Professional Documents
Culture Documents
Bushra Anjum
Department of Physics
Gulbarga University Gulbarga 585106 Karnataka, India
Abstract
Nanocomposite of polyethylene oxide/nickel ferrite nanoparicles were synthesized by Sol-Gel method these nanocomposites
were characterized by employing .X-ray diffraction (XRD), infrared (FT-IR) spectroscopy and TEM. The conductivity was
found to increase with the increase in temperature indicating the semiconducting behavior of all the compositions. Maximum
conductivity was observed in 1.5 wt%.
Keywords: Synthesis, X-Ray Diffraction, TEM, FT-IR
________________________________________________________________________________________________________
I. INTRODUCTION
Recent years polyethylene oxide based polymer electrolytes composite are showing great interest due to their optical as well as
theoretical importance for making of solid state batteries, sensors. electronic etc. (1-4). PEO is an exceptional polymer which
dissolves with concentrations of a wide variety of salts to form polymer electrolytes (5) Spinel Ferrite nanoparticles are belongs
to soft magnetic materials these ferrites are most attractive class of materials due to important properties such as low melting
point, high specific heating, large expansion coefficient, low saturation magnetic moment and low magnetic transition
temperature, etc. Because of these properties, the spinel ferrites have many technical applications, such as in photoelectric
devices, catalysis, sensors, nano devices, microwave devices and magnetic pigments. Nickel ferrite is one of the important soft
ferrite materials because of its typical ferromagnetic properties, low conductivity and thus lower eddy current losses, high
electrochemical stability, catalytic behavior, abundance in nature, etc. (6-14). PEO has the simplest structure of water-soluble
polymers. Its salt complexes have shown to be solid electrolytes and have attracted considerable research attention because they
are promising for applications in solid-state batteries and electrochromic devices.(15)
In this present work authors have carried out the synthesis, characterization, DC conductivity studies of PEO/Nickel ferrite
nanocomposites. The dc conductivity shows that N3 has high conductivity among all composites. It is observed that N3
composites have high current compare to other composites due to more feasibility for ion moments.
II. EXPERIMENTAL
Materials
Polyethylene oxide (relative molecular mass of 5 x 105) was obtained from Shanghai Research Institute of Chemicals, China and
dried under vacuum at 50 C for 24 h before use.
Nickel Ferrite Nanoparticles Were Prepared by the Solgel Method
Using Nickel nitrate and ferric nitrate in the molar ratio 1: 2. A certain amount of citric acid was dissolved in distilled water, A
small amount of ammonia was then added to the solution to adjust the pH value to 7 and stabilize the nitrate-citrate solution.
During this process the solution was continues stirring using magnetic stirrer for 56 h at 1200C. Finally, a gel is formed. This
gel is heated at a temperature of about 300 C for 1 h to remove water molecules. Finally, the gel is completely transformed into a
foam powder. The foam powder was then ground into a fine powder. The synthesized powder was ground and calcinate for 2
hour to remove impurities finally get pure nickel ferrite nanoparticles.
FTIR Spectra
Fig. shows the FTIR spectra of the polyethylene oxide /nickel ferrite composites ,. The absorption bands around 629.12 cm-1 in
NiFe2O4 are attributed to the stretching vibration of tetrahedral and octahedral group complexes of ferrites, respectively . The
bands at 1690.39 and 1487.89cm-1 in pure NiFe2O4/PEO are the characteristics bands of nitrogen quinoid and benzoid forms due
to the conducting state of the polymer. The bands at 2541 to 2931 cm-1 is due to hydrogen bonding . The interaction of nickel
ferrite with polyaniline is confirmed from IR spectra of the nanocomposites.
95
90
85
2 5 4 1 .8 1
2 6 3 4 .4 4
1 6 0 6 .4 9
1 1 7 7 .6 3
80
6 3 9 .7 1
9 2 1 .5 8
2 9 3 1 .6 5
75
%T
1 3 0 9 .0 8
70
1 2 0 1 .1 2
65
1 4 1 6 .2 7
60
55 1 6 9 0 .1 7
50
Wavenumbers (cm-1)
Fig. 1: Shows the FTIR spectra of the polyethylene oxide /nickel ferrite composites
X Ray Diffraction
The reinforcement of PEO is done by fillers like ferrite nanoparticles which play a major role in strengthening properties of
polymer nanocomposites. When nanosized ferrite particles are magnetic in polymer matrix, then such nanocomposites show
enhanced magnetic and transport properties over their individual constituents. XRD pattern of nickel ferrite (NF) shows all the
peaks corresponds to spinnel ferrite phase matches well with JCPDS data 10-325. The average crystallite size of the NiFe 2O4 was
found to be 30 nm. NiFe2O4 belongs to the class of ferrites with inverse spinel structure.
6000
PEO/Nickel ferrite composite
5000
4000
Intensity (a.u.)
