Abstract
An in situ electrical measurement technique for the investigation of nanoindentation using a Hysitron Triboindenter is described, together with details of experiments to address some technical issues associated with the technique. Pressure-induced phase transformations in silicon during indentation are of particular interest but are not fully understood. The current in situ electrical characterization method makes use of differences in electrical properties of the phase-transformed silicon to better understand the sequence of transformations that occur during loading and unloading. Here, electric current is measured through the sample/indenter tip during indentation, with a fixed or variable voltage applied to the sample. This method allows both current monitoring during indentation and the extraction of current-voltage (I-V) characteristics at various stages of loading. The work presented here focuses on experimental issues that must be understood for a full interpretation of results from nanoindentation experiments in silicon. The tip/sample contact and subsurface electrical resistivity changes dominate the resultant current measurement. Extracting the component of contact resistance provides an extremely sensitive method for measuring the electrical properties of the material immediately below the indenter tip, with initial results from indentation in silicon showing that this is a very sensitive probe of subsurface structural and electrical changes.
Similar content being viewed by others
References
J.Z. Hu, L.D. Merkle, C.S. Menoni, and I.L. Spain: Crystal data for high-pressure phases of silicon. Phys. Rev. B 34, 4679 (1986).
R.O. Piltz, J.R. Maclean, S.J. Clark, G.J. Auckland, P.D. Hatton, and J. Crain: Structure and properties of silicon XII: A complex tetrahedrally bonded phase. Phys. Rev. B 52, 4072 (1995).
J. Crain, G.J. Ackland, J.R. Maclean, R.O. Piltz, P.D. Hatton, and G.S. Pawley: Reversible pressure-induced structural transitions between metastable phases of silicon. Phys. Rev. B 50, 13043 (1994).
V. Domnich, Y. Gogotsi, and S. Dub: Effect of phase transformations on the shape of the unloading curve in the nanoindentation of silicon. Appl. Phys. Lett. 76, 2214 (2000).
J.E. Bradby, J.S. Williams, J. Wong-Leung, M.V. Swain, and P. Munroe: Mechanical deformation in silicon by micro-indentation. J. Mater. Res. 16, 1500 (2001).
J.E. Bradby, J.S. Williams, J. Wong-Leung, M.V. Swain, and P. Munroe: Transmission electron microscopy observation of deformation microstructure under spherical indentation in silicon. Appl. Phys. Lett. 77, 3749 (2000).
D.R. Clarke, M.C. Kroll, P.D. Kirchner, R.F. Cook, and B.J. Hockey: Amorphization and conductivity of silicon and germanium induced by indentation. Phys. Rev. Lett. 60, 2156 (1988).
A. Kailer, Y.G. Gogotsi, and K.G. Nickel: Phase transformations of silicon caused by contact loading. J. Appl. Phys. 81, 3057 (1997).
J.E. Bradby, J.S. Williams, and M.V. Swain: In situ electrical characterization of phase transformations in Si during indentation. Phys. Rev. B67, 085205 (2003).
G.M. Pharr, W.C. Oliver, and D.S. Harding: New evidence for a pressure-induced phase transformation during the indentation of silicon. J. Mater. Res. 6, 1129 (1991).
G.M. Pharr, W.C. Oliver, R.F. Cook, P.D. Kirchner, M.C. Kroll, T.R. Dinger, and D.R. Clarke: Electrical resistance of metallic contacts on silicon and germanium during indentation. J. Mater. Res. 7, 961 (1992).
E.R. Weppelmann, J.S. Field, and M.V. Swain: Observation, analysis, and simulation of the hysteresis of silicon using ultra-micro-indentation with spherical indenters. J. Mater. Res. 8, 830 (1993).
J.S. Williams, Y. Chen, J. Wong-Leung, A. Kerr, and M.V. Swain: Ultra-micro-indentation of silicon and compound semiconductors with spherical indenters. J. Mater. Res. 14, 2338 (1999).
Y.G. Gogotsi, V. Domnich, S.N. Dub, A. Kailer, and K.G. Nickel: Cyclic nanoindentation and Raman microspectroscopy study of phase transformations in semiconductors. J. Appl. Phys. 15, 871 (2000).
