Appl. Phys.
A (2017) 123:697
DOI 10.1007/s00339-017-1293-7
RAPID COMMUNICATION
Surfactant effect on synthesis and electrochemical properties
of nickel-doped magnesium oxide (Ni–MgO) for supercapacitor
applications
B. Saravanakumar1 · S. Muthulakshmi1 · G. Ravi1 · V. Ganesh2 · A. Sakunthala3 ·
R. Yuvakkumar1
Received: 21 July 2017 / Accepted: 1 October 2017
© Springer-Verlag GmbH Germany 2017
Abstract Nickel-doped magnesium oxide (Ni–MgO)
nanopowders were successfully synthesized by employing
a simple sol–gel process by adopting different surfactants
such as Hexamine, CTAB and PEG-400. XRD results clearly
revealed the formation of face centered cubic structure. The
characteristic PL peaks observed at 401, 490 and 552 nm
are owing to charge transfer characteristic in surface state of
the obtained product. The characteristic IR peaks observed
at 445 and 854 cm−1 could be attributed to Mg–O stretch-
ing vibration and the peak appeared at 1036 cm−1 belongs
to Mg–O vibrations modes. Scanning electron microscopy
(SEM) results clearly revealed the uniform distribution of
thin nanolayer morphology in different direction for Ni–
MgO (CTAB) product, the mixture of nanolayer and nano-
particle configurations for Ni–MgO (Hexamine) product and
more agglomerated particle formation for Ni–MgO (PEG-
400) product. The electrochemical studies were carried out
to estimate the specific capacitance of Ni–MgO (CTAB)
product at low scan rate 10 mV/s which showed an excellent
value of 360.5 F/g. The GCD studies for synthesized Ni–
MgO (CTAB) nanolayer morphology have superior specific
capacitance of 96 F/g at 1 A/g with the excellent specific
capacitance. The materials stability for 5000 charging and
* R. Yuvakkumar
yuvakkumar@gmail.com
1
Nanomaterials Laboratory, Department of Physics, Alagappa
University, Karaikudi, Tamil Nadu 630 003, India
2
Electrodics and Electrocatalysis (EEC) Division,
CSIR-Central Electrochemical Research Institute
(CSIR-CECRI), Karaikudi, Tamil Nadu 630003, India
3 mance [2]. The nanoporous material on graphene planes by
Department of Physics, School of Science and Humanities,
Karunya University, Karunya Nagar, Coimbatore,
Tamil Nadu 641 114, India
discharging cycles retains 68% of the specific capacitance
83 F/g at current density of 5 A/g.
1 Introduction
The usage of materials in day-to-day lives of human beings
is inevitable in nature and the demand for new materials for
different applications like solar cells, energy storage devices,
magnetic materials, biosensor, dye degradation effect and
so on is ever increasing [1–3]. Metal oxide nanoparticles
(MO) play a vital role in progressive innovation in designing
and supplying efficient materials for energy storage devices,
magnetic materials, photo catalytic and biosensor applica-
tions [4–11]. Therefore, it is inevitable to understand the
mechanism and formation of corresponding metal oxide
nanoparticles and their electrochemical properties for suit-
able applications. Even though many reports are available
for metal oxide nanoparticles formation ­(MnO2, ­Co3O4, ZnO,
NiO, etc [12–19]) and its electrochemical properties, further
studies to enhance electrochemical properties of metal oxide
based nanoparticles are the need of hour. Very few reports
are available on magnesium oxide-based nanomaterials syn-
thesis and its electrochemical supercapacitor applications.
Geng and his co-workers demonstrated the MgO tem-
plated hierarchical porous carbon sheets derived from coal
tar pitch for supercapacitors applications and achieved
high capacitance of 290 and 250 F g−1 at 1 and 20 A g−1,
respectively [1]. The 2D graphene like hierarchically porous
carbon nanosheets from a nano-MgO template and Z ­ nCl2
activation have been successfully synthesized and studied
for morphology, porosity and super capacitance perfor-
facilitating MgO template for preparing high-performance
supercapacitor electrodes was demonstrated and the specific
13
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697 Page 2 of 9
capacitance of 303 F g−1 with an aerial capacitance up to
17.3 mF cm−2 was achieved [3]. Karthikeyan and his team
have adopted microwave assisted green synthesis method to
blend the MgO–carbon nanotubes composites for electrode
material for high power and energy density supercapacitors
[4]. A mesoporous carbon for supercapacitors from coal
tar pitch by coupling microwave assisted KOH activation
with MgO template has been performed and explored a high
specific capacitance of 224 F g−1 [5]. An investigation on
the MgO decorated few-layered graphene as anode for Li
ion batteries was carried out and revealed a specific surface
area of 393 m2 g−1 along with an average pore volume of
0.9 cm3 g−1 [6].
In the present work, the synthesis and electrochemical
properties of nickel-doped magnesium oxide nanoparticles
in the presence of different surfactants such as Hexamine,
PEG-400 and CTAB by employing a simple sol–gel method
are focused in detail and we studied the surfactant influence
in the material formation mechanism and its electrochemical
properties. Surfactant plays an imperative part in the forma-
