Microstructure, grain growth, and hardness during annealing of nanocrystalline Cu powders synthesized via high energy mechanical milling

• Various grain structures are obtained with various annealing temperatures for NC Cu.
• The volume fraction of the recrystallized grains decreases with increases in temperature.
• The activation energy for the grain growth during annealing was determined.
• The abnormal grain growth led to a steep drop in microhardness during annealing.

In this paper, the microstructure and hardness evolutions of commercially pure Cu subjected to high energy mechanical milling and subsequent annealing treatments in the temperature range of 400–700 °C are investigated. The results demonstrated the simultaneous occurrence of recovery, recrystallization, and grain growth during annealing of the nanocrystalline Cu. The volume fraction of the recrystallized grains estimated using the grain orientation spread exhibits lower values as a result of its dynamic recovery at higher temperatures. The normal grain growth in the range of 400–600 °C and significant abnormal grain growth at higher temperatures are observed during annealing. As a result of the abnormal grain growth, the microhardness value rapidly decreases for the sample annealed at 700 °C. An analysis of the grain growth kinetics using the parabolic equation in the temperature range of 400–600 °C reveals a time exponent of n ≈ 2.7 and an activation energy of 72.93 kJ/mol. The calculated activation energy for the grain growth in the nanocrystalline Cu is slightly less than the activation energy required for the lattice diffusion. This low activation energy results from the high microstrain as well as the Zener-pinning mechanism that arises from the finely dispersed impurities drag effect.

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