Journal of Materials Science and Engineering B 1 (2011) 457-460
Formerly part of Journal of Materials Science and Engineering, ISSN 1934-8959
Synthesis and Characterization of Composite Polypyrrole-Vanadium Oxide (PPy/V2O5)
Nurhizwati Abd. Rahman1, Tunku Ishak Tunku Kudin1, Ab. Malik Marwan Ali1, 2 and Muhd Zu Azhan Yahya1, 2 1. Ionics Materials & Devices (iMADE) Rearch Laboratory, Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Malaysia
2. Institute of Science, Universiti Teknologi MARA, Shah Alam 40450, Malaysia
Received: April 30, 2011 / Accepted: May 18, 2011 / Published: September 25, 2011.
Abstract: Conducting polymer attracts broad attention to rearchers due to their good properties such as high environmental friendly, thermal and chemical stability as well as high conductivity. There are widely u in potential components of optical storage, nsors, batteries, supercapacitor and so on. In this work, polypyrrole was synthesized using chemical oxidation polymerization technique which involves FeCl3 and nanoparticle vanadium oxide (V2O5). The composite PPy/V2O5 has been synthesized under 0 °C with variation weight percentage of nanoparticle V2O5 from 10% to 50% with i
ncrement of 10%. The properties of composites have been characterized by x-ray diffraction (XRD) and Field Scanning Electron Microscopy (FESEM). The ac conductivity has been carried out under frequency range of 100 Hz to 1 MHz over temperature 273 K to 393 K. It is obrved that the ac conductivity of composite increass steeply after frequency of 105 Hz. The composite PPy-V2O5 has shown the larger d-spacing compared to pure PPy and FESEM shows the spongy-like graph of pure polypyrrole than composite PPy/V2O5.
Key words: Polypyrrole, V2O5, composite, chemical polymerization.
1. Introduction
Polymers have emerged as one of the most important materials in the twentieth century. It does contain a long chain of molecular structure and categorized as insulators. The discovery in 1977 of the high conductivity of doped acetylene stimulated studies on the synthesis and study of various conjugated polymers. The most popular conjugated conducting polymers are polyaniline [1], polythiophene [2] and polypyrrole [3]. Polypyrrole have attracted much interest worldwide due to its easy preparation, environmentally stable and has high electrical conductivity [4]. Scientist have discover around many years ago about the ability of conjugated polymer called polyacetylene [5] to c
onducts electrically after undergoing a structural modification process called doping[6]. The electrical
Corresponding author: Muhd Zu Azhan Yahya, professor, rearch field: conducting polymer. E-mail: ***************.ductivity of the polymers is between 10-5 S/cm and 102 S/cm while doped, whereas common insulators exhibit conductivities below 10-12 S/cm [7]. The potential applications of this conducting polymers or organic metals include nsors [8], batteries [9], corrosion protection [10], as well as supercapacitors due to high doping level and fast electrochemical switching with significant capacitance values [11]. Composite of polypyrrole with various nanoparticles have been studied. Nanocomposite polypyrrole/V2O5澳龙养殖
in applications of Li ion battery [12], polypyrrole/iron oxide in applications of nsors and. Several other small particles have been incorporated in to polypyrrole such as silica [13], and titanium dioxide [14].
2. Experiment
Composite PPy/V2O5 has been synthesized using
chemical oxidation polymerization method. Pyrrole
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Synthesis and Characterization of Composite Polypyrrole-Vanadium Oxide (PPy/V2O5) 458
(Aldrich, 98%) was distilled before ud. Ferric chloride (Sigma-Aldrich, 97%) as an oxidant was dissolve in 1 M hydrochloric acid (HCl) together with vanadium oxide (Sigma-Aldrich, 99.99) and stirred under temperature 0 °C-5 °C. the weight percentage of V2O5 was varied from 10% to 50% with increment every 10%. After stirring for 30 min, the pyrrole monomer was injected into the mixture to form composite PPy/V2O5. The final product was filtered and rind thoroughly with methanol (CH3OH) and acetone [(CH3)2CO] to remove the excess solvents. Finally, the precipitate
was dried in vacuum oven at 60°C for more than 12 h. Then, composite powders are ready to be characterized.