tion mechanism and confinement of nanoparticles size and
directly influences the electrochemical properties primarily
depending on contour, configuration, particle size and ori-
entation. The components that greatly impact the electro-
chemical properties of 4d-transtion metal (Nickel) doped
magnesium oxide materials are electrical stability, porous
nature, ability to store charges and path for intercalation of
electrolytic ions into working materials. Though there is a
minimum literature report available on 4d-transtion metal
(Nickel)-doped magnesium oxide for supercapacitor applica-
tion, the present study insists on to investigate nickel-doped
magnesium oxide materials electrochemical behavior and
their results are discussed and evaluated in detail.
2 Materials and methods
In this work, a sol–gel synthesis procedure to obtain
Ni–MgO nanoparticles with different molar concentrations
of precursor was adopted. 95 mM magnesium nitrate hexa-
hydrate (Mg ­(NO3)2·6H2O) and 5 mM nickel nitrate hexahy-
drate (Ni(NO3)2·6H2O) were separately dissolved in 50 ml
mixture of double distilled water and ethanol in the ratio
of 50:50. The dissolved precursor slats were poured into a
beaker and stirred for 30 min to obtain homogeneous solu-
tion. The small amount of CTAB as surfactant was added
to the above solution. In addition, 0.1 M citric acid solution
was added drop by drop to the homogenous precursor solu-
tion under rigorous stirring at 80 °C until the gel formation.
The obtained products were dried in hot air oven at 80 °C
overnight and annealed at 700 °C for 3 h to attain high crys-
talline nature and named as MC. Subsequently, the same
procedure was followed for other two products by adopting
13
B. Saravanakumar et al.
different surfactants namely Hexamine and PEG-400 and
named as MH and MP respectively.
X-ray powder diffraction (X’pert PRO analytical diffrac-
tometer) using Cu Kα as radiation (1.541 Å) source was used
to identify the phase and crystalline nature of the prepared
samples. The optical properties of the obtained product
were measured using Varian Cary Eclipse Photolumines-
cence Spectrometer with Oxford low temperature ­LN277K
setup. Infrared (IR) spectra were recorded using Fourier
transform infrared spectrophotometer using Thermo Nico-
let 380 with resolution 0.5 cm−1 and S/N ratio: 2000:1 ppm
for 1 min scan. The morphology studies were carried out
employing Scanning Electron Microscope (ZEISS- V80).
The CHI6008E instrument with three electrode cell con-
figurations was deployed for electrochemical studies. In a
three-electrode cell setup of electrochemical system, the Ag/
AgCl, platinum wire and Ni–MgO coated on Ni-foam acted
as reference, counter and working electrodes, respectively.
The working electrode was prepared by dissolving Ni-foam
in 3 M HCl for 15 min under ultrasonication to remove the
oxide layer in Ni-foam. Later, slurry was prepared by tak-
ing active material (Ni–MgO), activated carbon (AC) and
polyvinylidene fluoride (PVDF) in the ratio of 80:15:5 with
N-methly2-pyyrolidone (NMP) as a solvent. The slurry was
coated on the Ni-foam of area 1 × 1 cm and dried at 80 °C in
a hot air oven for 12 h. 6 M KOH has been used as electro-
lyte solution for all electrochemical studies.
3 Results and discussion
The X-ray diffraction patterns of synthesized Ni–MgO prod-
uct are shown in Fig. 1a–c. The obtained XRD results clearly
revealed the formation of face centered cubic structure with
lattice parameter a = 4.219 Å and volume of unit cell be
75.14 nm3. The characteristic peaks appeared at diffraction
angles of 36.9°, 42.9°, 62.4°, 74.9° and 78.7° will be readily
indexed to the diffraction planes of (111), (200), (220), (311)
and (222). The indexed planes to the diffraction angles are
well matched with the JCPDS No: 89-7746. The Scherer
formula used for crystallite size determination was given by
the expression: Dp = 𝛽0.94 ×𝜆
, where Dp is the crystallite size,
Cos 𝜃
λ the wavelength of the X-ray, β the wavelength of full width
half maximum and θ the diffraction angle. The clearly dis-
tinct peaks referred to high-quality crystalline formation
with an average crystalline size of sample MC, MH and MP
as, respectively, as 36.63, 26.93 and 36.63 nm.
The observed photoluminescence spectra of synthesized
Ni–MgO product are displayed in Fig. 2a–c. The character-
istic peaks are observed at 401, 490 and 552 nm, respec-
tively, excited at 380 nm wavelength of light from source.
The calculated energy bands employing E = hʋ for ascertain
Surfactant effect on synthesis and electrochemical properties of nickel-doped magnesium…
Fig. 1  XRD pattern of the obtained product a Ni–MgO (CTAB), b
Ni–MgO (Hexamine) and c Ni–MgO (PEG-400)
Fig. 2  Photoluminescence spectra of the obtained product a Ni–
MgO (CTAB), b Ni–MgO (Hexamine) and c Ni–MgO (PEG-400)
wavelength are, respectively, 3.09, 2.53 and 2.24 eV. Gener-
ally, the photoluminescence peaks appeared due to crystal
defects and oxygen vacancy in structural Mg–O nanoparti-
cles. The observed peaks at 401, 490 and 552 nm are owing
