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Polymers 2019, 11, 914 8 of 10 4. Conclusions The properties of composite Nafion membranes with a sulfated titania additive were investigated. A new template-driven synthesis was developed to obtain highly acidic inorganic particles with mesoporous structure. They were prepared by a sol-gel process with a polymeric template agent, followed by hydrothermal heat treatment. The resulting powder has a low surface development with a very large sulfate content. From the TG analysis, the sulfate groups bonded on the oxide surface were found to be equal to 17% in weight. This value suggests high acidity of the powder and justifies its low surface area. In order to understand the role of the inorganic oxide in a polymer matrix, three composite membranes based on Nafion were prepared, with TiO2-SO4 nominal content of 2%, 5% or 7% w/w. The physical-chemical characterizations, performed on the composite membranes in comparison to plain Nafion, have shown how the inorganic additive has an enormous influence on both the ion-exchange capacity and the hydration ability of the membrane. Fuel cell tests, combined with impedance studies, at 31% RH and temperatures from 80 ◦C to 110 ◦C, revealed the beneficial effect of sulfated titania in terms of lower ohmic resistance and improved charge-transfer behavior, due to a better membrane-electrode interface. Membrane properties, as well as fuel cell performances, were found to be strongly dependent on the concentration of the filler, whose distribution within the polymer matrix is apparently critical. Among all the samples here investigated, indeed, the M2 membrane, with the lowest filler concentration, shows the best performance. This research demonstrated that the incorporation of a minimum amount of mesoporous sulfated titania can be a strategy to improve the low relative humidity, high temperature PEMFC performances. Author Contributions: Conceptualization and methodology, M.A.N. and S.P.; Investigation, data curation and writing—original draft preparation, L.M.; Writing—review and editing and supervision, M.A.N. Acknowledgments: The authors acknowledge Ida Pettiti (Sapienza University of Rome) for the surface area and pore size distribution measurements. Conflicts of Interest: The authors declare no conflict of interest. References 1. Rosli, R.E.; Sulong, A.B.; Daud, W.R.W.; Zulkifley, M.A.; Husaini, T.; Rosli, M.I.; Majlan, E.H.; Haque, M.A. A review of high-temperature proton exchange membrane fuel cell (HT-PEMFC) system. Int. J. Hydrogen. Energy 2017, 42, 9293–9314. [CrossRef] 2. Bose, S.; Kuila, T.; Nguyen, T.X.H.; Kim, N.H.; Lau, K.T.; Lee, J.H. Polymer membranes for high temperature proton exchange membrane fuel cell: Recent advances and challenges. Prog. Polym. Sci. 2011, 36, 813–843. [CrossRef] 3. Kundu, S.; Simon, L.C.; Flowler, M.; Grot, S. Mechanical Properties of NafionTM Electrolyte Membranes under Hydrated Conditions. Polymer 2005, 46, 11707–11715. [CrossRef] 4. Ahmad, M.I.; Zaidi, S.M.J.; Rahman, S.U. Proton conductivity and characterization of novel composite membranes for medium-temperature fuel cells. Desalination 2006, 193, 387–397. [CrossRef] 5. Peighambardoust, S.J.; Rowshanzamir, S.; Amjadi, M. Review of the proton exchange membranes for fuel cell applications. Int. J. Hydrogen. Energy 2010, 35, 9349–9384. [CrossRef] 6. Casciola, M.; Capitani, D.; Donnadio, A.; Frittella, V.; Pica, M.; Sganappa, M. Preparation, Proton Conductivity and Mechanical Properties of Nafion 117–Zirconium Phosphate Sulphophenylphosphonate Composite Membranes. Fuel Cells 2009, 4, 381–386. [CrossRef] 7. Mauritz, K.; Moore, R. State of understanding of nafion. Chem. Rev. 2004, 104, 4535–4585. [CrossRef] [PubMed] 8. Li, Q.F.; Pan, C.; Jensen, J.O.; Noye, P.; Bjerrum, N.J. Cross-linked polybenzimidazole membranes for fuel cells. Chem. Mater. 2007, 19, 350–352. [CrossRef] 9. Scipioni, R.; Gazzoli, D.; Teocoli, F.; Palumbo, O.; Paolone, A.; Ibris, N.; Brutti, S.; Navarra, M.A. Preparation and characterization of nanocomposite polymer membranes containing functionalized SnO2 additives. Membranes 2014, 4, 123. [CrossRef] [PubMed]PDF Image | Polymer Electrolyte Membranes Based on Nafion Fuel Cell
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