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Examining pressure-induced phase transformations in silicon by spherical indentation and Raman spectroscopy: A statistical study

Published online by Cambridge University Press:  01 October 2004

Tom Juliano ,
Vladislav Domnich  and
Yury Gogotsi
Tom Juliano
Affiliation:
A.J. Drexel Nanotechnology Institute and Department of Materials Science and Engineering, Drexel University, Philadelphia, Pennsylvania 19104
Vladislav Domnich
Affiliation:
A.J. Drexel Nanotechnology Institute and Department of Materials Science and Engineering, Drexel University, Philadelphia, Pennsylvania 19104
Yury Gogotsi*
Affiliation:
A.J. Drexel Nanotechnology Institute and Department of Materials Science and Engineering, Drexel University, Philadelphia, Pennsylvania 19104
*
a) Address all correspondence to this author. e-mail: [email protected]
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Abstract

Unloading rate and maximum load have been previously shown to affect the response of silicon to sharp indentation, but no such study exists for spherical indentation. In this work, a statistical analysis of over 1900 indentations made with a 13.5-μm radius spherical indenter on a single-crystal silicon wafer over a range of loads (25–700 mN) and loading/unloading rates (1–30 mN/s) is presented. The location of “pop-in” and “pop-out” events, most likely due to pressure-induced phase transformations, is noted, as well as pressures at which they occur. Multiple occurrences of pop-in and pop-out events are reported. Raman micro-spectroscopy shows a higher intensity of metastable silicon phases at some depth under the surface of the residual impression, where the highest shear stresses are present. A stability range for Si-II is demonstrated and compared with previous results for Berkovich indentation.

Keywords

Raman spectroscopyIndentationPhase transformation
Type
Articles
Information
Journal of Materials Research , Volume 19 , Issue 10 , October 2004 , pp. 3099 - 3108
Copyright
Copyright © Materials Research Society 2004

