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International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963

SYNTHESIS, SENSING AND MAGNETIC PROPERTIES OF
POLYANILINE / NICKEL OXIDE NANOCOMPOSITES
Jakeer Husain1, Chakradhar Sridhar B2, M.V.N.Ambika Prasad1*
1

Department of Materials Science Gulbarga University Gulbarga.585106 Karnataka, India.
2
Department of Physics Gulbarga University Gulbarga.585106 Karnataka, India.

ABSTRACT
Nickel oxide Polyaniline nanocomposites were synthesized by in-situ polymerization technique. The formation of
nanocomposites was characterized by employing .X-ray diffraction (XRD), infrared (IR) spectroscopy, and
scanning electron microscopy (SEM). The crystallite size of nickel oxide was found to be 28.83 nm as indicated
by XRD. The sensing properties of these composite are studied at room temperature by using two probe method.
It is observed that the sensitivity increases with the addition of nickel oxide nanoparticles in polyaniline
nanocomposites .The synthesized nanocomposites shows good sensing and magnetic properties. The obtained
nanocomposites are used in making of Sensor and magnetic devices.

KEYWORDS: Polyaniline, nanocomposites, sensitivity, XRD, SEM, FT-IR

I.

INTRODUCTION

Composites containing inorganic particles have attracted great attention due to their different
properties through doping, polyaniline is the most widely studied because of its ease to synthesis, low
density, less cost, soluble in various solvents, good processibility and good conductivity[1- 5].
Polyanilne has also been used in many applications such as, chemical & biosensors, electromagnetic
interference (EMI) shielding electro-catalysts, light -emitting diodes (LEDs), corrosion devices and
microwave absorption devices, rechargeable battery and potential application in many fields. [69].Nickel oxide is one of the important metal oxide prepared by different methods like, combustion,
sol-gel, Hydrothermal and solvent thermal technique. Among these, combustion technique has
received considerable attention, based on their interesting properties and applications in gas sensor
device, Magnetic storage devises ,catalysis and ferrofluids[10-14].In recent years, the preparation of
polyaniline composites by doping inorganic particles has shown great interest [15].In the present
paper nickel oxide nanoparticles were synthesized by combustion method. The synthesized product
is characterized by employing X-ray diffraction (XRD), infrared (IR) spectroscopy, and scanning
electron microscopy (SEM). Their sensing properties are also studied at room temperature by using
two probe method.

II.

EXPERIMENTAL

2.1. Synthesis of nickel oxide nanoparticles
The nickel oxide nanoparticles were synthesized by self-propagating low temperature combustion
method, employing nickel oxalate as precursor. Precursor is prepared by dissolving equimolar
quantity of Nickel chloride and oxalic acid in distilled water. This solution is stirred for ½ hour on
magnetic stirrer. Light green precipitate of nickel oxalate dehydrate so obtained is filtered and
washed with distilled water. The prepared Nickel Oxalate was mixed with Polyethylene glycol (PEG)
in the weight ratio 1:5. The resultant compound was placed in a crucible and heated in air by using
electrical heater it was observed that initially PEG is melted, then frothed and finally ignited to give
nickel oxide as a residue, then the prepared compound was then calculated for 2 hours to remove
impurities. Finally pure nickel oxide nanoparticles were obtained.

620

Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963
2.2 Preparation of Polyaniline/nickel oxide nanocomposites
Synthesis of the PANI– nickel oxide nanocomposites was carried out by in-situ polymerization
method. Aniline (0.1 M) was mixed in 1 M HCl and stirred for 15 min to form aniline hydrochloride.
Nickel oxide nanoparticles were added in the mass fraction to the above solution with vigorous
stirring in order to keep the nickel oxide homogeneously suspended in the solution. To this solution,
0.1 M of ammonium persulphate, which acts as an oxidizer was slowly added drop-wise with
continuous stirring at 5◦C for 4 h to completely polymerize. The precipitate was filtered, washed with
deionized water, Acetone, and finally dried in an oven for 24 h to achieve a constant mass. In these
way, PANI– Nio2 nanocomposites containing various weight percentage of Nio2 (10 %, 20 %, 30 %,
40 %, and 50 %) in PANI were synthesized.

