Electroplating is one of the most technologically advanced methods to synthesize nanophase materials both as coatings and in bulk form. This paper demonstrates the formulation of a processing “window” for nanocrystalline Co-W alloys using factorial design. The microstructural evolution from polycrystalline to nanocrystalline to amorphous Co-W microstructures is shown for electrodeposits produced from a bath containing cobalt sulphate, sodium tungstate, Rochelle salt and ammonium chloride. The effect of operating variables such as temperature and current density is discussed.

The microstructural evolution during grain growth at large driving forces of an ultrafine‐grained Ni–1.2wt%P solid solution (starting grain size of 7nm) is evaluated for the temperature range 473 to 873 K. It is shown that the material is thermally stable as a nanocrystalline structure up to 623 K. At higher annealing temperatures the material transformed into a two‐phase Ni + Ni3P microstructure and considerable grain growth was observed. The Ni matrix showed continuous grain growth and displayed a temperature‐dependent grain growth exponent N. The effects of driving force, grain boundary mobility, and grain boundary pinning on the final microstructure are discussed.