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Nanomaterials 2021, 11, 1017 4 of 12 S-4700, Hitachi). The crystalline structures of the catalysts were investigated by X-ray diffraction (XRD, Rigaku, TX, USA) using Cu-Kα radiation over the 2θ range of 20–80◦. Brunauer-Emmett-Teller (BET) analysis was performed to investigate the specific surface area of the obtained samples (Autosorb iQ Station 2). 2.5. Electrochemical Analyses A three-electrode system was used to investigate the electrochemical activity of the synthesized catalysts. Glassy carbon with the synthesized catalysts, a Ag/AgCl saturated electrode, and Pt wire were employed as the working electrode, reference electrode, and counter electrode, respectively. First, the glassy carbon electrode was polished with alumina powder (mean diameter of 0.3 μm), then rewashed with DI water, sonicated for 1 min, and finally dried naturally at room temperature. The catalyst ink was prepared by suspending 10.0 mg of the synthesized catalyst in a mixture of Nafion (150 μL, 5 wt. %) and isopropanol (850 μL). This suspension was sonicated for 15 min to obtain a uniform black catalyst paste. Subsequently, 6 μL of this prepared mixture of catalysts was dropped onto the surface of the glassy carbon electrode for further electrochemical tests under O2 atmosphere. Cyclic voltammetry was performed using a CHI 150 electrochemical workstation (Shanghai, China) with a three-electrode cell system. 2.6. Membrane Electrode Assembly and Fuel Cell Testing Membrane electrode assemblies (MEAs) for single-cell direct urea fuel cells with an active working area of 5.0 cm2 were fabricated using FAS-30 (FuMA-Tech) membranes and carbon paper (AvCarb © MGL190 Teflon treated) fabricated by using the prepared catalyst paste. The paste was prepared by mixing 50 mg of the prepared powder in 850 μL iso-propanol/150 μL Nafion-5%. The mixture was sonicated for 15 min and magnetically stirred for 1 h. Using brushes, the paste was hand-painted onto carbon paper at a loading of ~6.0 mg cm−2. A Pd/C (~0.3 mg cm−2 loading, 40 wt. % Pd) commercial catalyst was used on the anode side, and the prepared catalysts were used on the cathode side. The anode, membrane, and cathode were subjected to hot pressing at 100 ◦C at 3.5 Pa for 5 min. The unit cell performance was investigated using a station VSP potentiostat-galvanostat (Biologic-Science, Seyssinet-Pariset, France) at 20 ◦C. The anode flow comprised 0.33 M urea solution and 1 M KOH (flow rate 10 mL min−1) and the cathode flow comprised oxygen only (flow rate 300 mL min−1). 3. Results and Discussion 3.1. Physicochemical Characterization of Co3O4@MWCNT and Pd/Co3O4@MWCNT Figure 1 shows the X-ray diffraction patterns of the Pd/Co3O4@MWCNT, Pd/MWCNT, Co3O4 @MWCNT, and f-MWCNTs. The XRD pattern of Pd/Co3O4@MWCNT presented reflection peaks at 2θ = 41◦, 46◦, and 68◦, corresponding to the (111), (200), and (220) planes of Pd, respectively. Most of the peaks in the XRD pattern of Co3O4@MWCNT fit well to the expected pattern, except for those of the (220) plane, and the other peaks were similar to those reported for Co3O4 at 2θ = 40◦, 45◦, 59◦, and 65◦, which correspond to the (331) (400), (511), and (440) planes, respectively [17,24]. Figure 1e,f shows the referred data which were indexed to the Co3O4 and Pd crystallite structures which corresponded to JCPDS No. 43-1003 and JCPDS No. 46-1043. As we could see, the peaks fitted well with the diffraction peaks in the obtained Pd and Co3O4 composite. This observation suggests the formation of Pd nanoparticles coated on Co3O4@MWCNT in the composite. The crystallite sizes were estimated by Debye-Scherrer equation at 2θ = 36.8◦ and 40.1◦ for Co3O4 and Pd, which were 12.3 nm and 7.8 nm, respectively. Those results relatively correspond to the sizes obtained in the TEM analysis.PDF Image | Effect of Co3O4 Nanoparticles on Improving Catalytic Behavior
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