2.3. Characterization
The X-ray diffraction studies were performed using Philips X-ray diffractometer with CuKα as the
radiation source. Fourier transformed infrared spectra of these composite were recorded on Thermo
Fisher ATR Nicolet model using diamond (iS5) in the range 4000-400cm-1. The morphology of the
nano nickel oxide and nanocomposites in the form of powder was investigated using SEM ModelEVO-18 Special Edison, zeinn germouny. Sensing properties of the composites were studied using
laboratory sensor set up. Magnetic properties were measured by using B-H loop tracer.

III.

RESULTS AND DISCUSSION

3.1 XRD Analysis
XRD pattern of the samples, are shown in Fig. 3.1(a). They show a broad peak at 2Ɵ=43.35 which has
a sharp and well defined peak, and it indicates the good crystallinity, Fig3.1 (b) shows the intensity of
diffraction peaks for Pani-nickel oxide nanocomposite and it is found to be lower than that for nickel
oxide. The pure nickel oxide nanoparticles peaks are also present in pani/ nickel oxide. The XRD
peaks are broad indicating that the particles are in nanometer size range (JCPDS .No.04-0835). The
amorphous background hump comes from the polyaniline
the crystallite sizes of the samples
increases with the increase of Pani content. The average particle size calculated by using Scherrer
equation is given D=KλβcosƟ Where K is the shape factor for the average crystallite , λ is the Xrays wavelength , β is full width at half maximum of the diffraction line and Ɵ is Braggs angle. It is
found that the
particle size of nickel oxide is 28.832nm and that of pani- nickel oxide
nanocomposite is 108.63nm.

XRD Analysis

3.1(a) Nickel oxide

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Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963

3.1(b) Pani/Nickel oxide nanocomposite
Fig. 3.1 XRD spectra of (a) nickel oxide nanoparticles. (b) Pani/nickel Nano composites.

3.2 FT-IR Analysis
Fig. 3.2(a) shows the FTIR spectra of pure nickel oxide and it has predominant peaks at the wave
number of 3465, cm-1 which is due to the O-H vibration and is formed at higher frequency due to
splitting of water molecules on the surface of nickel oxide nanoparticles , the peaks at 1112 cm-1 is
due to C-H in plane bending modes and the peaks at 414 cm-1 to 590 cm-1 corresponds to metallic
Stretch can be assigned to nickel oxide groups.
Fig 3.2(b). shows the spectra of polyaniline, nickel oxide nanocomposite where the large broad bands
appears from 3903 to 3437 cm-1 which is due to the O-H Stretch because of absorption of water
molecule,the peaks at 2852 cm-1 C-H Stretch, the peaks at 2372cm-1&2330 cm-1 is due to the ύ(NH)+ unsaturated amine,1458 cm-1 is due to C=O aromatic stretch ,1106 cm-1 is due to C-O ester
stretch,1559 cm-1 is due to N-H bending ,The peaks from 887 to 612 cm-1 is due to C-H bending ,and
the peaks from 575 to 447 cm-1 is due to the metallic stretch .
FT-IR Analysis

80
70
60
50
40
30

0

3465.04

10

- 10
- 20

590.13
496.10
487.15
454.90
443.28
546.47
566.59
514.06
422.73
472.11
463.54
414.55
407.11

1112.77

%T

20

- 30
- 40
- 50
400 0

350 0

300 0

250 0

200 0

150 0

100 0

500

W av enu mber s ( c m- 1)

3.2(a) Nickel oxide

622

Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963
100
90

80

70

60

%T

50

40

1458.52
1106.07
1559.921057.56
887.86
837.151544.52
813.341486.28
799.27
729.65
716.13
1288.85
699.92

