The proposed project is aimed at determining the nucleation/growth processes and structures (metal distributions and solvent population/distribution) of metallic films deposited in situ by different electrochemical protocols. We have successfully completed NR investigations of potentiostatic and potentiodynamic electrochemical methods in the deposition and stripping of single metal systems of Ag, Cu and Sn as well as alloy and multilayer systems of Ag/Cu and Cu/Sn all of which have significant industrial interests. The outcomes of these experiments have provided insights into the early stages of deposition and on the alloying/segregation of components within the deposited layer. Since deposit structure is in general a function of electrochemical protocol, our aim is to complete the exploration by making NR measurements during deposition under galvanostatic (constant current) control.