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By pyrolyzed the products from hydrothermal reaction of 1, 4, 5, 8‐naphthalene tetramethyl anhydride, NaOH and FeSO4, the nanoparticles of FeFe2O4 were produced, and then its electrochemical performance of oxygen reduction reaction (ORR) was evaluated in O2 saturated 0.1 M KOH solution. The results indicated that, among all the as‐prepared samples, FeFe2O4‐0.50 was mainly composed of uniformly dispersed spherical nanoparticles of 20‐30nm and behaved the best ORR catalytic performance. Its half‐wave potential and limiting diffusion current density was 0.61 V and −1.85 mA cm−2@0.4 V vs. RHE), respectively, higher about 20 mV and 1.29 mA cm−2 than that of FeFe2O4 (0.59 V and −0.56 mA cm−2@0.4 V vs. RHE). In addition, FeFe2O4‐0.50 also showed stronger stability as well as methanol/CO tolerance than that of commercial 20 % Pt/C. It was the evenly dispersed FeFe2O4 nanoscale and Fe−O bond in FeFe2O4‐0.50 that contributed its excellent electrochemical performance and tolerance for CO and methanol. The as‐prepare FeFe2O4‐0.50 might be a potential alternative catalyst for ORR in fuel cell. [ABSTRACT FROM AUTHOR]