A series of nickel layers was electrodeposited at different current densities from a Watts type electrolyte containing the additive 2-butyne-1,4-diol in various concentrations. The internal structure of the nickel electrodeposits was systematically investigated applying complementary microscopic and diffraction based characterization methods involving both surface and cross section investigations with different resolution and statistics. The complementary information gathered from combining the various techniques of microstructure characterization, in particular, supported the investigation of twins and the preferred crystallographic orientations of grains in the electrodeposits. Additive-free deposition results in relatively large columnar grains with numerous growth twins of nanoscale dimensions. The presence of the additive in the electrolyte yields considerable grain refinement already at low additive concentration, but the preferred crystallographic orientation of grains changes gradually with increasing additive concentration and twins with nanoscale dimensions are detected also in these samples.
- Electron microscopy