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The nanostructured platinum–bismuth catalysts supported on carbon (Pt3Bi/C, PtBi/C and PtBi3/C) were synthesised by reducing the aqueous metal ions using sodium borohydride (NaBH4) in presence of a microemulsion. The amount of metal loading on carbon support was found to be 10 wt.‐%. The catalyst materials were characterised by X‐ray diffraction (XRD), X‐ray fluorescence (XRF), transmission electron microscope (TEM) and electroanalytical techniques. The Pt3Bi/C, PtBi/C and PtBi3/C catalysts showed higher methanol tolerance, catalytic activity for oxygen reduction reaction (ORR) than Pt/C of same metal loading. The electrochemical stability of these nano‐sized catalyst materials for methanol tolerance was investigated by repetitive cycling in the potential range of –250 to 150 mVMSE. Bi presents an interesting system to have a control over the activity of the surface for MOR and ORR. All Pt–Bi/C catalysts exhibited higher mass activities for oxygen reduction (1–1.5 times) than Pt/C. It was found that PtBi/C catalyst exhibits better methanol‐tolerance than the other catalysts.

Carbon-supported platinum and Pt–Pd alloy electrocatalysts with different Pt/Pd atomic ratios were synthesized by a microemulsion method at room temperature (metal loading is 10 wt %). The Pt–Pd/C bimetallic catalysts showed a single-phase fcc structure and the mean particle size of Pt–Pd/C catalysts was found to be lower than that of Pt/C. The methanol-tolerant studies of the catalysts were carried out by activity evaluation of oxygen reduction reaction (ORR) on Pt–Pd catalysts using a rotating disk electrode (RDE). The studies indicated that the order of methanol tolerance was found to be PtPd3/C>PtPd/C>Pt3Pd/C. The oxygen reduction activities of all Pt–Pd/C were considerably larger than that of Pt/C with respect to onset and overpotential values. The Pd-loaded catalysts shift the onset potential of ORR by 125 mVMSE, 53 mVMSE, and 41 mVMSE to less cathodic potentials for Pt3Pd/C, PtPd/C, and PtPd3/C, respectively, with reference to Pt/C and the Pt3Pd/C catalyst showed greater shift in the onset value than the other PtPd catalysts reported in literature. Moreover, the Pt–Pd/C catalysts exhibited much higher methanol tolerance during ORR than the Pt/C, assessing that these catalysts may function as a methanol-tolerant cathode catalysts in a direct methanol fuel cell.

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