High-Temperature Scanning Indentation: A new method to investigate in situ metallurgical evolution along temperature ramps
Source abstract
Abstract
A new technique, High-Temperature Scanning Indentation (HTSI), is proposed to investigate metallurgical evolution occurring during anisothermal heat treatments. This technique is based on the use of high-speed nanohardness measurements carried out during linear thermal ramping of the system with appropriate settings. A specific high-speed loading procedure, based on a quarter sinus loading function, a creep segment and a three-step unloading method, permits the measurement of elastic, plastic and creep properties. The indentation cycle lasts one second to minimize thermal drift issues. This approach enables quasi-continuous measurements of elastic modulus and hardness as a function of temperature in much shorter times than previous techniques. The HTSI technique is validated on fused silica and pure aluminum. The application to cold-rolled aluminum undergoing thermal cycling highlights the potential of the HTSI technique to investigate in situ thermally activated mechanisms linked with microstructural changes such as viscoplasticity, static recovery and recrystallization mechanisms in metals. Results on aluminum were confirmed using Electron Back-Scattering Diffraction measurements.
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Research context
OpenAlex topics: Metal and Thin Film Mechanics · Microstructure and mechanical properties · Semiconductor materials and interfaces
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References (57)
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1. J.S.K.-L. Gibson, S. Schröders, C. Zehnder, S. Korte-Kerzel, On extracting mechanical properties from nanoindentation at temperatures up to 1000 °C. Extreme Mech. Lett. 17, 43 (2017)10.1016/j.eml.2017.09.007 ↗
2. B.D. Beake, A.J. Harris, J. Moghal, D.E.J. Armstrong, Temperature dependence of strain rate sensitivity, indentation size effects and pile-up in polycrystalline tungsten from 25 to 950 °C. Mater. Des. 156, 278 (2018)10.1016/j.matdes.2018.06.063 ↗
3. B.D. Beake, A.J. Harris, Nanomechanics to 1000 °C for high temperature mechanical properties of bulk materials and hard coatings. Vacuum 159, 17 (2019)10.1016/j.vacuum.2018.10.011 ↗
4. C. Minnert, W.C. Oliver, K. Durst, New ultra-high temperature nanoindentation system for operating at up to 1100 °C. Mater. Des. 192, 108727 (2020)10.1016/j.matdes.2020.108727 ↗
5. P. Baral, M. Laurent-Brocq, G. Guillonneau, J.-M. Bergheau, J.-L. Loubet, G. Kermouche, In situ characterization of AA1050 recrystallization kinetics using high temperature nanoindentation testing. Mater. Des. 152, 22 (2018)10.1016/j.matdes.2018.04.053 ↗
