ࡱ> fhcdeq`NbjbjqPqP4::;%        8 D x,VXX"zzz+++++++$.h61+Q +  zz2,h&h&h& z z+h&+h&h&O(  (zL O#g(+H,0x,o(,D2%D2(D2 (|#hh&T++&dx,   d D             Electrochemical performance of supercapacitors formed by PAni/CF and PAni/CNT/CF Dalva A. L. Almeida, A. A. R. Carvalho Jr., C. Polo Fonseca, Maurcio R. Baldan and Neidenei G. Ferreira. Laboratrio Associado de Sensores e Materiais Instituto Nacional de Pesquisas Espaciais - INPE Av. dos Astronautas 1758, 12227-010 - S. J. Campos, SP Binary and ternary composites of polyaniline /carbon fiber (PAni/CF) and polyaniline/carbon nanotube/carbon fiber (PAni/CNT/CF are presented. PAni deposits were optimized in both electrodes considering different deposition times. The electrodes morphologies were observed by scanning electron microscopy. The devices were characterized by cyclic voltammetry, charge/discharge response at different current densities and electrochemical impedance spectroscopy. The cycle life was evaluated for both devices as their capacitive performances and demonstrated to be very stable in the range of 3,200 cycles studied. The electrochemical capacitors formed by PAni/CF and PAni/CNT/CF composite electrodes showed high specific capacitance values, potentially viable for application in supercapacitors. Introduction The development of modern devices, which enables solutions for the global energy problem with less environmental impact, has been the subject of intense research [1-3]. Among them, supercapacitors or electrochemical capacitors (ECs) and batteries are very similar devices, but their difference is concerning the charge storage. For supercapacitors the charge storage is capacitive and Faradic while for battery the process is only Faradic. In most cases, supercapacitors are used to deliver a high power during a short time, being often associated to a battery, which in turn provides a high specific energy [4,5]. ECs themselves are grouped into two major categories-symmetric and asymmetric. Symmetric ECs (or SECs) use the same electrode material (usually carbon) for both the positive and negative electrodes. Asymmetric ECs (or AECs) use two different materials for the positive and negative electrodes. An SEC using aqueous electrolyte is also known as a Type I SEC and an SEC using organic electrolyte is known as a Type II SEC [6]. The supercapacitor electrical properties are determined by the selection of electrode material. Double-layer charge storage is a surface process, and the surface characteristics of the electrode greatly influence the capacitance of the cell. Therefore, these devices require the search of new materials as electrodes with high efficiency. In this context, conducting polymer is one of the most promising materials in polymer-based redox supercapacitor for its fast chargedischarge kinetics and the fast dopingundoping process. From an economic point of view, conducting polymers can be generally available with significantly lower cost compared to metal oxide based supercapacitors. The versatility of conducting polymer allows different configurations of redox supercapacitors. These materials can be p doped, when oxidized with the anion insertions on their polymeric chain, or n doped, when they are reduced with the cation insertions to balance the charges [7-9]. Among the conducting polymers, polyaniline (PAni) has attracted much attention because of their environmental stability, controllable electrical conductivity, and easy processability. However, it has some disadvantages for practical application, such as low stability during cycling due to changes in volume with the process of charge/ discharge. To reduce this effect, several authors used a matrix, which serves as a template for the growth of the polymer. In this case, carbonaceous materials such as carbon nanotubes (CNT), carbon fiber (CF) among others, have proven to be excellent materials to orient the polymer chains during the synthesis process [10]. With the aim of improving the life time of the polyaniline electrode, this work shows the development of binary and ternary composites, consisting of PAni/CF and PAni/CNT/CF, respectively. These composites were produced and characterized in order to evaluate their applicability as electrodes for supercapacitors. The high specific surface area of CF and CNTs increased considerably the performance of these conducting polymer devices. The electrodes morphologies were observed by scanning electron microscopy (SEM). The devices were characterized by cyclic voltammetry, charge/discharge response at different current densities, and electrochemical impedance spectroscopy (EIS). Experimental Procedure The PAni/CNT/CF composites were synthesized by oxidative polymerization. For production of the ternary composite PAni/CNT/CF, the CF were cut in size 2x1 cm and weighed. The CNTs multi walls with 90% (Aldrich) were functionalized with H2SO4 and HNO3 in the ratio 3:1 for 24 h. Then filtered