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Micromachines 2021, 12, 72 2 of 12 dioxide (CO2) and poisoning the catalyst by irreversibly attaching to the active sites of Pt, which greatly reduces the performance, stability, and life of the catalyst [8]. Of the utmost importance within the catalytic membrane, the anode electrode in the membrane directly contacts and reacts with methanol fuel; therefore, its performance has the greatest impact on the overall performance of the fuel cell. Previous studies have shown that different catalyst compositions and their supporting materials can significantly affect the performance of anode electrodes [9–13]. Among many materials, graphene, for its two-dimensional periodic structure, consisting of six-membered carbon rings, and its high conductivity properties, is considered one of the best options as catalyst supporting material for μDMFC. In this work, the preparation process of the reduced graphene oxide catalyst prepared by the high-temperature polyol method was optimized, and the influence of the reduced graphene oxide catalyst prepared by different reduction methods on the performance of the methanol fuel cell was compared. In order to further improve the performance of the fuel cell, the composition of the reduced graphene oxide composite electrode was optimized, including the Pt-Ru molar ratio, Pt content, Nafion content, carbon loading, and PTFE content. This work provides a feasible strategy for improving the performance of μDMFC based on reduced graphene oxide composite electrodes. 2. Experiment 2.1. Reagents and Materials Conductive carbon paper (TGP-H-060, Toray Corporation, Tokyo, Japan), conductive carbon powder (Vulcan XC-72C, Cabot Inc, Alpharetta, GA, USA), chloroplatinic acid (H2PtCl6) (pure reagent for analysis), ruthenium(III) chloride (RuCl3) (pure reagent for analysis), sodium hydroxide (NaOH), methanol (pure reagent for analysis), 5 wt.% Nafion solution and 60 wt.% PTFE emulsion, Nafion 117 membrane (DuPont Inc., Seoul, Korea), graphene oxide (Laboratory Grade, Suzhou Hengqiu Branch Technology Co., Ltd, Suzhou, China), and isopropanol (pure reagent for analysis). IT8510 DC Electronic Load (Nanjing Edks Electronics Co., LTD. Nanjing, China), HS-XX40 Hot Press (Shanghai Hesen Elec- tric Co., LTD. Shanghai, China), 040S Ultrasonic Cleaning Apparatus (Shenzhen Chaojie Technology Co., LTD. Shenzhen, China). 2.2. Preparation of Catalyst Layer Slurry Firstly, 72 mg graphene oxide powder was added to 30 mL ethylene glycol, and the mixture was ultrasonically shaken for 1 h to make the graphene oxide uniformly dispersed to form 2.4 mg/mL graphene oxide dispersion. Subsequently, 6 mL 0.05 mM chloroplatinic acid solution and 9 mL 0.05 mM ruthenium chloride solution were added to the graphene oxide dispersion and sonicated for 1 h. After adjusting the pH to 10 with 0.5 M sodium hydroxide solution, the solution was processed according to two preparation methods: the first preparation method was to pour enough glycol as reducing agent into the reagent and stir at 160 ◦C for 6 h; the second method was to add sodium borohydride to the reagent as reducing agent and stir at room temperature for 6 h. After processing as above, the prepared solution was stirred and separated centrifugally. Next, the solution was dried in an oven at 80 ◦C for 12 h to obtain reduced graphene oxide-supported Pt/Ru catalyst powder. Finally, the catalyst powder was shaken with 0.5 mL Nafion solution and 5 mL isopropanol for 0.5 h to form a catalytic layer slurry. 2.3. Preparation of Electrode The electrode of μDMFC mainly includes the diffusion layer and the catalyst layer. In this work, carbon papers with a size of 15 × 15 mm were prepared as the base of the diffusion layer. A micro-porous layer was fabricated on the carbon paper by the slurry spray method. The micro-porous layer slurry was prepared by dissolving 3.5 mg of carbon powder into 2 mL isopropanol and 0.5 mL PTFE emulsion. After ultrasonic agitation for 30 min, the micro-porous layer slurry could be prepared for use. The carbon loadingPDF Image | Micro Direct Methanol Fuel Cell Reduced Graphene Oxide
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