6. F.J. Humphreys, M. Hatherly, Recrystallization and Related Annealing Phenomena (Elsevier, Oxford, 2004).
7. J.M. Wheeler, P. Brodard, J. Michler, Elevated temperature, in situ indentation with calibrated contact temperatures. Phil. Mag. 92(25–27), 3128 (2012)10.1080/14786435.2012.674647 ↗
8. J.M. Wheeler, J. Michler, Indenter materials for high temperature nanoindentation. Rev. Sci. Instrum. 84(10), 101301 (2013)10.1063/1.4824710 ↗
9. J.M. Wheeler, High temperature nanoindentation: the state of the art and future challenges. Curr. Opin. Solid State Mater. Sci. 19(6), 354 (2015)10.1016/j.cossms.2015.02.002 ↗
10. N.M. Everitt, M.I. Davies, J.F. Smith, High temperature nanoindentation—the importance of isothermal contact. Phil. Mag. 91(7–9), 1221 (2011)10.1080/14786435.2010.496745 ↗
11. J.M. Wheeler, J. Michler, Elevated temperature, nano-mechanical testing in situ in the scanning electron microscope. Rev. Sci. Instrum. 84(4), 045103 (2013)10.1063/1.4795829 ↗
12. N. Bozzolo, S. Jacomet, R.E. Logé, Fast in-situ annealing stage coupled with EBSD: a suitable tool to observe quick recrystallization mechanisms. Mater. Charact. 70, 28 (2012)10.1016/j.matchar.2012.04.020 ↗
13. E.M. Lauridsen, S. Schmidt, S.F. Nielsen, L. Margulies, H.F. Poulsen, D.J. Jensen, Non-destructive characterization of recrystallization kinetics using three-dimensional X-ray diffraction microscopy. Scripta Mater. 55(1), 51 (2006)10.1016/j.scriptamat.2006.02.028 ↗
14. F. Christien, M.T.F. Telling, K.S. Knight, R. Le Gall, A method for the monitoring of metal recrystallization based on the in-situ measurement of the elastic energy release using neutron diffraction. Rev. Sci. Instrum. 86(5), 053901 (2015)10.1063/1.4919414 ↗
15. E.M. Lauridsen, H.F. Poulsen, S.F. Nielsen, D. Juul Jensen, Recrystallization kinetics of individual bulk grains in 90% cold-rolled aluminium. Acta Mater. 51(15), 4423 (2003)10.1016/S1359-6454(03)00278-7 ↗
16. M.A.Z. Vasconcellos, R.P. Livi, M.N. Baibich, Comparative study of isothermal and isochronal crystallisation of metallic glasses. J. Phys. F: Met. Phys. 18, 1343 (1988)10.1088/0305-4608/18/7/005 ↗
17. J.M. Pelletier, J. Perez, J.L. Soubeyroux, Physical properties of bulk amorphous glasses: influence of physical aging and onset of crystallisation. J. Non-Cryst. Solids 274(1), 301 (2000)10.1016/S0022-3093(00)00221-0 ↗
18. T. Fukami, K. Okabe, D. Okai, T. Yamasaki, T. Zhang, A. Inoue, Crystal growth and time evolution in Zr–Al–Cu–Ni glassy metals in supercooled liquid. Mater. Sci. Eng. B 111(2), 189 (2004)10.1016/S0921-5107(04)00204-1 ↗
19. T.G. Nieh, C. Iwamoto, Y. Ikuhara, K.W. Lee, Y.W. Chung, Comparative studies of crystallization of a bulk Zr–Al–Ti–Cu–Ni amorphous alloy. Intermetallics 12(10), 1183 (2004)10.1016/j.intermet.2004.04.011 ↗
20. Z. Zhang, J. Xie, Influence of relaxation and crystallization on micro-hardness and deformation of bulk metallic glass. Mater. Sci. Eng. A 407(1), 161 (2005)10.1016/j.msea.2005.07.020 ↗
21. M. Apreutesei, A. Billard, P. Steyer, Crystallization and hardening of Zr-40at.% Cu thin film metallic glass: Effects of isothermal annealing. Mater. Des 86, 555 (2015)10.1016/j.matdes.2015.07.149 ↗
22. M. Idriss, F. Célarié, Y. Yokoyama, F. Tessier, T. Rouxel, Evolution of the elastic modulus of Zr–Cu–Al BMGs during annealing treatment and crystallization: role of Zr/Cu ratio. J. Non-Cryst. Solids 421, 35 (2015)10.1016/j.jnoncrysol.2015.04.028 ↗
