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Microstructure evolution and hardness variation during annealing of equal channel angular pressed ultra-fine grained nickel subjected to 12 passes

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Abstract

The microstructure, thermal stability and hardness of ultra-fine grained (UFG) Ni produced by 12 passes of equal channel angular pressing (ECAP) through the route Bc were studied. Comparing the microstructure and hardness of the as-ECAPed samples with the published data on UFG Ni obtained after 8 passes of ECAP through the route Bc reveals a smaller average grain size (230 nm in the present case compared with 270 nm in 8-pass Ni), significantly lower dislocation density (1.08 × 1014 m−2 compared with 9 × 1014 m−2 in 8-pass Ni) and lower hardness (2 GPa compared with 2.45 GPa for 8-pass Ni). Study of the thermal stability of the 12-pass UFG Ni revealed that recovery is dominant in the temperature range 150–250°C and recrystallisation occurred at temperatures >250 °C. The UFG microstructure is relatively stable up to about 400 °C. Due to the lower dislocation density and consequently a lower stored energy, the recrystallisation of 12-pass ECAP Ni occurred at a higher temperature (~250 °C) compared with the 8-pass Ni (~200 °C). In the 12-pass Nickel, hardness variation shows that its dependence on grain size is inversely linear rather than the common grain size−0.5 dependence.

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Notes

  1. A conventional AFM image (image of topography) is obtained by recording the changes in the vibrational amplitude (deflection) during scanning. In contrast, a phase image is obtained by monitoring the phase change between the input signal that drives the cantilever and the output signal.

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Acknowledgements

KAP thanks the DFG for a Mercator Visiting Professorship at the Institute of Materials Physics, University of Muenster, Germany. VSS thanks the Indo-US Science and Technology Forum for a sabbatical research fellowship. The authors are grateful to Prof. R.Z. Valiev, Ufa Aviation Technical University, Russia, for supplying the ECAP specimens used in the study. They are also thankful to Dr. Satyam Suwas for his keen interest in this work. KSR thanks A. Sankaran for a discussion on twinning. The facilities provided by the School of Physics and the Centre for Nanotechnology, University of Hyderabad are acknowledged. The EBSD studies were carried out using the SEM facility at the Institute Nano-Science Initiative, Indian Institute of Science, Bangalore and Indian Institute of Technology, Madras, set up with a DST-FIST grant. GW thanks the DFG for support. The authors are thankful to Dr. R. Sundaresan, ARCI, Hyderabad for allowing the use of an annealing furnace.

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Authors and Affiliations

  1. School of Physics and Centre for Nanotechnology, University of Hyderabad, Hyderabad, 500 046, India

    K. Sitarama Raju, M. Ghanashyam Krishna & K. A. Padmanabhan

  2. School of Engineering Sciences & Technology, University of Hyderabad, Hyderabad, 500 046, India

    K. A. Padmanabhan

  3. Institute of Materials Physics, University of Muenster, Wilhelm-Klemm-Strasse 10, 48149, Muenster, Germany

    K. A. Padmanabhan & G. Wilde

  4. Department of Metallurgical and Materials Engineering, Indian Institute of Technology Madras, Chennai, 600 036, India

    V. Subramanya Sarma

  5. Department of Materials Engineering, Indian Institute of Science, Bangalore, 560 012, India

    N. P. Gurao

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  1. K. Sitarama Raju
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Correspondence to K. Sitarama Raju.

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Sitarama Raju, K., Ghanashyam Krishna, M., Padmanabhan, K.A. et al. Microstructure evolution and hardness variation during annealing of equal channel angular pressed ultra-fine grained nickel subjected to 12 passes. J Mater Sci 46, 2662–2671 (2011). https://doi.org/10.1007/s10853-010-5122-z

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