to the charge transfer in the surface state of MgO [20].
Figure 3a–c shows the obtained IR spectra of the synthe-
sized Ni–MgO product. In IR spectra, the observed peaks
Page 3 of 9 697
Fig. 3  Infra red spectra of the obtained product a Ni–MgO (CTAB),
b Ni–MgO (Hexamine) and c Ni–MgO (PEG-400)
below 1000 cm−1 belong to characteristics metal oxide
vibrations peak, whereas peaks above 1000 cm−1 belong
to characteristics functional group vibration modes due to
the presence hydroxyl, amide, amines, carboxyl groups, etc.
The peaks observed at 445 and 854 cm−1 can be attributed
to the Mg–O stretching vibration modes [21, 22]. The peak
appeared at 1036 cm−1 belongs to the Mg–O vibrations
[23]. The small peak appeared at 1450 and 2920 cm−1 cor-
responds to presence of scanty amount of OH group in the
synthesized products from ethanol or water absorbed during
the product synthesis.
Generally, the surfactant role in nanomaterial synthesis
plays a vital role in controlling the size and to achieve the
defined morphology in nanometer scale. Especially, in the
present study, different surfactants namely CTAB, PEG-
400 and Hexamine have been adopted to analyse the role
of surfactant in the synthesis process. While using CTAB,
the ­CH3−N+ headed group extended a bound to the parti-
cle surface and it lengthened alkyl hydrophobic chain out-
wards. Similarly, the coordinative saturation dangling bonds
of PEG-400 extend the order chain on the surface of metal
cations which greatly inhibits the growth of Ni–MgO prod-
uct and controls the morphology [24]. In accordance with
hexamine, which acts as a weak base, supplies one hydroxyl
ion per mole and decomposition of hexamine results in the
formation of layer of hydroxyl ion over metal cations and
controls the nanomaterials configuration [25]. Hence, in the
present study, these surfactants have been used and stud-
ied for their influence on the electrochemical properties of
synthesized nanomaterials. The morphology of synthesized
13
697 Page 4 of 9
Ni–MgO product was examined by employing scanning
electron microscopy studies. Figure 4a–c shows the observed
SEM images of the obtained product (a) Ni–MgO (CTAB),
(b) Ni–MgO (Hexamine) and (c) Ni–MgO (PEG-400),
respectively, at 300 nm scales. Figure 4a typically shows the
nanolayer morphology of Ni–MgO formation with CTAB
as surfactant. The observed results clearly revealed the uni-
form distribution of thin nanolayers in different direction.
The formation of nanolayer morphology of Ni–MgO prod-
uct surfaces is sheltered by a layer of CTAB molecules and
Fig. 4  SEM images of the obtained product at 300 nm scale a Ni–MgO (CTAB), b Ni–MgO (Hexamine) and c Ni–MgO (PEG-400)
13
B. Saravanakumar et al.
­CH3–N+ headed group lengthened alkyl hydrophobic chain
outwards [26, 27]. The Ni–MgO product formation with the
assistance of hexamine shows the mixture of nanolayer and
nanoparticles configurations (Fig. 4b). Figure 4c shows the
morphology of the synthesized products with the help of
PEG-400 and observed results clearly revealed the agglom-
eration of Ni–MgO nanoparticles which reflects in its elec-
trochemical properties.
The electrochemical studies of synt hesized
Ni–MgO product were carried out in three electrode cell
Surfactant effect on synthesis and electrochemical properties of nickel-doped magnesium…
configurations in CHI6008E instrument and the active mate-
rial Ni–MgO nanoparticle coated on Ni-foam acted as work-
ing electrode, saturated Ag/AgCl electrode as reference elec-
trode and platinum wire as counter electrode in 6 M KOH
electrolyte solution, respectively. The cyclic voltammetry
study of the obtained product (a) Ni–MgO (CTAB), (b)
Ni–MgO (Hexamine) and (c) Ni–MgO (PEG-400) is dis-
played in Fig. 5a–c.
The observed results exhibit redox peaks on both cathodic
and anodic regions of potential window (0–0.6 V of 6 M
KOH electrolyte solution). The pattern of cyclic voltamme-
try for different scan rates (10–100 mV/s) shows analogous
pseudo-capacitance behavior with an increase in redox
potential and sweep area from 10 to 100 mV/s scan rate. The
specific capacitance can be calculated from cyclic voltam-
metry data by applying the equation ∫ ms (V
I dV
−V )
, where I dV
2 1
Fig. 5  CV studies of the
obtained product a Ni–MgO
(CTAB), b Ni–MgO (Hexam-
ine) and c Ni–MgO (PEG-400).
d Scan rate vs specific capaci-
tance of MC, MH and MP
Page 5 of 9 697
is the integral sweep area by cyclic voltammetry curve, m
mass of the active material coated on Ni-foam, s scan rate
and (V2 − V1 ) stands for applied potential window of elec-
trolyte. The calculated specific capacitance by cyclic voltam-
metry for Ni–MgO (CTAB) product is 360.5, 261.3, 235.1,
177.1, 143.5, 102.0 F/g for scan rate starts from 10 to
100 mV/s represented in Fig. 5a. The specific capacitance
of product Ni–MgO (CTAB) at low scan rate 10 mV/s shows
an excellent value of 360.5 F/g and gets declined as scan rate
amplifies. This is due to the fact that low scan rate allows the
charge carrier (electrons) to access the active sites in the
working electrodes and instigation of the intercalation pro-
