Thermal stability of nanocrystalline Ni

Thermal stability of electroplated nanocrystalline Ni of 10 and 20 nm grain size was investigated by differential scanning calorimetry (DSC). The temperature dependence and heat release ΔH during grain growth have been determined by linear anisothermal measurements (linear heating at 10 K min−1). The corresponding change in microstructure has been monitored in the temperature range between 373 K and 693 K using transmission electron microscopy (TEM). The TEM and DSC studies identified three exothermic reactions: “nucleation” and abnormal grain growth (353–562 K), normal grain growth (562–593 K) and growth towards equilibrium (643–773 K). The grain growth behaviour, and the similar heat releases ΔH = 18 J g−1, and 16 J g−1 measured for the 10 nm and 20 nm Ni nanocrystals respectively in the DSC experiments may be related to the observed sulphur segregation at grain boundaries and triple junctions.