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Polymers 2019, 11, 914 3 of 10 Polymers 2018, 10, x FOR PEER REVIEW 3 of 10 immersed in sodium chloride (NaCl) aqueous solution and the exchanged protons were neutralized immersed in sodium chloride (NaCl) aqueous solution and the exchanged protons were neutralized with a standard solution of sodium hydroxide (NaOH) 0.1 M [23]. with a standard solution of sodium hydroxide (NaOH) 0.1 M [23]. For all the membranes the total water uptake (WU) was evaluated at room temperature by a For all the membranes the total water uptake (WU) was evaluated at room temperature by a gravimetric method, according to the following equation: gravimetric method, according to the following equation: W. U. W W 100 W Wwet − Wdry (1) W.U. = W where Wwet is the weight of fully hydrated membranes, obtained by equilibrating the samples in a × 100 (1) where Wwet is the weight of fully hydrated membranes, obtained by equilibrating the samples in a close container under saturated water atmosphere (100% RH) for two weeks. Wdry is the weight of close container under saturated water atmosphere (100% RH) for two weeks. Wdry is the weight of dry dry membranes, measured after one night a◦t 80 °C under vacuum. For both W.U. and IEC values, membranes, measured after one night at 80 C under vacuum. For both W.U. and IEC values, errors errors were evaluated with standard deviation of three different measurements. were evaluated with standard deviation of three different measurements. Hydration number, known as λ, is a parameter that allows to define the number of water Hydration number, known as λ, is a parameter that allows to define the number of water molecules molecules for each acid group [24]. It was calculated by the following equation: for each acid group [24]. It was calculated by the following equation: λ molHO W.U.10 dry mol acidmgorloHup2Os IEC W.1U8. 10 λ = mol acid groups = IEC × 18 (2()2) Fuel cell tests were performed by using a compact system (850C, Scribner Associates Inc, Southern Fuel cell tests were performed by using a compact system (850C, Scribner Associates Inc, Pines, NC, USA) connected to a 5 cm2 cell fi2xture. The membrane electrode assembly (MEA) was SouthernPines,NC,USA)connectedtoa5cm cellfixture.Themembraneelectrodeassembly(MEA) −2 prepared as follows: The surface of the electrodes (Basf, 0.5 mg Pt cm −2) was brushed with Nafion waspreparedasfollows:Thesurfaceoftheelectrodes(Basf,0.5mgPtcm )wasbrushedwithNafion solution (5% w/w E.W. 1100, Ion Power Inc, München, Germany), resulting in ca. 0.4 mg dry Nafion solution (5% w/w E.W. 1100, Ion Power Inc, München, Germany), resulting in ca. 0.4 mg dry Nafion −2 cm−2 after the evaporation of the solvent. The membrane was hot-pressed between two electrodes at cm after the evaporation of the solvent. The membrane was hot-pressed between two electrodes at 120 ◦C and 10 atm for 7 min. The cell was fed by hydrogen (H ) and air with a backpressure of 1 atm. 120 °C and 10 atm for 7 min. The cell was fed by hydrogen (H2)2 and air with a backpressure of 1 atm. The humidification of the cell was accomplished by bubbling the fed gases through stainless steel The humidification of the cell was accomplished by bubbling the fed gases through stainless steel cylinders incorporated in the compact system and containing distilled water. The temperature of the cylinders incorporated in the compact system and containing distilled water. The temperature of the humidifiers, as well as that of the cell, was properly set to achieve the desired relative humidity. In situ humidifiers, as well as that of the cell, was properly set to achieve the desired relative humidity. In electrochemical impedance spectroscopy (EIS) was performed with the 880 Impedance Analyzer in the situ electrochemical impedance spectroscopy (EIS) was performed with the 880 Impedance Analyzer 10 KHz–1 Hz frequency range. The amplitude of the sine wave was chosen to be 5% of the DC current in the 10 KHz–1 Hz frequency range. The amplitude of the sine wave was chosen to be 5% of the DC present at 0.6 V cell voltage. current present at 0.6 V cell voltage. 3. Results and Discussion 3. Results and Discussion 3.1. Characterization of Powder 3.1. Characterization of Powder The XRD pattern of the titania powder is reported in Figure 1a. The sample resulted in a pure The XRD pattern of the titania powder is reported in Figure 1a. The sample resulted in a pure anatase phase, characterized by tetragonal I41/amd space group. Blue tick marks correspond to the anatase phase, characterized by tetragonal I41/amd space group. Blue tick marks correspond to the anatase TiO2 (CIF number 96-900-8214). The mean crystallite size, determinate by the Maud code, anatase TiO2 (CIF number 96-900-8214). The mean crystallite size, determinate by the Maud code, is is 18 ± 0.36 nm. 18 ± 0.36 nm. a b Fiigurre1..X--rraayydififffrraccttiionpattterrn((a))andSEMiimage((b))offTiO2--SO44ppoowddeerr..PDF Image | Polymer Electrolyte Membranes Based on Nafion Fuel Cell
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