cess and migration of ions in electrolyte will be favored. The
cyclic voltammetry for the obtained product Ni–MgO (Hex-
amine) and Ni–MgO (PEG-400) shows the lower specific
capacitance than the obtained product Ni–MgO (CTAB),
13
697 Page 6 of 9
which is due to the mixed structure of nanolayers and nano-
particles and agglomeration of nanoparticles, respectively,
for Ni–MgO product assisted with Hexamine and PEG-400
as correlated with SEM observations. Inappropriate nano-
particle formation of the obtained product Ni–MgO (Hex-
amine) and Ni–MgO (PEG-400) plays vital role in the inac-
cessibility of active sites in working electrode (Ni–MgO
product) and it can be strongly emphasised in the SEM
images. The SEM images clearly encages that the high sur-
face area of Ni–MgO (CTAB) product reflects in the excel-
lent specific capacitance with high current density. Figure 5d
discloses the specific capacitance of all three synthesized
Ni–MgO products (MC, MH, and MP) versus different scan
rates, where Ni–MgO (CTAB) product may facilitate better
specific capacitance which is presumably due to the more
significant nanolayer morphology structure with high sur-
face area and enables the electron in active material to inter-
act with the active sites. The impedance nature of synthe-
sized (a) Ni–MgO (CTAB), (b) Ni–MgO (Hexamine) and
(c) Ni–MgO (PEG-400) was analyzed by electroimpedance
spectra as shown in Fig. 6a–c.
Figure 6 explains the impedance characteristics of the
obtained products MC, MH and MP. The obtained curves
revealed the charge transfer resistance Rct and electrolyte
resistance of synthesized Ni–MgO product at high fre-
quency, where the impedance starts off with the small arc
pattern which reveals the diminutive blocking behavior of
capacitance and then rapidly straighten up at low frequency
and ensures the superior capacitive performance. The
Fig. 6  EIS studies of the obtained product a Ni–MgO (CTAB), b
Ni–MgO (Hexamine) and c Ni–MgO (PEG-400)
13
B. Saravanakumar et al.
estimated solution resistance (Rs) value stands to be as 0.5,
0.82 and 0.63 Ω, respectively, due to the small semi arc at
high frequency. The blocking behavior at low frequency may
be owing to the equivalent distributed resistance (EDR) due
to the nature of the electrode material [28].
Especially for Ni–MgO (CTAB) products, the slopes are
sharper than the Ni–MgO (Hexamine) and Ni–MgO (PEG-
400) products and make certain that it possess the high spe-
cific capacitive character.
Figure 7a–c shows the galvanstatic charging and dis-
charge studies of (a) Ni–MgO (CTAB), (b) Ni–MgO (Hex-
amine) and (c) Ni–MgO (PEG-400) products. The pattern
of charge–discharge curves exhibits the nonlinear behavior
primarily due to the faradic electron transfer than linear
behavior of the electric double layer capacitance signify-
ing that capacitance is essentially due to pseudo-capacitance
[29]. The low specific capacitance of Ni–MgO (PEG-400)
product are primarily due to the fact that the agglomera-
tion of the product obtained disables the charge carrier to
not to reach the active sites and low surface area for charge
transfer mechanism. The charging and discharging patterns
of Ni–MgO (CTAB) product seem excellent specific capaci-
tance for high current density, especially Fig. 7d illustrates
that the superior stability of the materials for 500 cycles of
charging and discharging retains the 92% of specific capaci-
tance for current density of 5 A/g. The specific capacitance
can be calculated by employing the expression, Cs = mI ∇∇ Vt ,
where I stands for the current applied to cathode, ∇ t the dis-
charging time, m mass of the active material and ∇ V is the
potential window applied. The variation of specific capaci-
tance with respect to the current density from 0.5 to 10 A
­g−1 is as shown in Table 1. The GCD studies of synthesized
Ni–MgO nanolayer morphology (MC) have superior specific
capacitance of 96 F/g at 0.75 A/g which have equivalent
and good values with already reported work [4]. We can
claim that the achieved excellent specific capacitance for
Ni–MgO nanolayer morphology (Ni–MgO (CTAB) product)
have remarkable stability of the materials for 500 cycles of
charging and discharging and retains the 92% of specific
capacitance for current density 5 A/g. It should be noted that
even for high current density of 5 A/g, the specific capaci-
tance of 83 F/g are maintained and exhibits the stability of
material which is at 88% of highest specific capacitance
96 F/g at 0.75 A/g current density.
In addition, the galvanstatic charge–discharge studies
were executed for 5000 cycles as shown in Fig. 8. At first,
the remarkable stability of the materials for 500 cycles of
charging and discharging retains the 92% of specific capaci-
tance for current density 5 A/g. After 2000 cycles of charg-
ing and discharging, the specific capacitance starts to fall by
80% and at the end of the 5000 cycles the estimated specific
capacitance remains at 68% of 83 F/g at current density of
5 A/g.
Surfactant effect on synthesis and electrochemical properties of nickel-doped magnesium… Page 7 of 9 697

