An overview is presented about the preparation of nanocrystalline metals by pulsed electrodeposition out of aqueous electrolytes and ionic liquids. Appropriate selection of the bath chemistry and the plating parameters provide the flexibility to control the crystallite size. For selected examples we demonstrate how these electrochemical methods can be used for the preparation of nanostructured bulk metals and nanoparticle for fuel cell applications. Electrochemical analytical methods like cyclic voltammetry and chronoamperometry are used to fundamentally understand the deposition mechanisms, the effect of bath additives on the micro- and nanostructure of the deposits and to characterize the catalytic activity of the electrocatalysts. Some improved physical properties of electrodeposited nanocrystalline metals are discussed, namely thermal stability of n-Fe, magnetisation of n-Ni and hardness of n-Al.
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