23. Z. Wang, Influences of sample preparation on the indentation size effect and nanoindentation pop-in on nickel (2012)
24. W.D. Nix, H. Gao, Size effects in crystalline: a law for strain gradient plasticity. J. Mech. Phys. Solids 46(3), 411 (1998)10.1016/S0022-5096(97)00086-0 ↗
25. O. Franke, J.C. Trenkle, C.A. Schuh, Temperature dependence of the indentation size effect. J. Mater. Res. 25(7), 1225 (2010)10.1557/JMR.2010.0159 ↗
26. R.D. Doherty, D.A. Hughes, F.J. Humphreys, J.J. Jonas, D.J. Jensen, M.E. Kassner, W.E. King, T.R. McNelley, H.J. McQueen, A.D. Rollett, Current issues in recrystallization: a review. Mater. Sci. Eng. A 238, 219 (1997)10.1016/S0921-5093(97)00424-3 ↗
27. B.N. Lucas, W.C. Oliver, Indentation power-law creep of high-purity indium. Metall. Mater. Trans. A 30(3), 601 (1999)10.1007/s11661-999-0051-7 ↗
28. G. Kermouche, J.L. Loubet, J.M. Bergheau, Cone indentation of time-dependent materials: the effects of the indentation strain rate. Mech. Mater. 39(1), 24 (2007)10.1016/j.mechmat.2006.02.005 ↗
29. A.H.W. Ngan, H.T. Wang, B. Tang, K.Y. Sze, Correcting power-law viscoelastic effects in elastic modulus measurement using depth-sensing indentation. Int. J. Solids Struct. 42(5–6), 1831 (2005)10.1016/j.ijsolstr.2004.07.018 ↗
30. W.C. Oliver, G.M. Pharr, An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7(6), 1564 (1992)10.1557/JMR.1992.1564 ↗
31. J.L. Loubet, M. Bauer, A. Tonck, S. Bec, B. Gauthier-Manuel, in Mechanical properties and deformation behavior of materials having ultra-fine microstructures. ed. by M. Nastasi, D.M. Parkin, H. Gleiter (Springer, Netherlands, Dordrecht, 1993), pp. 429–44710.1007/978-94-011-1765-4_28 ↗
32. P. Baral, G. Kermouche, G. Guillonneau, G. Tiphene, J.-M. Bergheau, W.C. Oliver, J.-L. Loubet, Indentation creep vs. indentation relaxation: a matter of strain rate definition? Mater. Sci. Eng. A 781, 139246 (2020)10.1016/j.msea.2020.139246 ↗
33. G. Kermouche, J.L. Loubet, J.M. Bergheau, Extraction of stress–strain curves of elastic–viscoplastic solids using conical/pyramidal indentation testing with application to polymers. Mech. Mater. 40(4–5), 271 (2008)10.1016/j.mechmat.2007.08.003 ↗
34. O.D. Sherby, P.E. Armstrong, Prediction of activation energies for creep and self-diffusion from hot hardness data. Metall. Mater. Trans. B 2(12), 3479 (1971)10.1007/BF02811630 ↗
35. J.W. Marx, J.M. Sivertsen, Temperature dependence of the elastic moduli and internal friction of silica and glass. J. Appl. Phys. 24(1), 81 (1953)10.1063/1.1721138 ↗
36. S. Spinner, Elastic moduli of glasses at elevated temperatures by a dynamic method. J. Am. Ceram. Soc. 39(3), 113 (1956)10.1111/j.1151-2916.1956.tb15634.x ↗
37. S. Spinner, G.W. Cleek, Temperature dependence of young’s modulus of vitreous germania and silica. J. Appl. Phys. 31(8), 1407 (1960)10.1063/1.1735852 ↗
38. J.A. Bucaro, H.D. Dardy, High-temperature Brillouin scattering in fused quartz. J. Appl. Phys. 45(12), 5324 (1974)10.1063/1.1663238 ↗
39. B.D. Beake, High-temperature nanoindentation testing of fused silica and other materials. Phil. Mag. Part A 82(10), 2179 (2002)10.1080/01418610208235727 ↗
40. C.A. Schuh, C.E. Packard, A.C. Lund, Nanoindentation and contact-mode imaging at high temperatures. J. Mater. Res. 21(3), 725 (2006)10.1557/jmr.2006.0080 ↗
41. G. Simmons, H. Wang, Single Crystal Elastic Constants and Calculated Aggregate Properties: A Handbook (MIT Press, Cambridge, 1971).
