The oxygen reduction reaction (ORR) is an important cathode reaction used in fuel cells and metal-air batteries for renewable energy applications. [1][2][3] Platinum has been studied extensively as an essential catalytic component to reduce undesired overpotentials observed in the ORR. [4] Previous computational and experimental investigations have revealed that once alloyed with first-row transition metals, such as Fe, Co, and Ni, Pt alloy thin films and nanoparticles (NPs) can show dramatic activity enhancement in ORR catalysis, [5,6] especially when the Pt-skin structure is formed on the surface of MPt. [7] This enhancement is believed to originate from the downshift of the d-band center of Pt in the alloy structure; this downshift results in a decrease of the bonding strength between Pt and the oxygenated species (often called blocking species or spectators) and an increased number of available Pt sites for oxygen adsorption.[5] Recent experiments also indicate that elongated Pt nanostructures are less subject to dissolution, Ostwald ripening, and aggregation than the Pt NPs in acidic conditions, [8][9][10][11] and that they may be robust for catalyzing the ORR with high activity and durability.Herein, we report an advanced organic-phase synthesis of thin FePt and CoPt alloy nanowires (NWs) for enhanced catalysis of the ORR. Different from the previous approach to FePt NPs [12] and FePt NWs, [13] the current synthesis through decomposition of metal pentacarbonyl and reduction of platinum acetylacetonate, [Pt(acac) 2 ], was performed in sodium oleate solution of 1-octadecene (ODE) and oleylamine (OAm). Depending on the metal carbonyl used, FePt or CoPt NWs were obtained at a high synthetic yield and with the desired control over alloy composition. Electrochemical studies showed that these NWs were active catalysts for the ORR. The specific activity and the mass activity of the 2.5 nm wide FePt NWs reached 1.53 mA cm À2 and 844 mA mg À1 Pt at 0.9 V (vs. reversible hydrogen electrode, RHE; 0.2 mA cm À2 and 110 mA mg À1 Pt at 0.95 V), while those of the benchmark Pt catalyst reached 0.32 mA cm À2 and 155 mA mg À1 Pt at 0.9 V (0.080 mA cm À2 and 35 mA mg À1 Pt at 0.95 V). The annealed 6.3 nm wide FePt NWs showed an even higher specific activity of 3.9 mA cm À2 at 0.9 V and 0.46 mA cm À2 at 0.95 V.