The {[PdPW11O39]5–/Pt/PAMAM}n multilayer composites constructed from G4.0 Amino‐terminated poly (amidoamine) dendrimer (PAMAM), Pt and Keggin‐type palladium(II)‐substituted polyoxometalates anion ([PdPW11O39]5–) were prepared via layer by layer electro‐depositing technique. The X‐ray photoelectron spectroscopy (XPS), X‐ray diffraction (XRD), and field emission scanning electron microscope (FE‐SEM) characterization indicate that the Pt nanoparticles have been anchored on the as‐prepared nanocomposites. And the morphologies of Pt nanoparticles are influenced by deposition potential, the number of layers of {[PdPW11O39]5–/Pt/PAMAM}n multilayer nanocomposites, and the existence of PAMAM. The electrocatalytic properties and stability of {[PdPW11O39]5–/Pt/PAMAM}n multilayer nanocomposites were investigated by cyclic voltammetry. Experimental investigation results reveal that PAMAM is a good support for Pt nanoparticle growth due to its interior cavity structure and high stability. [PdPW11O39]5– play an important role to prevent intermediate product (mainly as CO) in the methanol oxidation from poisoning the as‐prepared catalyst. The {[PdPW11O39]5–/Pt/PAMAM}3/GC shows better electrocatalytic properties, stability, and CO tolerance ability than Pt/GC and {Pt/PAMAM}3/GC fabricated by similar electrodeposition processes.

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