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The indentation hardness of silicon measured by instrumented indentation: What does it mean?

Published online by Cambridge University Press:  05 December 2012

Bianca Haberl ,
Leonardus Bimo Bayu Aji ,
J.S. Williams  and
Jodie E. Bradby
Bianca Haberl*
Affiliation:
Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, Australian Capital Territory 0200, Australia
Leonardus Bimo Bayu Aji
Affiliation:
Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, Australian Capital Territory 0200, Australia
J.S. Williams
Affiliation:
Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, Australian Capital Territory 0200, Australia
Jodie E. Bradby
Affiliation:
Department of Electronic Materials Engineering, Research School of Physics and Engineering, The Australian National University, Canberra, Australian Capital Territory 0200, Australia
*
a)Address all correspondence to this author. e-mail: bianca.haberl@anu.edu.au
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Abstract

The indentation hardness of three different pure forms of silicon was investigated by two different methods. The hardness was probed by direct imaging of the residual impressions and by instrumented indentation using the Oliver–Pharr method. The forms of silicon used were a defective form of amorphous silicon, an amorphous form close to a continuous random network, and a crystalline silicon. The first form deforms via plastic flow and the latter two via phase transition. Two different unloading rates, fast and slow, were used to vary the phase transition behavior. This influenced the relative hardness as measured by instrumented indentation, which is not a reliable method to quantify hardness values in phase transforming materials. Thus, for our phase transforming silicon system, the relative hardness between samples can only be determined correctly by direct imaging, provided that the image accurately reveals the extent of the phase transformed volume.

Keywords

hardnessSiphase transformation
Type
Articles
Information
Journal of Materials Research , Volume 27 , Issue 24 , 28 December 2012 , pp. 3066 - 3072
Copyright
Copyright © Materials Research Society 2012