The composite powder are presd into round pallet with diameter of 1.53 cm and thickness in range of 0.81 mm to 1.34 mm using hydraulic pressure by applying the pressure of 2-3 tonnes. The ac conductivity was measured in the frequency of 100 Hz to 1 MHz using HIOKI 3532-50 LCR Hi-Tester over temperature of 273 K to 393 K. The x-ray pattern of the composites were recorded in Xpert Pro Pan Analytical using Cu Kαradiation (λ = 1.5406 Å) at 45 kV and 20 mA in the range of 5-90o. The morphology images of composite polypyrrole-vanadium oxide were recorded by FEI Quanta FEG 200 F field emission scanning electron microscope (FESEM).
3. Results and Discussions
Fig. 1 depicts the room temperature conductivity plots of composite polypyrrole with various vanadium oxide contents at 100 kHz. The addition of nanoparticle vanadium oxide results in decrea in conductivity up to 10% vanadium oxide in polypyrrole. A low value plateau formed and thereafter remains constant starting from the 20% to 50% addition of vanadium oxide.
A different ac conductivity of pure polypyrrole and composite polypyrrole-vanadium oxide are shown
in Fig. 2. It can be en that the ac conductivity of pure polypyrrole increas constantly while the ac conductivity of composite polypyrrole-vanadium oxide
PPy/V2O5.
of V2O5 weight percentage.
remains constant until frequency of 105 Hz and increas steeply thereafter.
Fig. 3 shows an ac conductivity of composite polypyrrole-vanadium oxide in frequency range 102 Hz to 106 Hz. From the graph, it can be en that all composite polypyrrole-vanadium oxide which from 10% to 50% weight percentage of vanadium oxide shows the increa in ac conductivity steeply starting from frequency of 105 Hz which reprent the characteristic feature of disorder material. It can be said that the increa of ac conductivity at higher frequency is due to the contribution of polarons. The smaller distance in polymeric chain directed the polaron to move easily. In addition, the movement of the charge in amorphous region also happens at higher frequency. From the XRD pattern in Fig. 4, the sharp peak was obrved at 2θ = 14.8o for Fig. 4b and broad peak at 2θ = 26.8o in Fig. 4a. The peak suggesting the pha of the composite is more to crystalline compared to
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Synthesis and Characterization of Composite Polypyrrole-Vanadium Oxide (PPy/V2O5) 459
amorphous pha in pure polypyrrole. By applying Bragg’s equation, the d-spacing or interlayer spac
ing can be determined. The d-spacing of pure polypyrrole and composite PPy-V2O5 is 3.32 and 5.96 respectively. The larger d-spacing would result in lower conductivity where there is a difficulty of electron to hop from one layer to another. The results are in agreement conductivity in Fig. 1.
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Fig. 5 shows scanning electron micrograph of pure polypyrrole while Fig. 6 shows micrograph of composite polypyrrole-vanadium oxide at vanadium oxide weight percent of 20% in polypyrrole. It can be en that the degree of surface density of composite PPy-V2O5has a much denr structure compared to pure PPy which can be said that the pure polypyrrole is spongier than composite PPy/V2O5. The spongy
PPy/V2O.
PPy/V2O5 (20 wt% of V2O5).
Fig. 5 Scanning electron micrograph of polypyrrole.
Fig. 6 Scanning electron micrograph of composite PPy-V2O5 at 20 wt.% of V2O5.男士洗面乳
feature in pure polypyrrole shows that the more amorphous of the structure. This result is in-line with the result of ac conductivity where the increa in conductivity is due to the amorphousity of the sam
ple.
4. Conclusions
The synthes have been made and their characteristics are collected. The results in conductivity are in-line with the result of FESEM and XRD. The denr structure was found in composite PPy-V2O5while the spongy-like structure was obrved at pure PPy. The addition of V2O5in polypyrrole shows the changing of pha which is from amorphous to more crystalline pha. The sample of composite PPy-V2O5has shown the larger d-spacing than pure polypyrrole which result the
Synthesis and Characterization of Composite Polypyrrole-Vanadium Oxide (PPy/V2O5) 460
lower conductivity. It can conclude that the amorphousity of the samples will affect its conductivity.
Acknowledgment
The author would like to express the great gratitude to Ministry of Science, Technology and Innovation Malaysia for the PGD scholarship awarded and Ministry of Higher Education for supported in Fundamental Rearch Grant Scheme [grant no. 600-RMI/ST/FRGS 5/3/Fst (21/2009).
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