2357.50
2330.55

2852.96

3197.54

3593.88

3492.12
3437.07

10

3946.85
3907.14
3871.24
3821.71
3751.20
3691.65

20

0

677.91
660.04
612.97
575.68
564.73542.45
528.62
505.55778.11
498.13
481.82 641.92
461.53 521.26
447.52 489.30
426.44415.87407.63

30

- 10
400 0

350 0

300 0

250 0

200 0

150 0

100 0

500

W av enu mber s ( c m- 1)

3.2(b) Pani/Nickel oxide nanocomposite
Fig 3.2 FTIR spectra of (a) nickel oxide nanoparticles (b) pani/nickel oxide nanocomposites.

3.3 Scanning Electron Microscopy
SEM micrograph showing the surface morphology of nickel oxide and Pani - nickel oxide
nanocomposite is given in fig 3.3(a&b). And it is observed that the nickel oxide nanoparticles appear
in a uniform sphere-like shape. Fig 3.3(b) shows the micrograph of pani / nickel oxide nano
composite present in different sizes and shapes compared to the bare nickel oxide nanoparticles where
the layers are wrapped on the surface of nickel oxide nanoparticles appearing as small aggregated
globules.

Scanning Electron Microscopy

3.3(a) Nickel oxide

623

Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963

3.3(b) Pani/Nickel oxide nanocomposites
Fig 3.3 (a) nickel oxide & (b) Pani/ nickel oxide nanocomposites.

3.4 Sensing studies
Figure 3.4 shows sensitivity vs time for Pani/nickel oxide composites. It is observed from figure 3.4,
there is a linear increment in sensitivity and it is also found that it increases up to sometime and
decreases after being transferred to clear air. Among all the Pani / nickel oxide nanomposites, 50 wt%
are showing maximum Sensitivity when compared to pure pani and other composites and this is due
to reaction between the metal oxide and LPG. In the case of pure pani and 10wt% the change in
sensitivity is very low due to lower adsorption because of lower surface area. The result clearly
shows that pani / nickel oxide composite is good candidate for LPG sensing with better sensitivity.
Sensing graph
3

4.0x10

3

pani
10wt%
20wt%
30wt%
40wt%
50wt%

3.5x10

3

3.0x10

Sensitivity%

3

2.5x10

3

2.0x10

3

1.5x10

3

1.0x10

2

5.0x10

0.0
-200

0

200

400

600

800

1000 1200 1400 1600 1800 2000

Time in Seconds

Fig.3.4 variation of sensitivity against lpg.

3.5 Magnetic hysteresis
From magnetic hysteresis measurement, it is observed that pure Nickel oxide nanoparticles exhibits a
saturation magnetization (Ms) at room temperature and was found to be 13.6emu/g, remnant induction
Mr=4.8 emu/g and coercive field Hc=172 Oe .in the case of nickel oxide polyaniline composite the
values of (Ms,Mr,Hc,Oe) are shown in the following table.
Table 1. Shows the hysteresis loop values of Pani/nickel oxide nanocomposites
Wt% of nickel oxide in polyaniline Ms emu/g Mr emu/g Hc Oe
composite
10wt%
0.6
0.3
28
20wt%
1.5
0.7
32

624

Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963
30wt%
40wt%
50w%

IV.

2.8
4.2
9.5

1.8
2.3
4.2

68
79
136

CONCLUSIONS

Nickel oxide nanocomposites were successfully synthesized by in-situ polymerization method. The
results of XRD, FTIR spectra and SEM conformed the formation of the composite and indicate an
interaction between Pani and nickel oxide nanoparticles. The maximal sensitivity is observed for
20wt% of nickel oxide nanocomposites and it decreases with increase in the concentration of nickel
oxide, and the composites particles exhibit a better sensitivity to vapors compared with Pani. The
prepared nanocomposites show supermagnetic behaviors and hence this composite is a promising
material for potential and sensing applications.

V.

