /SWCNT. (d) Specific capacitance v/s discharge current for NiCo2 O4 /SWCNT. (e) SEM image of 3D graphene on Ni foam. (f) Specific capacitance v/s scan rate for
NiO nanoflake-3D graphene composite (NGC). (g) SEM micrograph of graphene sheet/porous NiO hybrid film. (h) Cycling performance of the graphene sheet/porous NiO
hybrid film. (i) FESEM image of NiO:RGO. (j) Cyclic performance of NiO:RGO. (k) SEM image of RG-O/NiO. (l) Specific capacitance of RG-O/NiO composites at various scan
rates. (m) SEM image of NiO/MWCNTS. (n) Specific capacitance with charge–discharge cycle number of NiO/MWNTs composite. (a&b) Reprinted with permission from
Ref. [90], Copyright 2006, Elsevier, (c&d) reprinted with permission from Ref. [91], Copyright 2012, American Chemical Society, (e&f) reprinted with permission from Ref. [99],
Copyright 2014, Wiley, (g&h) reprinted with permission from Ref. [100], Copyright 2011, Wiley, (i&j) reprinted with permission from Ref. [101], Copyright 2012, Elsevier,
(k&l) reprinted with permission from Ref. [98], Copyright 2011, Elsevier, (m&n) reprinted with permission from Ref. [102], Copyright 2006, Elsevier.

and have pave way for promising electrode material for energy
storage systems. NiO have been successfully combined with single
walled carbon nanotubes (SWCNTs), multi-walled carbon nan-
otubes (MWCNTs), activated carbon, graphene and other transition
metal oxides. CNT have got great deal of attention due to its unique
pore structure, superior electrical properties, good mechanical and
thermal stability [85,86]. Among all electrode material, graphene
has higher specific area of 2630 m2 /g which can be fully utilised
to achieve higher capacitance; also it is chemically stable [87,88].
Activated carbon is widely used as electrode material because of
its large surface area, good conductivity and moderate cost but
compared to other electrode material, activated carbon show low
conductance [89]. Also metal oxides offer high specific capacitance
and low resistance, making it an efficient electrode material, also it
introduce impurity band effects and enhance the performance. Fan
et al. have used binary oxides constituting nickel oxide and cobalt
oxide which are formed by thermally decomposing their respective
precursors on the CNT/graphite surface [90]. They have reported
that Ni–Co/CNT have more capacitance than Ni/CNT and Co/CNT.
Capacitive properties of NiO/CNT composite has been improved
by incorporation of cobalt oxide with specific capacitance of 569
F/g. CNT provides large surface area that have improved the Ni–
Co oxide electrochemical performance provided with high charge–
discharge cycle stability compared to other low cost transition
metal oxides. In another work done by Wang et al. [91] formed
Ni–Co oxide on SWCNTs bundles and have reported high capac-
itance and excellent retention of 94.1% after 2000 cycles. Use of
SWCNT showed enhanced cycling stability and moreover it helps
to reduce interfacial resistance [92]. Nickel oxide has also been
coupled with MWCNT by many researchers and it have considered
 R. Paulose et al. / Nano-Structures & Nano-Objects 11 (2017) 102–111 109

Table 3
NiO based composite and its capacitance from some published papers.
NiO based composite Specific capacitance Current density No. of cycles Retention capacity (%) Ref.
(F/g) (A g−1 )
Ni–Co oxide/CNT 569 10 2000 96.4% [90]
NiCo2 O4 -p3 SWCNT 1642 20 2000 94.1% [91]
NiO-nanoflake 3D graphene ∼1829 3 - - [99]
Hierarchical composite (NGC) 980 15 5000 85%
NiO porous hybrid film/graphene sheet 400 2 2000 94% [100]
RGO–NiO 576 1 1100 [101]
RG-O/NiO ∼700 0.2 1000 96% [98]
NiO/activated carbon 194.01 – - – [103]
NiO/MWCNTs 170 2 200 89% [102]
ERGO/NiO 1715.5 2 2000 78.8% [104]
Nickel–manganese oxide 407 1 1000 98.4% [105]
NiO-GNS/PANI (graphene/polyaniline) 1409 1 2500 92% [106]
Cu/NiO 296.2 – 500 97% [107]
Co3 O4 -NiO 687 0.5 2500 92% [108]
NiO–Co3 O4 1250 10 5000 98% [109]
Ni-Zn-Co oxide 776 2 10,000 88.9% [110]

as potential candidate as electrode material [93] because of its
unique entangled network , electrical conductive properties and
dominant porous character [94,95]. These entangled structures
provide easy transport of electrolyte ions and also it eliminates
diffusion hindrance. Nickel oxide has been extensively investigated
with graphene and has emerged with excellent capacitive prop-
erty. Reports on NiO–graphene composite claims to have achieve
high capacitance due to its two dimensional plane structure with
one atom thickness, ultra high specific surface area (up to 2630
m2 g−1 ) [96] as well as extraordinary electrical, thermal, physical
and chemical properties comparable or even better than CNT [97].
Also it was found that restacking of graphene ensembles and
agglomeration can be avoided or decreased by loading fine metal
oxide and consecutively it provides higher electrochemical active
surface area, for high electrochemical performance [98].
Fig. 5 illustrates various morphology of NiO based composite
material with its electrochemical behaviour and Table 3. sum-
marises the data reported in literature about the composite ma-
terial, its Cs values and its retention capacity.
5. Summary
We have evaluated NiO as an electrode material, discussing its
fundamental methods of synthesis and various physical properties.
The capacitance is greatly influenced by morphology, particle size,
pore properties and surface area. It has high theoretical capacitance
but yet suffers low conductivity. To overcome the poor conduc-
tivity and to improve its cycling stability, nickel based composite
were formed, enhancing its synergistic effect and increasing its
Cs value, charge–discharge cycling stability and rate capability.
Potential of NiO need to be exploited to obtain all its benefits.
Optimising its structural parameters and synthesis methodologies
is a primary challenge now.
Acknowledgement
This work is supported by Department of Science and Technol-
ogy (DST)-India for the financial assistance under the Early Career
Research (ECR) Award Ref: ECR/2015/000143.
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