and dried were dispersed in aqueous solution containing 0.1 mol L-1 of the surfactant sodium dodecyl sulfate. This solution was added into another solution containing distilled aniline (12.6 mmol L-1) and 1.0 mol L-1 HCl, 3.0 mol L-1NaCl. The CF were fixed in a platinum wire and placed in reaction medium. Another solution containing 1.0 mol L-1 HCl, 3.0 mol L-1 NaCl and 0.03 mol L-1 ammonium persulfate, (NH4)2S2O8, was added to the aniline solution with 90 min of the deposition times at -10 oC with vigorous stirring. The binary composites, PAni/CF, were produced in similar conditions described above using the optimized deposition time of 60 min, but without CNTs, with the aim to observe their influence in the electrochemical properties of the electrode. The resulting composites were filtered and washed with 1.0 mol L-1 HCl, then dried under vacuum for 24 h. The composite morphologies were analyzed by scanning electron microscopy SEM analyses using a JEOL JSM-5310 system. The cells were assembled as supercapacitor devices of type I, with two same composite electrodes of the PAni/CF and PAni/CNT/CF (area: 1 cm 1 cm). Cyclic voltammograms were recorded from -0.44 to 0.44 V at a scan rate of 10 mV s"1 and was subjected to charge discharge cycling in the same potential range. The electrolyte used in assembling the cell was 1.0 mol L-1 H2SO4. The electrochemical impedance spectroscopy (EIS) measurements were performed using the same build cell electrochemical supercapacitor using Ag / AgCl electrode as reference electrode. All measurements were done at OCP in 1 mol L-1 H2SO4 with 10 mV of the potential amplitude in the frequency range of 10-3 to 105 Hz. Results and Discussion SEM image of PAni/CF electrode in Fig 1(a) present a uniform deposit where the PAni covered the entire substrate surface. The polyaniline morphology was composed of plates and clusters with a foam aspect. All the composites prepared by chemical polymerization presented a similar and well-dispersed carbon fiber enwrapped uniformly with the PAni. This complete coverage by the PAni on the CF is related to the Van der Waals interaction between CFs and the PAni by effective interaction between the p- bonds of the aromatic ring of the polyaniline and the CF. This interaction facilitates the growth of a homogeneous conductive polymer on the carbon fiber, due to the electronic conductivity increase provided by the carbon fiber. The ternary composite of PAni/CNT/CF is shown in Fig 1(b) and presents a complete coating of CNT over the CF/PAni substrate. For the PAni/CNT/CF composite, the PAni plays an important role as a binder between carbon fibers and CNT. This ternary composite shows a superficial area and roughness higher than those for CF/PAni composite.  (a) (b) Figure 1. SEM images of the (a) PAni/CF and (b) PAni/CNT/CF composites. The supercacitors that were assembled from the both composite materials of PAni/CF and PAni/CNT/CF are Tipe I and present the following configurations: (a) CF/PAni ( H2SO4 1 mol L-1 (PAni/CF denominated as Type I Electrochemical Capacitor of binary (ECb); (b) CF/CNT/PAni ( H2SO4 1 mol L-1 ( PAni/CNT/CF denominated as Type I Electrochemical Capacitor of ternary (ECt). The devices were studied by cyclic voltammetry (CV) and for both composite types the devices were named as ECb and ECt in the device configurations. Figure 2 shows the CV curves for both supercapacitors that are characterized by rectangle-like shape and symmetric response of ideal capacitive behavior. This behavior was kept up to sweep rate of 50 mV s-1. Nonetheless, in the range from 75 to 100 mVs-1 occurred a small distortion in the voltammograms for both supercapacitors, but it was less evident for the ECt due to the low resistivity of the PAni/CNT/CF. The current values are in the same order of magnitude for the ECb indicating that the redox processes of the PAni is occurring but the peaks are hidden as a result of the capacitive response to be predominant.  Fig. 2. Cyclic voltammetry of ECb (solid line) and ECt (dash line) electrode at 10 mV s-1. The values of specific capacitance were calculated based on the weight of active materials for PAni/CF and in case of the PAni/CNT/CF including the CNT, in order to evaluate their capacitive performance. Figure 3 shows the specific capacitance as a function of the cycle numbers for both assembled devices: CF/PAni ( H2SO4 1 mol L-1 (PAni/CF and CF/CNT/PAni ( H2SO4 1 mol L-1 ( PAni/CNT/CF. For the ECb the initial capacitance value is around 228 F g-1 and after 1000 cycles, the value was 225 F g-1 with a decrease of 11%. Finally, in the last cycles the capacitance remains around 174 F g-1 that means a decrease of 24 %, with a columbic efficiency around 99 %. According to the literature, the PAni electrodes present a capacitance decrease of 26% in the first 1000 cycles of charge/discharge response [10]. However, this result is very promising showing the benefic CF influence in this response. Taking into consideration the ternary composite, the ECt capacitance values also started at de 225 F g-1 and after 1000 cycles the decrease was higher than that for ECb, around 24%. Nevertheless, the capacitance tended to stabilize around 143 F g-1 with a columbic efficiency around 99 %. These results indicate that both electrodes presented a long-life electrochemical stability.  