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Development of High Temperature Nanoindentation Methodology and its Application in the Nanoindentation of Polycrystalline Tungsten in Vacuum to 950 °C

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Abstract

The capability for high temperature nanoindentation measurements to 950 °C in high vacuum has been demonstrated on polycrystalline tungsten, a material of great importance for nuclear fusion and spallation applications and as a potential high temperature nanomechanics reference sample. It was possible to produce measurements with minimal thermal drift (typically ~0.05 nm/s at 750–950 °C) and no visible oxidative damage. The temperature dependence of the hardness, elastic modulus, plasticity index, creep, creep strain, and creep recovery were investigated over the temperature range, testing at 25, 750, 800, 850, 900 and 950 °C. The nanoindentation hardness measurements were found to be consistent with previous determinations by hot microhardness. Above 800 °C the hardness changes relatively little but more pronounced time-dependent deformation and plasticity were observed from 850 °C. Plasticity index, indentation creep and creep recovery all increase with temperature. The importance of increased time-dependent deformation and pile-up on the accuracy of the elastic modulus measurements are discussed. Elastic modulus measurements determined from elastic analysis of the unloading curves at 750–800 °C are close to literature bulk values (to within ~11 %). The high temperature modulus measurements deviate more from bulk values determined taking account of the high temperature properties of the indenter material at the point (850 °C) at which more significant time-dependent deformation is observed. This is thought to be due to the dual influence of increased time-dependency and pile-up that are not being accounted for in the elastic unloading analysis. Accounting for this time-dependency by applying a viscoelastic compliance correction developed by G. Feng and A.H.W. Ngan (J. Mater. Res. (2002) 17:660–668) greatly reduces the values of the elastic modulus, so they are agree to within 6 % of literature values at 950 °C.

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Acknowledgments

DEJA acknowledges The Royal Academy of Engineering for a Research Fellowship at the University of Oxford and the Culham Centre for Fusion Energy for funding via a Research Fellowship at St Edmund Hall, Oxford.

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Authors and Affiliations

  1. Micro Materials Ltd, Willow House, Ellice Way, Yale Business Village, Wrexham, LL13 7YL, UK

    A. J. Harris, B. D. Beake & M. I. Davies

  2. Department of Materials, University of Oxford, Parks Road, Oxford, OX1 3PH, UK

    D. E. J. Armstrong

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Harris, A.J., Beake, B.D., Armstrong, D.E.J. et al. Development of High Temperature Nanoindentation Methodology and its Application in the Nanoindentation of Polycrystalline Tungsten in Vacuum to 950 °C. Exp Mech 57, 1115–1126 (2017). https://doi.org/10.1007/s11340-016-0209-3

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