Synthesis and Characterization of Polypyrrole/ NiTio 3 Composite
L I Nadaf
1, Lakshmi P Murgod
2, Anita Menasangi
3, Sapna B Ayatawad
41
Dept. of chemistry Secab ARS Inamdar Degree College Vijaypura.
2,3,4
Dept. of Physics Akkamahadevi Women’s University Vijaypura.
ABSTRACT
Conducting polymer composites of Polypyrrole/ Nickel (II) titanate (PPy/NiTio3) were synthesized by chemical polymerization of Polypyrrole with NiTio3 using Ammonium per sulphate as an oxidant, where NiTio3 was varied in three different weights in PPy/NiTio3 composites. The synthesized polymer composites are characterized by Fourier transform Infrared (FTIR), XRD and SEM.
KEYWORDS
: Conducting polymer, Composite, NiTio
3,Polypyrrole, 1. INTRODUCTION
Conducting polymers are important materials emerging with lot of applications in various fields. Research in the field of such polymers aims mainly at some suitable modifications of existing polymers so that their applicability can be improved. Some of these modifications involve preparing hybrid materials in which organic materials and inorganic oxides or salts of different metals[1]. Conductive polymers are a class of polymers which can replace inorganic materials as they exhibit attractive electrical properties and variation in colour because of conjugated double-bond chain structure. Among the conjugated conducting polymers, Polyaniline (PANI) and Polypyrrole (PPy) have attracted much interest because of their high environmental, thermal and chemical stability and high conductivity [8].
Here we presented the synthesis of PPy /NiTio3 composite by in situ chemical oxidative polymerization. For comparison, PPy was synthesized first. The morphology of the resulting PPy/NiTio3 composite was characterized by scanningelectron microscopy (SEM). Information aboutits structure was obtained from FTIR and XRD techniques [5].
2. EXPERIMENTAL
2.1Synthesis of PolypyrroleThe solution of 0.2M Pyrrole and solution of o.4M Ammonium per sulphate were prepared in 2 separate flasks.
The solution of 0.2M of Pyrrole is kept for constant stirring about 15 minutes with magnetic stirrer, a colourless solution will occur. Then 0.4M of Ammonium per sulphate is added to 0.2M of Pyrrole solution drop wise under magnetic stirring, A colourless solution is turn into black. It was left for few hours to settle down and then it was
filter using funnel. The black coloured residue was obtained in the form of thick paste, and it was washed with distilled water and this paste was kept to dry completely. The dried material was grinded to fine powder and this powder is known as Polypyrrole.
2.2 Synthesis of Polypyrrole/NiTio3 composite
Synthesis of the Polypyrrole/NiTio3 composite was carried out by polymerization method. The solution of 0.2M Pyrrole and 0.4M of Ammonium per sulphate was prepared in two separate flasks. NiTio3 of various measures of weight is considered. 0.2M of Pyrrole is kept on the magnetic stirring for about 10-15 minutes, and then known amount of NiTio3 is taken and slowly added in the Pyrrole solution kept on stirring for 15 minutes.
Ammonium per sulphate is added to the solution drop wise. The solution slowly turns to black. It was left for few hours to settle down and then it was filtered. The black colored residue in the form thick paste was obtained.
The paste was washed continuously with distilled water until the filtered solution became neutral. The paste was allowed to dry completely. The dried material was grinded to fine powder. In this way Polypyrrole/NiTio3 composites were synthesized.
3. RESULT AND DISCUSSION
3.1 FTIR: (Fourier transformation infrared spectroscopy)
70.0 72.5 75.0 77.5 80.0 82.5 85.0 87.5 90.0 92.5 95.0
%T
Polpyrrol1
55 60 65 70 75 80 85 90 95
%T
Polpyrrol Ni Tio3( 1.500)1
Figure 1: FT-IR spectra (Transmittance (%) V/S wavenumber (cm-1)) of (a) pure PPy and (b) doped PPy Figure.1 shows the FT-IR spectra, in the range 400-4000 cm-1. In the spectrum, (fig 1(a)) 1550cm-1 for weak aromatic Rings C=C stretch, 1450cm -1 and 1200 cm-1 are C-N medium stretch, 3100cm-1 and 3000cm-1 are the C-H(aromatic rings) medium stretch, 1675 cm -1 and 1635 cm -1 are the N-H(amines) medium bend. (fig 1(b)) 1650cm-1, for C=C weak medium Stretch,1600cm-1,1550cm-1,for C=C weak stretch,1350cm-1 for C-H variable scissoring and bending,1150cm-1,1050cm-1 are the C-N medium stretch, 950cm-1,900cm-1,850cm-1, 800cm-1 are the C-H strong bend, 650cm-1 for C-H broad bend [7].
3.2 Structural characterization by X-ray Diffractometer
(a) (b) Figure 2: XRD images of (a) PPy (b) doped PPy
The crystal structures of the synthesized composite were investigated by powder X-ray diffraction (XRD). The X-Ray diffraction (XRD) patterns of PPy and PPy/NiTio3 are shown in Figure 2 (a) and (b) respectively. PPy has diffraction peak at approximately 2ɵ= 24.620. This broad peak shows the amorphous behavior of Polypyrrole[1]. XRD results of composite indicate that NiTio3 composite improve the crystalline nature of Polypyrrole. Because of in chemical polymerization of Pyrrole in presence of NiTio3 composite, the interaction of NiTio3 and polymer leads to packed chain with higher crystallinity [6]
0 10 20 30 40 50 60 70 80 90
0 50 100 150 200 250
Intensity(a.u)
2(degree)
0 10 20 30 40 50 60 70 80 90
50 100 150 200 250 300 350
Intensity(a.u)
2(Degree)
0.5 1 1.5
a
b c
3.3 SEM (Scanning electron microscopy)
(a)
(b)
Figure 3: Comparison between SEM images of PPy/ Nitio3 composites at the same scales (a) pure PPy (b) PPy/ Nitio3
Figure3 (a) and (b) displays the morphologies of samples and the schematic representations of formation mechanisms. As shown by the SEM images, PPy displays a typically cauliflower-like or tumor-like structure [5].
The particle size of PPy was measured with scanning electron microscopy (SEM).The SEM micrograph is presented in Figure. Small compact globular particles of PPy with distribution dimensions in the range of 5-200 micron were observed.The SEM images of the samples PPy/ Nitio3 are shown in Figure 3(b) [4]. The individual grains observed were nearly spherical and have close packing. The size of particles is in the micrometers range [8].
4. CONCLUSION
In summary, Polypyrrole/ Nickel (II) titanate composites were synthesized by chemical polymerization and characterized by FTIR, XRD, SEM. FTIR analysis showed the synthesis of Polypyrrole[8].XRD pattern of
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