Three-dimensional EBSD study on the relationship between triple junctions and columnar grains in electrodeposited Co-Ni films.

Electrodeposited nanocrystalline materials are expected to have a homogeneous grain size and a narrow grain size distribution. In Co-Ni electrodeposited films, however, under certain conditions an undesired columnar grain structure is formed. Fully automated three-dimensional (3D) orientation microscopy, consisting of a combination of precise material removal by focussed ion beam and subsequent electron backscatter diffraction (EBSD) analysis, was applied to fully characterize the grain boundaries of these columnar grains in order to gain further understanding on their formation mechanisms. Two-dimensional orientation microscopy on these films indicated that the development of columnar grains could be related to the formation of low-energy triple junctions. 3D EBSD allowed us to verify this suggestion and to determine the boundary planes of these triples. The triplets are formed by grain boundaries of different quality, a coherent twin on the {1011} plane, an incoherent twin and a large-angle grain boundary. These three boundaries are related to each other by a rotation about the <1120> direction. A second particularity of the columnar grains is the occurrence of characteristic orientation gradients created by regular defects in the grain. Transmission electron microscopy was applied to investigate the character of the defects. For this purpose, a sample was prepared with the focussed ion beam from the last slice of the 3D EBSD investigation. From the TEM and 3D EBSD observations, a growth mechanism of the columnar grains is proposed.