A.B. Mann, D. van Heerden, J.B. Pethica, P. Bowes, and T.P. Weihs: Contact resistance and phase transformations during nanoindentation of silicon. Philos. Mag. A. 82, 1921 (2002).
A.B. Mann, D. van Heerden, J.B. Pethica, and T.P. Weihs: Size dependent phase transformation during point loading of silicon. J. Mater. Res. 15, 1754 (2000).
Hysitron Incorporated: Quoted Tip Resistivity (Hysitron, Inc., Minneapolis, MN, 2005).
E.H. Rhoderickand R.H. Williams: Metal-Semiconductor Contacts (Oxford University Press, Oxford, UK, 1988).
A.C. Fischer-Cripps: Nanoindentation Mechanical Engineering Series (Springer-Verlag: New York, 2004).
G.L. Pearson: Pressure dependence of the resistivity of silicon. Phys. Rev. 98, 1755 (1955).
T.Y. Zhangand W.H. Xu: Surface effects on nanoindentation. J. Mater. Res. 17, 1715 (2002).
B. Bhushanand X. Li: Micromechanical and tribological characterization of doped single-crystal silicon and polysilicon films for microelectromechanical systems devices. J. Mater. Res. 12, 59 (1997).
Private communication, Hysitron Incorporated.
J-i. Jang, M.J. Lance, S. Wen, T.Y. Tsui, and G.M. Pharr: Indentation-induced phase transformations in silicon: Influences of load, rate and indenter angle on the transformation behavior. Acta Mater. 53, 1759 (2005).
Y. Gogotsi, T. Miletich, M. Gardner, and M. Rosenberg: Microindentation device for in situ study of pressure-induced phase transformations. Rev. Sci. Instrum. 70, 4612 (1999).
M. Werner, R. Job, A. Denisenko, A. Zaitsev, W.R. Fahrner, C. Johnston, P.R. Chalker, and I.M. Buckley-Golder: How to fabricate low-resistance metal-diamond contacts. Diamond Relat. Mater. 5, 723 (1996).
Y. Chen, M. Ogura, S. Yamasaki, and H. Okushi: Ohmic contacts on p-type homoepitaxial diamond and their thermal stability. Semicond. Sci. Technol. 20, 860 (2005).
C. Uzan-Saguy, R. Kalish, R. Walker, D.N. Jamieson, and S. Prawer: Formation of delta-doped, buried conducting layers in diamond, by high-energy, B-ion implantation. Diamond Relat. Mater. 7, 1429 (1998).
A.T. Collins: Properties and Growth of Diamond edited by G. Davies (Inspec: London, 1994), p. 273.
S. Jeffery, C.J. Sofield, and J.B. Pethica: The influence of mechanical stress on the dielectric breakdown field strength of thin SiO2 films. Appl. Phys. Lett. 73, 172 (1998).
S.A. Syed Asif, K.J. Wahl, and R.J. Colton: The influence of oxide and adsorbates on the nanomechanical response of silicon surfaces. J. Mater. Res. 15, 546 (2000).
R. Hsiaoand D. Bogy: Nanoindentation Characteristics of Silicon: Application Notes (Hysitron Incorporated, Minneapolis, MN, 2003).
T. Juliano, V. Domnich, and Y. Gogotsi: Examining pressure-induced phase transformations in silicon by spherical indentation and Raman spectroscopy: A statistical study. J. Mater. Res. 19, 3099 (2004).
T. Juliano, Y. Gogotsi, and V. Domnich: Effect of indentation unloading conditions on phase transformation induced events in silicon. J. Mater. Res. 18, 1192 (2003).
S. Ruffell, J.E. Bradby, and J.S. Williams: Identification of nanoindentation-induced phase changes in silicon by in-situ electrical characterization. J. Appl. Phys. (2007, submitted).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Ruffell, S., Bradby, J.E., Williams, J.S. et al. An in situ electrical measurement technique via a conducting diamond tip for nanoindentation in silicon. Journal of Materials Research 22, 578–586 (2007). https://doi.org/10.1557/jmr.2007.0100
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/jmr.2007.0100