It is known that palladium‐based catalysts are initially very active in direct formic acid oxidation but they suffer from fast deactivation caused by a strongly adsorbed CO intermediate. Reactivation of the catalysts involving application of anodic potential may cause palladium dissolution. The aim of the present study is to increase the stability and performance of palladium‐based catalysts in direct formic acid fuel cells (DFAFCs). Preparation and characterization of palladium/multiwalled carbon nanotubes (Pd/MWCNTs) and towards formic acid oxidation via different treatments are described. The catalysts were characterized by thermogravimetric analysis (TGA), X‐ray diffraction (XRD), transmission electron microscopy (TEM) and cyclic voltammetry (CV). It was shown that the Pd and Pd–Au MWCNTs supported catalysts after reduction in H2–Ar at 200 °C (R200 treatment) were highly active in formic acid electro‐oxidation, whereas the catalysts after heating in argon at 250 °C (C250 treatment) were inactive. The catalysts after hydrogen treatment have smaller metal particles and better contact with MWCNTs support. CV, simulating reactivation of the catalysts, showed that the Pd catalyst suffers from severe Pd dissolution, whereas for the Pd–Au selective leaching of Pd is considerably slower.

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