2.1. Fabrication of the Composite Electrodes and the Modification of the Nafion 117 Membrane

We fabricated a series of composite electrodes including carbon paper–titanium dioxide (C–TiO2), carbon paper–palladium oxide (C–PdO), and carbon paper–titanium dioxide–palladium oxide (C–TiO2–PdO) from our previous study [13]. First of all, graphite carbon paper electrodes (C electrodes; Shenhe Carbon Fiber Materials Co. Ltd., Liaoning, China) were acid-treated and modified using the sol–gel and electroless plating methods to form various composite electrodes. The C–TiO2 electrode was fabricated using the tetrabutyric acid mixed with EtOH/HCl (pH = 1) aqueous solution with a tetrabutyric acid/EtOH/HCleq molar ratio of 1:8:4 in a flask, which was mechanically stirred to carry out the hydrolysis reaction at room temperature. The electroless plating solution was 19 g/L Na2C4H4O4·6H2O, 10 g/L PdCl2, 8.5 g/L HCl, and 25.6 g/L C2H4(NH2)2. The effective area of the electrode was 5 × 5 cm2. Finally, these composite electrodes were sintered at 400 °C in an oven for one hour. In addition, we modified a Nafion 117–SiO2–SO3H (N-117–SiO2–SO3H) membrane using 3-mercaptopropyl trimethoxysilane (MPTMS, Acros Organics, Bergen County, NJ, USA) and hydrogen peroxide (H2O2, SHIMAKYU, Japan) in our laboratory [30]. The Nafion 117(N-117) and Nafion 212 (N-212) membranes were purchased from DuPont Inc. (DuPont de Nemours, Inc., Wilmington, DE, USA). All chemicals used were of analytical reagent grade.

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