We present the deposition of Pt particles and films by chemical vapor deposition from platinum(II) acetylacetonate for electrochemical water splitting. High‐surface‐area particles can be obtained at substrate temperatures as low as 150 °C by this technique. Clear differences in morphology were identified, which depended on the type of reactive gas introduced in the process. Although oxygen leads to a crystalline film growth, hydrogen leads to an open structure of stacked Pt spheres. The electrochemically active surface area of these deposits were determined by hydrogen adsorption–desorption measurements in alkaline solution. With respect to water splitting and other catalytic processes, we present a way to synthesize and characterize high‐surface‐area Pt samples easily. To evaluate their electrocatalytic performance, the catalysts were analyzed in terms of the overvoltage for the hydrogen evolution reaction.

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