Evolution of the microstructure in nanocrystalline copper electrodeposits during room temperature storage

. The microstructure evolution in copper electrodeposits at room temperature (self-annealing) was investigated by means of X-ray diffraction analysis and simultaneous measurement of the electrical resistivity as a function of time. In-situ studies were started immediately after electrodeposition and continued with an unprecedented time resolution until sta-tionary values of the recorded data were obtained. Independent of the copper layer thickness, the as-deposited microstructure consisted of nanocrystalline grains with orientation dependent crystallite sizes. Orientation dependent grain growth, crystallographic texture changes by multiple twinning and a decrease of the electrical resistivity occurred as a function of time at room temperature. The kinetics of self-annealing is strongly affected by the layer thickness: the thinner the layer the slower is the microstructure evolution and self-annealing is sup-pressed completely for a thin layer of 0.4 μm.