FUTURE WORK

The author would like investigates the various transport properties and also studies on sensing
properties such as response time, recovery time etc.

ACKNOWLEDGEMENTS
The author acknowledges the financial support from DST INSPIRE Program.

REFERENCES
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Physics, vol.1,pp-269.
[2] L. Li, J. Jiang, F. Xu, (2007) “Synthesis and ferromagnetic properties of novel Sm-substituted Li, Ni
ferrite– polyaniline nanocomposites” Materials Letters, Vol. 61, pp-1091–1096.
[3]. R. Mathur, D. R. Sharma, S. R. Vadera, N. Kumar, (2001) “Doping of emeraldine base with the monovalent
bridging iron oxalate ions and their transformation into nanostructured conducting polymer composites”,
Acta mater, Vol.49, pp.- 181-187.
[4]. A.G. MacDiarmid, A.J. Epstein, (1995) “Application of thin films of polyaniline and Polypyrrole in Novel
Light-Emitting Devices and Liquid Crystal Devices”, Synthetic Metals, Vol. 69, pp-86-92.
[5] .S,Srivastava ,S, Kumar , VN,Singh , M Singh , VK Vijay, (2011) “Synthesis and characterization of
TiO2 doped polyaniline composites for hydrogen gas sensing”, Int. J Hydro. Energ.vol 36: pp-63436355.
[6]. J.C. Aphesteguy, S.E. Jacobo, (2004) “Composite of polyaniline containing iron oxides” Physica B,
Vol. 354, pp-224–227.
[7]. A. B. Moghaddam, T. Nazari, J. Badraghi, and M. Kazemzad, (2009). “Synthesis of ZnO
nanoparticles and electrodeposition of polypyrrole/ZnO nanocomposite film,”International Journal of
Electrochemical Science, vol. 4, pp. 247–257.
[8]. A. S. Sarac*, M. Ates and B. Kilic, (2008) “Electrochemical Impedance Spectroscopic Study of
Polyaniline on Platinum, Glassy Carbon and Carbon Fiber Microelectrodes” Int. J. Electrochem. Sci,
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[9]. A,Subramania , S-L,Devi ,(2008) “Polyaniline nanofibers by surfactant assisted dilute polymerization for
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[10]. M. P. Pileni, (2001) “Magnetic fluids: fabrication, magnetic properties, and organization of
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[11]. J. Park, E. Kang, S. U. Son et al., (2005) “Monodisperse nanoparticles of Ni and NiO: synthesis,
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Vol. 7, Issue 2, pp. 620-626

International Journal of Advances in Engineering & Technology, May, 2014.
©IJAET
ISSN: 22311963
[14]. I. S. Lee, N. Lee, J. Park et al (2006). “Ni/NiO core/shell nanoparticlesfor selective binding and
magnetic separation of histidinetagged proteins,”Journal of the Ame Chem Soc, Vol.128, pp-10658–
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AUTHORS
Jakeer Husain: obtained M.Sc. in Materials Science Gulbarga University Gulbarga.
Pursuing Ph.D in Materials Science Under the supervision of Prof M.V.N.Ambika Prasad
Department of Materials Science Gulbarga University, Gulbarga. His current research
field is: Conducting polymer nanocomposites.

Chakradhar Sridhar B: received the M.Sc. degree in Physics from Gulbarga University,
Gulbarga. He is currently pursuing his Ph.D. in Physics under the supervision of Prof
M.V.N.Ambika Prasad, Department of Physics, Gulbarga University, Gulbarga. His current
research interest includes conducting polymer nano-composites.

M.V.N.Ambika Prasad: is Professor & chairman Department of Materials Science,
Gulbarga University, Gulbarga. His Research field: Conducting Polymer and
nanocomposites Composites – Understanding the electrical and thermal behavior of the
materials at Nano Size. Sensing behaviors of various conducting polymers exposed to gas
and humidity. Solid State Battery using polymers electrolytes.

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