Composition depth profile analysis of electrodeposited alloys and metal multilayers: the reverse approach

The reverse depth profile analysis is a recently developed method for the study of a deposit composition profile in the near-substrate zone. The sample preparation technique enables one to separate the deposit and a thin cover layer from its substrate, and the initial roughness of the sample is much smaller than in the conventional sputtering direction. This technique is particularly suitable to study the zones being formed in the early phase of the electrodeposition of alloys. It has been demonstrated with the reverse depth profile analysis that in many cases when one component of an alloy is preferentially deposited, an initial zone is formed that is rich in the preferentially deposited component. This phenomenon is demonstrated for Ni–Cd, Ni–Sn, Fe–Co–Ni, Co–Ni, and Co–Ni–Cu alloys. The composition change is confined to the initial 150-nm-thick deposit, and it is the result of the interplay of the deposition preference and the depletion of the electrolyte near the cathode with respect to the ion reduced preferentially. The reverse depth profile analysis made it possible to compare the measured and the calculated composition depth profile of electrodeposited multilayers. It has been shown that the decay in the composition oscillation intensity in Co/Cu multilayers with the increase of the sputtering depth can be derived from the roughness measured as a function of the deposit thickness.