42. P. Ludwik, Über die Änderung der inneren Reibung der Metalle mit der Temperatur. Zeitschrift für Physikalische Chemie 91U(1), 232 (1916)10.1515/zpch-1916-9112 ↗
43. J.M. Wheeler, V. Maier, K. Durst, M. Göken, J. Michler, Activation parameters for deformation of ultrafine-grained aluminium as determined by indentation strain rate jumps at elevated temperature. Mater. Sci. Eng. A 585, 108 (2013)10.1016/j.msea.2013.07.033 ↗
44. P.S. Phani, W.C. Oliver, A direct comparison of high temperature nanoindentation creep and uniaxial creep measurements for commercial purity aluminum. Acta Mater. 111, 31 (2016)10.1016/j.actamat.2016.03.032 ↗
45. J. Shen, S. Yamasaki, K. Ikeda, S. Hata, H. Nakashima, Low-temperature creep at ultra-low strain rates in pure aluminum studied by a helicoid spring specimen technique. Mater. Trans. 52(7), 1381 (2011)10.2320/matertrans.M2010405 ↗
46. D. Tabor, The hardness of solids. RevPhysTech 1(3), 145 (1970)
47. D. Tumbajoy-Spinel, X. Maeder, G. Guillonneau, S. Sao-Joao, S. Descartes, J.-M. Bergheau, C. Langlade, J. Michler, G. Kermouche, Microstructural and micromechanical investigations of surface strengthening mechanisms induced by repeated impacts on pure iron. Mater. Des. 147, 56 (2018)10.1016/j.matdes.2018.03.014 ↗
48. M. Richou, A. Durif, M. Lenci, M. Mondon, M. Minissale, L. Gallais, G. Kermouche, G. De Temmerman, Recrystallization at high temperature of two tungsten materials complying with the ITER specifications. J. Nucl. Mater. 542, 152418 (2020)10.1016/j.jnucmat.2020.152418 ↗
49. A. Leitner, V. Maier-Kiener, D. Kiener, Dynamic nanoindentation testing: is there an influence on a material’s hardness? Mater. Res. Lett. 5(7), 486 (2017)10.1080/21663831.2017.1331384 ↗
50. J.C. Trenkle, C.E. Packard, C.A. Schuh, Hot nanoindentation in inert environments. Rev. Sci. Instrum. 81(7), 073901 (2010)10.1063/1.3436633 ↗
51. F. Bachmann, R. Hielscher, H. Schaeben, Grain detection from 2d and 3d EBSD data—specification of the MTEX algorithm. Ultramicroscopy 111(12), 1720 (2011)10.1016/j.ultramic.2011.08.002 ↗
52. F. Roudet, Propriétés mécaniques par indentation multi-échelles des matériaux bio-sourcés aux céramiques (2015)
53. P. Sudharshan Phani, W.C. Oliver, A critical assessment of the effect of indentation spacing on the measurement of hardness and modulus using instrumented indentation testing. Mater. Des. 164, 107563 (2019)10.1016/j.matdes.2018.107563 ↗
54. K. Demmou, Nanoindentation (Viscoplasticité & Piézo-Mécanique de Films de Dithio-Phosphate de Zinc Triboformés, These, Ecole Centrale de Lyon, 2007).
55. S. Bec, A. Tonck, J.-M. Georges, E. Georges, J.-L. Loubet, Improvements in the indentation method with a surface force apparatus. Philos. Mag. A 74(5), 1061 (1996)10.1080/01418619608239707 ↗
56. G. Guillonneau, Nouvelles Techniques de Nano-Indentation Pour Des Conditions Expérimentales Difficiles : Très Faibles Enfoncements (Surfaces Rugueuses, Température, These, Ecully, Ecole Centrale de Lyon, 2012).
57. G. Guillonneau, J.M. Wheeler, J. Wehrs, L. Philippe, P. Baral, H.W. Höppel, M. Göken, J. Michler, Determination of the true projected contact area by in situ indentation testing. J. Mater. Res. 34(16), 2859 (2019)10.1557/jmr.2019.236 ↗