| Abstract: | We report a study of thermal stability and impact of thermal pretreatment procedures for 46% Pt/Vulcan XC72 (Tanaka) fuel cell catalyst. Stability in air and in inert gas (nitrogen, argon, helium) has been investigated by thermal gravimetric analysis (TGA), TGA‐mass spectrometry (TGA‐MS) and differential scanning calorimetry (DSC). Two distinct low temperature mass loss processes (100–200 and 285–300 °C) were observed, each exhibiting unique pretreatment temperature dependencies. TGA‐MS data in helium show fragment ions that suggest the thermal degradation processes are associated with decomposition of materials such as processing aids. Transmission electron microscopy (TEM) reveals a modest increase in average Pt nanoparticle size upon thermal pretreatment. After a pretreatment protocol based on TEM and thermal characterisation (300 °C/15 min, N2), the electrochemically active surface area did not increase. At the kinetically controlled potential region (E >0.8 V) there was a small drop in current density for treated 46% Pt/C in comparison with as‐received catalyst. The slowing in ORR kinetics is significant. Apparently, the removal of organic components, which would improve mass transport, is negated by increased nanoparticle size. |
