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Development and Fabrication of a 1.5 F – 5 V Solid State Supercapacitor

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Development and Fabrication of a 1.5 F – 5 V Solid State Supercapacitor Development and fabrication of a 1.5 F – 5 V solid state supercapacitor Pietro Staiti and Francesco Lufrano CNR-ITAE, ISTITUTO DI TECNOLOGIE AVANZATE PER L’ENERGIA “NICOLA GIORDANO” Via Salita S. Lucia sopra Contesse n. 5 Messina, Italy Phone: 0039 090 624226 / fax: 0039 090 624247 E-mail: [email protected] Acknowledgments The authors acknowledge the Consiglio Nazionale delle Ricerche that has financially supported the research project for the development of this type of supercapacitor. Keywords Supercapacitor, energy storage, solid electrolyte, acidic electrolyte. Abstract A five cells supercapacitor prototype with special electrolyte is designed and fabricated at the Institute CNR-ITAE of Messina. It has a nominal capacitance of 1.5 F and a maximum voltage of 5 V. The electrodes of prototype are formed of high surface area carbon material and Nafion ionomer. Nafion is used as an electrolyte membrane separator between the electrodes of each single cell and as a binder/ion conductor in the electrodes. The fabricated prototype achieves specific capacitance of 114 F/g (referred to the weight of active carbon materials for single electrode), that is comparable to the specific capacitance previously obtained from a smaller scale single cell of same type of supercapacitor. A power density of 1.4 kW/l and a RC-time constant of 0.3 s have been calculated for the device. Introduction Electric double layer capacitors (EDLCs) or supercapacitors (SCs) are promising energy storage devices, which are being considered for applications such as electric vehicles, uninterruptible power systems, and computer memory protection. Their main characteristic is the excellent high-rate charging-discharging ability that makes these devices, referring to this specific aspect, more efficient than batteries and fuel cells. High surface area carbons are the active materials commonly used in the electrodes. In fact, in first approximation the capacitance of supercapacitors is proportional at the electrode/electrolyte interface and then dependent from surface area of carbon material. Other parameters such as electrolyte accessibility in the carbon pores and electric conductivity of the entire device are important figures of merit too. A typical supercapacitor is composed of two electrodes, made of high surface area activated carbon material, and an aqueous or non-aqueous electrolyte impregnated in a porous separator that is stacked between the electrodes. Usually, the aqueous electrolyte is a low cost and high ionic conductivity component that provides a high supercapacitor power density. Instead the nonaqueous electrolyte provides a higher achievable voltage leading to a higher supercapacitor energy density. Both type of devices have been used in the EDLC manufacturing respectively for pulse power application or stable current operation systems. This paper describes the performance of a carbon and Nafion polymer based supercapacitor developed for pulse power applications. Water is the solvating agent of ionic species and the charge carrier in the solid polymer electrolyte, therefore, the device may be considered an aqueous type of supercapacitor. Differently from commonly used acidic aqueous solutions, the acid electrolyte in solid polymer form shows reduced corrosion of the auxiliary components and no leakages of dangerous liquid from the device are possible. Thus this device has a high level of safety. Our recent researches on this type of SC, in single-cell configuration, achieved interesting results in terms of electrochemical performances and stability [1-5]. From the point of view of electrochemical performance, supercapacitor based on a Nafion polymer electrolyte and on electrodes containing a Norit activated carbon material gave a specific capacitance as high as 130 F/g (referred to the weight of activated carbon material in the electrode) [3]. Moreover, the internal resistance of the capacitor with Nafion electrolyte was comparable to that measured with a 1 M H2SO4 solution [2, 3]. The solid polymer electrolyte used in the experiments (Nafion, from Du Pont) is different than other gel-like materials tested as supercapacitor electrolyte [6-9]. The latter includes materials obtained by mixing liquid electrolyte with inert supports, for instance phosphoric acid with nylon [6], phosphoric acid doped silica gel and polymers [7], perchloric acid doped silica [8], phosphoric acid and polyvinyl alcohol [9], and TEABF4 with propylene carbonate (or ethylene carbonate) and poly(vinylidene fluoride-hexafluoropropylene) [10]. Such gel-like electrolytes exhibited insufficient mechanical strength, lower ion conductivity, and lower dimension stability in solvents than solid polymer electrolyte. Solid polymer electrolytes, like Nafion used in this work, consist of an inert hydrophobic backbone and highly hydrophilic terminal functional groups bound to the backbone, are homogeneous materials with outstanding mechanical strength and exhibit high ionic conductivity in their highly