In situ annealing studies on the microstructural evolution of a macro defect free electroformed nanocrystalline Ni-Co sheet metal and its relation to tensile properties

The effect of annealing at temperatures between 200 – 400 °C on the microstructural evolution and tensile properties of a recently developed macro defect free electroformed nanocrystalline Ni-32at%Co free-standing sheet metal was investigated. The tensile strength of the materials exhibited an extrinsic Hall-Petch (HP) to inverse Hall-Petch (IHP) transition due to grain growth. In situ transmission electron microscopy (TEM) annealing revealed for the first time that at lower annealing temperatures, in addition to reordering of atoms at grain boundaries, grain rotation and grain recovery were also found to be mechanisms for grain boundary relaxation (GBR). Combined, these mechanisms contribute to the increase in ultimate tensile strength (UTS) observed in the IHP regime of the Ni-32at%Co alloy. TEM energy dispersive X-ray spectroscopy (EDX) and in situ synchrotron X-ray diffraction (XRD) annealing analyses showed that the drop in UTS and ductility in the HP regime after annealing at higher temperatures was associated with the onset of abnormal grain growth and sulfur impurity segregation to random high angle boundaries. Atom probe tomography (APT) further showed that there is no sulfur impurity segregation in the electroformed material before annealing. Increasing in annealing temperature led therefore to a transition from ductile to brittle fracture manifested as a change in dimple to mixed and eventually to faceted brittle fracture surfaces at 400 °C.