Direct ethanol fuel cells (DEFC) still lack active and efficient electrocatalysts for the alkaline ethanol oxidation reaction (EOR). In this work, a new instant reduction synthesis method was developed to prepare carbon supported ternary PdNiBi nanocatalysts with improved EOR activity. Synthesized catalysts were characterized with a variety of structural and compositional analysis techniques in order to correlate their morphology and surface chemistry with electrochemical performance. The modified instant reduction synthesis results in well-dispersed, spherical Pd 85 Ni 10 Bi 5 nanoparticles on Vulcan XC72R support (Pd 85 Ni 10 Bi 5 /C (II-III) ), with sizes ranging from 3.7 ± 0.8 to 4.7 ± 0.7 nm. On the other hand, the common instant reduction synthesis method leads to significantly agglomerated nanoparticles (Pd 85 Ni 10 Bi 5 /C (I) ). EOR activity and stability of these three different carbon supported PdNiBi anode catalysts with a nominal atomic ratio of 85:10:5 were probed via cyclic voltammetry and chronoamperometry using the rotating disk electrode method. Pd 85 Ni 10 Bi 5 /C (II) showed the highest electrocatalytic activity (150 mA⋅cm −2 ; 2678 mA⋅mg −1 ) with low onset potential (0.207 V) for EOR in alkaline medium, as compared to a commercial Pd/C and to the other synthesized ternary nanocatalysts Pd 85 Ni 10 Bi 5 /C (I) and Pd 85 Ni 10 Bi 5 /C (III) . This new synthesis approach provides a new avenue to developing efficient, carbon supported ternary nanocatalysts for future energy conversion devices. Keywords Pd 85 Ni 10 Bi 5 nanocatalyst . Modified instant reduction synthesis method . Ethanol oxidation reaction activity . Structure . Morphology . Alkaline direct ethanol fuel cell Electronic supplementary material The online version of this article (https://doi.

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