Fig 3. Stability tests of the ECb and ECt at constant i (1.0 mA for 3200 cycles. The Nyquist diagrams for ECb, before and after 3,200 charge/discharge cycles, are presented in Fig. 4 (a). It is important to point out that the vertical line in the diagrams, almost parallel to Z-axis represent an equivalent circuit consisting of a resistance in parallel with an ideal capacitor [10]. The capacitive behavior in low frequency region was observed in both conditions. The behavior for high and medium frequency regions are depicted in Fig 4 (b) and (c) for before and after cycling process. Qualitative values of electrochemical parameter of the ECb can be obtained analyzing the Nyquist diagram. All the Nyquist diagrams showed a warped semi-cycle in the high frequency region, where the first value extrapolated with the real Z-axis is attributed to the solution resistance around 0.66 ( at open circuit potential (OCP). The transfer charge resistance (Rct) is observed at second intersection of semi-cycle with Z- axis Before the cycling, the Rct was around 0.6 (, while after the cycling the Rct values was 2.7 (. This little increase shows the great electrochemical reversible performance of the electrodes. This behavior was clearly confirmed by the small decrease in the specific capacitance in addition to the fact that the columbic efficiency was kept constant at approximately 100%.  (a) (b) Fig.4. Nyquist diagrams for ECb at open circuit potential (OCP), (a) before and after the charge/discharge cycling the whole frequency range and (b) zoom of high and medium frequency interval for both electrodes before and after the cycling in H2SO4 1 mol L-1. The Nyquist diagrams for ECt before and after 3,200 charge/discharge cycles, are presented in Fig. 5 (a) for the whole range of frequency measured. The Nyquist diagrams presented the capacitive behavior in the low frequency region, i.e., an almost parallel line along the Z-axis, very similar to those observed in the ECb results (Fig.4). Nonetheless, observing the expanded Nyquist diagrams in the high frequency ranges in Fig. 5 the diameters of the semicycles for the ECt are smaller than those for the ECb, afterwards the cycling process. According to literature the [9], the low value of the Rct indicates high electronic transference velocity because these composites presented higher surface area available for the electrolyte. This behavior may be attributed to the composite morphologies with the CNT impregnated with the PAni around the CF promoting a suitable porosity, which make easier the composite surface wettability increasing the electron transfer process.  (a) (b) Fig.5. Nyquist diagrams for ECt at open circuit potential (OCP), (a) before and after the charge/discharge cycling and (b)zoom of high and medium frequency interval for before and after the cycling in H2SO4 1 mol L-1. Conclusions The binary and ternary composites were produced with sucess. According to the morphologic analyses the CFs were completely coated by the PAni as well as by the CNT, where the PAni worked as a binder improving the CNT adherence for the ternary composite. Although the CF only acted as a substrate, its presence was fundamental to obtain the binary and ternary composites because the CF improved the electrochemical PAni response associated to its mecanic and electrochemical stability. This fact may be related to the high CF surface area. The EIS analyzes showed that the ECt presented a lowest Rct values associated to the more capacitive behavior, indicating that the CNT favored the charge tranfer process. In summary, the supercapacitors assembled with binary and ternary composites showed a good specific capacitances and high columbic efficiencies confirming their promissing application for supercapacitors. Acknowledgements We are very grateful to CNPq and FAPESP (Process 2009/17584-0) by the financial support. References [1] X. Lu, H. Dou, S. Yang, L. Hao, L. Zhang, L. Shen, F. Zhang, X. Zhang. Electroch. Acta 56 (2011) 9224 9232, [2] V. Khomenko, E. Raymundo-Piero, F. Bguin, J. of Power Sources 195 (2010) 42344241 [3] A.G. Pandolfo, A.F. Hollenkamp, J. Power Sources, 157 (2006) 1127. [4] R. Ktz, M. Carlen, Electroch. Acta, 45 (2000) 2483-2498. [5] A. Burke, Electrochim. Acta 53 (2007) 1083. [6] P. Sharma and T.S. Bhatti, Energy Conversion and Management 51 (2010) 29012912 [7] J. Stejskal, I. Sapurina, M. Trchova, Progress in Polymer Science 35 (2010) 14201481 [8] K.A. Noh, D.W. 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