hydrated form. The EDLC prototype presented in this paper has been fabricated by stacking five cells and was charged up to 5 V. The goal of our design and prototype fabrication is to highlight the problems arising from the scale-up process from a single-cell to a multi-cell stack as well as from a small to a larger geometrical area. The paper discusses and attempts to explain the problems encountered in scaling-up process. Moreover, the performance of the electrodes is compared to that of electrodes previously studied in the small 4 cm2 single cell. Experimental Preparation of electrodes The electrodes were cut from a larger electrode prepared by a casting method consisting in spreading onto a glass plate with a film applicator the ink containing the activated carbon, the Nafion ionomer electrolyte, the graphite fibers, and the N,N–dimethylacetamide (DMAc) solvent. The activated carbon powder (Norit A Supra Eur) used in the ink preparation has been furnished by Norit Italia S.p.A. (Ravenna, Italy) and had a surface area of 1500 m2/g. The graphite fibers were cut in length 400- 500 µm with a high speed grinder from a carbon fabric (Avcarb 1071) furnished by Ballard Material Products Inc. (MA, USA). The presence of graphite fibers in the final composite electrode allowed the formation of an electrically more conductive and mechanically stronger composite film. The Nafion ionomer (a Du Pont product) intermixed with the carbon in the electrode is acting as the binder of carbon materials (powder and fibers) and as the ion conductor. The composite electrode film was obtained after drying at 70 °C for 5-6 hours the ink cast onto the glass plate. Further thermal treatments at 120 °C for 1 hour and at 160 °C for 20 min were made to produce an electrode with adequate mechanical strength and insolubility of polymer binder in water. Subsequently, the electrode was rinsed several times in distilled water and then chemically treated in 1M H2SO4 solution to obtain the material free from contaminant ionic species eventually attracted by sulfonic groups of Nafion during the preparation process. Further washing of electrode in warm distilled water, till neutral pH, was made to eliminate all the free sulphuric acid adsorbed in the porous structure. The final electrode composition was 65 wt.% of activated carbon powder, 30 wt. % of Nafion and 5 wt. % of graphite fibers. The carbon loading was 8.2 ± 0.9 mg/cm2 and the electrode thickness 150 ± 30 µm. The electrodes prepared with the casting technique showed uniform distribution of the materials and exhibited excellent mechanical strength. Polymer electrolyte membrane The Nafion 115 membrane produced by Du Pont was utilized as electrolytic separator between the electrodes. The water-swelled membrane had an approximate thickness of 160 µm. It was purified by hydrogen peroxide at 3 wt.% for about 1 hour at 70 °C, to remove organic impurities. After three-four washings in pure water to remove H2O2 and traces of soluble organic impurity, a treatment in 1 M sulphuric acid solution at 70-80 °C was carried out to exchange with protons the eventual metallic ionic species attracted on the sulfonic groups of Nafion. The membrane was finally rinsed several times in warm distilled water till the complete elimination of free sulphuric acid. Membrane and electrodes assembly The membrane and electrode assemblies (MEAs), which were inserted in the prototype, were pre- formed out the device by contacting face-to-face the membrane and two electrodes. Each MEA was realized by a hot pressing procedure carried out at 100 kg/cm2 and 130 °C for 10 min. The assembly, after the hot-pressing process, was re-hydrated by immersion in 1M H2SO4 solution first and then rinsed in warm distilled water. All the assemblies exhibit good mechanical characteristics and they did not need particular precaution in handling during the stacking of prototype. Titanium & aluminum External plate Monopolar plate Electrodes Membrane Bipolar plate Monopolar plate Fig.1. Schematic representation of the supercapacitor prototype Preparation of the supercapacitor A supercapacitor prototype was fabricated by stacking five well humidified 16 cm2 MEAs. The assemblies were separated by four bipolar plates of carbon fiber paper 150 µm thick (AvCarb P50T by Ballard Material Products). Two end monopolar plates of the same Ballard carbon fiber paper interfaced the external cells of stack with the metallic current collectors. These latter were formed of titanium foils having a thickness of 250 µm and were externally strengthened by thicker aluminum plates (thickness 2 mm). The use of the metallic current collectors allowed electrical wire connection with testing equipment. The aluminum plate helped the maintaining of titanium foil flatness also during and after the sealing of the device. The prototype was fastened on three sides with an “U” shaped iron that was electrically insulated from the bottoms of the current collectors by a thin PTFE foil. The remaining side of the prototype was sealed with silicon rubber. The so-formed case, containing the active elements of the supercapacitor, is completely sealed and thus the drying of the Nafion electrolyte is not allowed.
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