Nickel electrodeposits, of various thicknesses, were prepared from Watts' baths containing several addition agents to study the development of the surface structure. By electron‐microscopic examinations of replicas, thin films, and electrolytically thinned bulk metal the reasons for the formation of several structural features, previously observed, were found. Selected‐area diffraction was found to be the best method of measuring the grain size of the electrodeposits studied. Markings believed to be sites of lattice‐included foreign substances were observed.