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References

REFERENCES

Gridneva, V., Milman, Y.V., and Trefilov, V.I.: Phase transition in diamond-structure crystals during hardness measurements. Phys. Status Solidi A 14, 77 (1972).CrossRefGoogle Scholar
Gerk, P. and Tabor, D.: Indentation hardness and semiconductor-metal transition of germanium and silicon. Nature 271, 732 (1978).CrossRefGoogle Scholar
Mujica, A., Rubio, A., Muñoz, A., and Needs, R.J.: High-pressure phases of group-IV, III-V, and II-VI compounds. Rev. Mod. Phys. 75, 863 (2003).CrossRefGoogle Scholar
Ackland, G.J.: High-pressure phases of group IV and III-V semiconductors. Rep. Prog. Phys. 64, 483 (2001).CrossRefGoogle Scholar
Pharr, G.M., Oliver, W.C., and Harding, D.S.: New evidence for a pressure-induced phase transformation during the indentation of silicon. J. Mater. Res. 6, 1129 (1991).CrossRefGoogle Scholar
Bradby, J.E., Williams, J.S., Wong-Leung, J., Swain, M.V., and Munroe, P.: Transmission electron microscopy observation of deformation microstructure under spherical indentation in silicon. Appl. Phys. Lett. 77, 3749 (2000).CrossRefGoogle Scholar
Bradby, J.E., Williams, J.S., Wong-Leung, J., Swain, M.V., and Munroe, P.: Mechanical deformation in silicon by micro-indentation. J. Mater. Res. 16, 1500 (2001).CrossRefGoogle Scholar
Pharr, G.M., Oliver, W.C., Cook, R.F., Kirchner, P.D., Kroll, M.C., Dinger, T.R., and Clarke, D.R.: Electrical resistance of metallic contacts on silicon and germanium during indentation. J. Mater. Res. 7, 961 (1992).CrossRefGoogle Scholar
Vandeperre, L.J., Guiliani, F., Lloyd, S.J., and Clegg, W.J.: The hardness of silicon and germanium. Acta Mater. 55, 6307 (2007).CrossRefGoogle Scholar
Kailer, A., Nickel, K.G., and Gogotsi, Y.G.: Raman microspectroscopy of nanocrystalline and amorphous phases in hardness indentations. J. Raman Spectrosc. 30, 939 (1999).3.0.CO;2-C>CrossRefGoogle Scholar
Domnich, V. and Gogotsi, Y.: Phase transformations in silicon under contact loading. Rev. Adv. Mater. Sci. 3, 1 (2002).Google Scholar
Field, J.S. and Swain, M.V.: A simple predictive model for spherical indentation. J. Mater. Res. 8, 297 (1993).CrossRefGoogle Scholar
Oliver, W.C. and Pharr, G.M.: An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7, 1564 (1992).CrossRefGoogle Scholar
Williamson, D.L., Roorda, S., Chicoine, M., Tabti, R., Stolk, P.A., Acco, S., and Saris, F.W.: On the nanostructure of pure amorphous silicon. Appl. Phys. Lett. 67, 226 (1995).CrossRefGoogle Scholar
Haberl, B., Bradby, J.E., Swain, M.V., Williams, J.S., and Munroe, P.: Phase transformations induced in relaxed amorphous silicon by indentation at room temperature. Appl. Phys. Lett. 85, 5559 (2004).CrossRefGoogle Scholar
Haberl, B., Bradby, J.E., Ruffell, S., Williams, J.S., and Munroe, P.: Phase transformations induced by spherical indentation in ion-implanted amorphous silicon. J. Appl. Phys. 100, 013520 (2006).CrossRefGoogle Scholar
Williams, J.S., Field, J.S., and Swain, M.V.: Mechanical Property Characterisation of Crystalline, Ion Implantation Amorphised and Annealed Relaxed Silicon with Spherical Indenters, in Symposium M1 - Thin Films: Stresses and Mechanical Properties IV, edited by Townsend, P.H., Weihs, T.P., and Sanchez, P.B.J.E. Jr. (Mater. Res. Soc. Symp. Proc. 308, Pittsburgh, PA, 1990) p. 571.Google Scholar
Williams, J.S., Chen, Y., Wong-Leung, J., Kerr, A., and Swain, M.V.: Ultra-micro-indentation of silicon and compound semiconductors with spherical indenters. J. Mater. Res. 14, 2338 (1999).CrossRefGoogle Scholar
Follstaedt, D.M., Knapp, J.A., and Myers, S.M.: Mechanical properties of ion-implanted amorphous silicon. J. Mater. Res. 14, 338 (2004).CrossRefGoogle Scholar
Nagy, P.M., Aranyi, D., Horváth, P., Petö, G., and Kálmán, E.: Nanomechanical properties of ion-implanted Si. Surf. Interface Anal. 40, 875 (2008).CrossRefGoogle Scholar
Roorda, S., Sinke, W.C., Potae, J.M., Jacobson, D.C., Dierker, S., Dennis, B.S., Eaglesham, D.J., Spaepen, F., and Fuoss, P.: Structural relaxation and defect annihilation in pure amorphous silicon. Phys. Rev. B 44, 3702 (1991).CrossRefGoogle ScholarPubMed
Laaziri, K., Kycia, S., Roorda, S., Chicoine, M., Robertson, J.L., Wang, J., and Moss, S.C.: High-energy x-ray diffraction study of pure amorphous silicon. Phys. Rev. B 60, 13520 (1999).CrossRefGoogle Scholar
Urli, X., Dias, C.L., Lewis, L.J., and Roorda, S.: Point defects in pure amorphous silicon and their role in structural relaxation: A tight-binding molecular-dynamics study. Phys. Rev. B 77, 155204 (2008).CrossRefGoogle Scholar
Haberl, B., Liu, A.C.Y., Bradby, J.E., Ruffell, S., Williams, J.S., and Munroe, P.: Structural characterization of pressure-induced amorphous silicon. Phys. Rev. B 79, 155209 (2009).CrossRefGoogle Scholar
Fujisawa, N. and Swain, M.V.: On the indentation contact area of a creeping solid during constant-strain-rate loading by a sharp indenter. J. Mater. Res. 22, 893 (2007).CrossRefGoogle Scholar
Oliver, W.C. and Pharr, G.M.: Measurement of hardness and elastic modulus by instrumented indentations: Advances in understanding and refinements to methodology. J. Mater. Res. 19, 3 (2004).CrossRefGoogle Scholar
Tsui, T.Y. and Pharr, G.M.: Substrate effects on nanoindentation mechanical property measurement of soft films on hard substrates. J. Mater. Res. 14, 292 (1999).CrossRefGoogle Scholar
Bradby, J.E., Williams, J.S., and Swain, M.V.: In situ electrical characterization of phase transformations in Si during indentation. Phys. Rev. B 67, 085205 (2003).CrossRefGoogle Scholar
Hysitron, TriboScan. (Minneapolis, MN, 2011).Google Scholar
Rusband, W.: ImageJ 1.41o (National Institutes of Health, Bethesda, MD, 2008). http://rsb.info.nih.gov/ij/.Google Scholar
Tabor, D.: The Hardness of Metals (Oxford University Press, Oxford, UK, 1951).Google Scholar
Durandurdu, M. and Drabold, D.A.: High-pressure phases of amorphous and crystalline silicon. Phys. Rev. B 67, 212101 (2003).CrossRefGoogle Scholar
Ivashchenko, V.I., Turchi, P.E.A., and Shevchenko, V.I.: Simulations of indentation-induced phase transformations in crystalline and amorphous silicon. Phys. Rev. B 78, 035205 (2008).CrossRefGoogle Scholar
Piltz, R.O., Maclean, J.R., Clark, S.J., Ackland, G.J., Hatton, P.D., and Crain, J.: Structure and properties of silicon XII: A complex tetrahedrally bonded phase. Phys. Rev. B 52, 4072 (1995).CrossRefGoogle ScholarPubMed
Ruffell, S., Bradby, J.E., Williams, J.S., and Munroe, P.: Formation and growth of nanoindentation-induced high pressure phases in crystalline and amorphous silicon. J. Appl. Phys. 102, 063521 (2007).CrossRefGoogle Scholar
Haberl, B.: Structural characterization of amorphous silicon. Ph.D. Thesis, Australian National University, Canberra, Australian Capital Territory, Australia, 2010.Google Scholar
Ruffell, S., Bradby, J.E., and Williams, J.S.: High pressure crystalline phase formation during nanoindentation: Amorphous versus crystalline silicon. J. Appl. Phys. 89, 091919 (2006).Google Scholar
Fujisawa, N., Williams, J.S., and Swain, M.V.: On the cyclic indentation behaviour of crystalline silicon with a sharp tip. J. Mater. Res. 22, 2992 (2007).CrossRefGoogle Scholar