3000
2000
1000
0
0 20 40 60 80
2 (degree)
Fig. 2: Shows the XRD spectra of the polyethylene oxide/nickel ferrite composites
DC Conductivity
Conductivity DC electrical conductivity of the Ni-PEO system was found to increase from 8.04 X10-05 (-cm) to 4.71 X10-03
(-cm) at room temperature with the increase in Cu concentration form 0.5 to 2.5 This increase in conductivity is due to the fact
that PEO has smaller value of resistivity as compared to that of Ni (7.010-6 -cm) .The increase in conductivity may be due to
the hopping of electrons between Fe2+ Fe3+ on tetrahedral sites that increases the conduction as PEO is added, which are
produced during sintering.
5
1.4x10 0.5
1.5
5
1.2x10 2.5
5
1.0x10
dc conductivity(S/cm)
4
8.0x10
4
6.0x10
4
4.0x10
4
2.0x10
0.0
IV. CONCLUSION
The polyethylene oxide /nickel ferrite composites with different weight percentages of NiFe2O4 in PEO were synthesized by Sol-
Gel method. Detailed characterizations of the nanocomposites were carried out using the techniques such as XRD, FTIR and
TEM,. The results of XRD, FTIR and TEM reveals that the crystalline nature of the NiFe2O4 nanocomposites. FTIR spectra of
the nanocomposites show the characteristic absorption bands which confirm the formation of NiFe2O4/PEO nanocomposites.
The DC conductivity as a function of temperature NiFe2O4/PEO nanocomposites was studied in the temperature range from
30oC-160oC. At higher temperatures, DC conductivity increases because of hopping of polarons from one localized state to
other localized states. The DC conductivity of the nanocomposites increases with an increase in temperature, which is
characteristic behavior of semiconducting materials.
ACKNOWLEDGMENTS
The First author is working as faculty in the Department of S&H and grateful to the management of Farah Institute of
Technology, Chevella for the financial support in the research work.
REFERENCES
[1] M.A.Ratner, D.F.Shriver, Chem. Rev. 1988, 88,109. DOI: 10.1021/cr00083a006
[2] M.Armand, Polymer Electrolytes Ann. Rev. Mater. Sci. 1986, 16, 254. DOI: 10.1146/annurev.ms.16.080186.001333
[3] Appetecchi G B, Hassoum J, Scrosati B, Croce F, Cassel F and Salomon M J. Power Sources 2003, 124, 246 DOI: 10.1016/S0378-7753(03)00611-6
[4] A. Tiwari, V. Singh, Carbohydrate Polymers 2008, 74, 427 DOI:10.1016/j.carbpol.2008.03.015
[5] K. Hanai, K. Kusagawa, M. Ueno, T. Kobayashi, N. Imanishi, A. Hirano, Y. Takeda, O. Yamamoto, (2010) J. Power Sources 195:2956.
DOI:10.1016/j.jpowsour.2009.08.087
[6] Xu Q, Wei Y, Liu Y, Ji X, Yang L, Gu M: Preparation of Mg/Fe spinel ferritenanoparticles from Mg/Fe-LDH microcrystallites under mild conditions.Solid
State Sci 2009, 11(2):472-478.
[7] Tian MB: Magnetic Material Beijing: Tsinghua University Press; 2001.
[8] Hu J, Li L-s, Yang W, Manna L, Wang L-w, Alivisatos AP: Linearly PolarizedEmission from Colloidal Semiconductor Quantum Rods. Science 2001,
292(5524):2060-2063.
[9] Sloczynski J, Janas J, Machej T, Rynkowski J, Stoch J: Catalytic activity of chromium spinels in SCR of NO with NH3. Appl Catal B 2000, 24(1):45-60.
[10] Pena MA, Fierro JLG: Chemical Structures and Performance of PerovskiteOxides. Chem Rev 2001, 101(7):1981-2018.
[11] Ajayan PM, Redlich P, Ru"hle M: Structure of carbon nanotube-basednanocomposites. J Micro 1997, 185(2):275-282.
[12] Baykal A, Kasapoglun , Durmus Z, Kavas H, Toprak MS, Koseoglu Y: CTABAssistedHydrothermal Synthesis and Magnetic Characterization ofNiXCo1-
xFe2O4 Nanoparticles (x = 0.0, 0.6, 1.0). Turk J Chem 2009, 33:33-45.
[13] Gunjakar JL, More AM, Gurav KV, Lokhande CD: Chemical synthesis ofspinel nickel ferrite (NiFe2O4) nano-sheets. Appl Surf Sci 2008,254(18):5844-
5848.
[14] Wang X, Yang G, Zhang Z, Yan L, Meng J: Synthesis of strong-magneticnanosized black pigment ZnxFe3-xO4. Dyes Pigm 2007, 74(2):269-272.
[15] Polymer Electrolyte Reviews; McCallum, J. R., Vincent, C. A.,Eds.; Elsevier Applied Science: London, 1987, 1989; Vols. 1 and 2.