Fig. 7  GCD studies of the

obtained product a Ni–MgO
(CTAB), b Ni–MgO (Hexam-
ine) and c Ni–MgO (PEG-400)
and d GCD for 500 cycles of
the product MC

The trend of specific capacitance in Galvanstatic charg-

ing and discharging studies is tabulated in Table 1. Specific
Table 1  The details of specific capacitance vs current density capacitance vs current density plot of the obtained product
Ni–MgO (CTAB) is as shown in Fig. 9. The observed results
Product Potential Current Specific
window density capacitance exhibit the high specific capacitance attained at 0.75 A/g
(V) (A/g) (F/g) and then reducing gradually with increase in current density
up to 10 A/g. The discharge curves of Ni–MgO (CTAB)
Ni–MgO (CTAB) product 0.5 0.5 90
product demonstrate the slow rate at the reduction peak of
0.5 0.75 96
materials and enable us an excellent capacitance over other
0.5 1 85
synthesized nanoparticles. The obtained good performance
0.5 2 63
can be attributed to nanolayer morphology of Ni–MgO
0.5 5 83
(CTAB) product obtained which promises high surface area
0.5 10 53
to intercalate and deintercalate on the surface and inner

13
697 Page 8 of 9 B. Saravanakumar et al.

and PEG-400-assisted sol–gel method and achieved the

nanolayer morphology which enables the high surface area
for supercapacitor application. The synthesized nickel-doped
magnesium oxide product’s structural, optical and vibration
properties have been confirmed by standard characteriza-
tions. The electrochemical studies revealed that the specific
capacitance for synthesized Ni–MgO nanolayer morphology
(CTAB) exhibits the excellent value of 360.5 F/g at low scan
rate 10 mV/s. The GCD studies for synthesized Ni–MgO
nanolayer morphology (CTAB) have superior specific
capacitance of 96 F/g at 1 A/g with the excellent specific
capacitance for Ni–MgO nanolayer morphology (CTAB)
and the material stability for 5000 cycles of charging and
discharging retains at 68% of the specific capacitance 83 F/g
at current density of 5 A/g.

Acknowledgements This work was supported by UGC Start-Up

Research Grant No. F.30-326/2016 (BSR).

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