In order to investigate the effect of carbonization temperature on the electrocatalytic performance of CF/Pd catalysts for methanol oxidation, a series of CF/Pd catalysts were prepared by electrospinning heat treatment carbonization impregnation method. The carbonization temperatures were set at 800, 1 000, and 1 200 ℃, respectively. The obtained CF/Pd catalyst samples were characterized by microscopic morphology, composition analysis, and electrochemical testing. Research has found that at 800 ℃, PAN/CA fibers have completely carbonized, but as the carbonization temperature increases, the degree of fibrosis of CF/Pd catalysts gradually decreases, and the bonding phenomenon becomes more obvious. The electrocatalytic performance of methanol oxidation shows a trend of first increasing and then decreasing. When the carbonization temperature is 1 000 ℃, the CF/Pd catalyst has the best electrocatalytic performance for methanol oxidation, with a catalytic activity 5.4 times that of commercial Pd/C catalysts and a stability 16.2 times that of commercial Pd/C catalysts.