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References

REFERENCES

1Jamieson, J.C.: Crystal structures at high pressures of metallic modifications of silicon and germanium. Science 139, 762 (1963).CrossRefGoogle ScholarPubMed
2Hu, J.Z., Merkle, L.D., Menoni, C.S. and Spain, I.L.: Crystal data for high-pressure phases of silicon. Phys. Rev. B 34, 4679 (1986).CrossRefGoogle ScholarPubMed
3Crain, J., Ackland, G.J., Maclean, J.R., Piltz, R.O., Hatton, P.D. and Pawley, G.S.: Reversible pressure-induced structural transitions between metastable phases of silicon. Phys. Rev. B 50, 13043 (1994).CrossRefGoogle ScholarPubMed
4Piltz, 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
5Wentorf, R.H. and Kasper, J.S.: Two new forms of silicon. Science 139, 338 (1963).CrossRefGoogle Scholar
6Kailer, A., Gogotsi, Y.G. and Nickel, K.G.: Phase transformations of silicon caused by contact loading. J. Appl. Phys. 81, 3057 (1997).CrossRefGoogle Scholar
7Williams, 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
8Zarudi, I. and Zhang, L.C.: Structure changes in mono-crystalline silicon subjected to indentation - experimental findings. Tribol. Int. 32, 701 (1999).CrossRefGoogle Scholar
9Mann, A.B., van Heerden, D., Pethica, J.B. and Weihs, T.P.: Size-dependent phase transformations during point loading of silicon. J. Mater. Res. 15, 1754 (2000).CrossRefGoogle Scholar
10Bradby, 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
11Domnich, V., Gogotsi, Y. and Dub, S.: Effect of phase transformations on the shape of the unloading curve in the nanoindentation of silicon. Appl. Phys. Lett. 76,2214 (2000).Google Scholar
12Bradby, 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
13Ge, D., Domnich, V. and Gogotsi, Y.: High-resolution transmission-electron-microscopy study of metastable silicon phases produced by nanoindentation. J. Appl. Phys. 93, 2418 (2003).CrossRefGoogle Scholar
14Bradby, 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).Google Scholar
15Zarudi, I., Zou, J. and Zhang, L.C.: Microstructures of phases in indented silicon: A high resolution characterization. Appl. Phys. Lett. 82,874 (2003).Google Scholar
16Weppelmann, E.R., Field, J.S. and Swain, M.V.: Observation, analysis and simulation of the hysteresis of silicon using ultra-micro-indentation with spherical indenters. J. Mater. Res. 8, 830 (1993).CrossRefGoogle Scholar
17Weppelmann, E.R., Field, J.S. and Swain, M.V.: Influence of spherical indentor radius on the indentation-induced transformation behavior of silicon. J. Mater. Sci. 30,2455 (1995).CrossRefGoogle Scholar
18Juliano, T., Domnich, V. and Gogotsi, Y.: The effect of indentation loading conditions on the phase transformation induced events in silicon. J. Mater. Res. 18, 1192 (2003).CrossRefGoogle Scholar
19Aspnes, D.E. and Studna, A.A.: Dielectric functions and optical properties of Si, Ge, GaP, GaAs, GaSb, InP, InAs, and InSb from 1.5 to 6.0 eV. Phys. Rev. B 27, 985 (1983).Google Scholar
20Carlson, D.E. and Wronski, C.R.: Amorphous Silicon Solar Cells in Amorphous Semiconductors (Springer, New York, 1979), pp. 287–330Google Scholar
21Johnson, K.L.: Contact Mechanics (Cambridge University Press, Cambridge, U.K., 1985), p. 452Google Scholar
22Field, J.S. and Swain, M.V.: A simple predictive model for spherical indentation. J. Mater. Res. 8, 297 (1993).CrossRefGoogle Scholar
23Iwashita, N., Swain, M., Field, J.S., Ohta, N. and Bitoh, S.: Elasto-plastic deformation of glass-like carbons heat-treated at different temperatures. Carbon 39, 1525 (2001).CrossRefGoogle Scholar
24Juliano, T., Domnich, V., Buchheit, T. and Gogotsi, Y. Numerical derivative analysis of load-displacement curves in depth-sensing indentation. In Mechanical Properties of Nanostructured Materials and Nanocomposites, edited by Ovid’ko, I., Pande, C.S., Krishnamoorti, R., Lavernia, E., and Skandan, G. (Mater. Res. Soc. Symp. Proc. 791, Warrendale, PA, 2004), p. 191 (Q7.5.1-Q7.5.11)Google Scholar
25Armstrong, R.W., Ruff, A.W. and Shin, H.: Elastic, plastic and cracking indentation behavior of silicon crystals. Mater. Sci. Eng., A 209,91 (1996).CrossRefGoogle Scholar
26Bradby, J.E., Williams, J.S., Wong-Leung, J., Swain, M.V., and Munroe, P.: Mechanical deformation of crystalline silicon during nanoindentation, in Fundamentals of Nanoindentation and Nanotribology II, edited by Baker, S.P., Cook, R.F., Corcoran, S.G., and Moody, N.R. (Mater. Res. Soc. Symp. Proc. 649, Warrendale, PA, 2001), pp. Q8.10.1–Q8.10.6.Google Scholar
27Saka, H., Shimatani, A., Suganuma, M. and Suprijadi, : Transmission electron microscopy of amorphization and phase transformation beneath indents in Si. Philos. Mag. A 82, 1971 (2002).Google Scholar
28Pharr, G.M., Jang, J.I. and Wen, S.Phase transformation and cracking in brittle materials during nanoindentation, presented at High Pressure Phase Transformations Workshop, University of North Carolina at Charlotte, NC, August 20, 2003Google Scholar
29Leipner, H.S., Lorenz, D., Zeckzer, A. and Grau, P.: Dislocation-related pop-in effect in gallium arsenide. Phys. Status Solidi 183, R4 (2001).Google Scholar
30Zarudi, I., Zhang, L. and Swain, M.: Behavior of moncrystalline silicon under cyclic microindentations with a spherical indenter. Appl. Phys. Lett. 82, 1027 (2003).CrossRefGoogle Scholar
31Galanov, B.A. and Kindrachuk, V.M. Contact mechanics models accounting for phase transformations. In High-Pressure Surface Science and Engineering (Institute of Physics, Bristol, U.K., and Philadelphia, PA, 2004), pp. 21–56Google Scholar
32Gilman, J.J.: Shear-induced metallization. Philos. Mag. B 67, 207 (1993).Google Scholar
33De Wolf, I.: Micro-Raman spectroscopy to study local mechanical stress in silicon integrated circuits. Semicond. Sci. Technol. 11, 139 (1996).CrossRefGoogle Scholar
34Lucazeau, G. and Abello, L.: Micro-raman analysis of residual stresses and phase transformations in crystalline silicon under micro-indentation. J. Mater. Res. 12,2262 (1997).CrossRefGoogle Scholar
35Byakova, A.V., Dub, S.N., Milman, Y.V., Efimov, N.A., and Vlasov, A.A.: Structure and Mechanical Properties of Si-based Coatings (E-MRS 2003 Spring Meeting Abstracts, Strasbourg, France, 2003).Google Scholar