Nanoindentation Behaviour and Microstructural Evolution of Annealed Single-Crystal Silicon
The nanoindentation behaviour and phase
transformation of annealed single-crystal silicon wafers are examined.
The silicon specimens are annealed at temperatures of 250, 350 and
450ºC, respectively, for 15 minutes and are then indented to maximum
loads of 30, 50 and 70 mN. The phase changes induced in the indented
specimens are observed using transmission electron microscopy
(TEM) and micro-Raman scattering spectroscopy (RSS). For all
annealing temperatures, an elbow feature is observed in the unloading
curve following indentation to a maximum load of 30 mN. Under
higher loads of 50 mN and 70 mN, respectively, the elbow feature is
replaced by a pop-out event. The elbow feature reveals a complete
amorphous phase transformation within the indented zone, whereas
the pop-out event indicates the formation of Si XII and Si III phases.
The experimental results show that the formation of these crystalline
silicon phases increases with an increasing annealing temperature and
indentation load. The hardness and Young’s modulus both decrease as
the annealing temperature and indentation load are increased.
[1] S. G. Kaplan and L. M. Hanssen, “Silicon as a standard material for
infrared reflectance and transmittance from 2 to 5,” Infrared Phys.
Techno. 43, 389-396 (2002).
[2] W. C. Oliver and G. M. Pharr, “An improved technique for determining
hardness and elastic modulus using load and displacement sensing
indentation experiments,” Mater. Res. 7, 1564-1583 (1992).
[3] D. Beegan, S. Chowdhury and M. T. Laugier, “Work of indentation
methods for determining copper film hardness,” Surf. Coat. Technol. 192,
57-63(2005).
[4] 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, 4679-4684 (1986).
[5] I. Zarudi, L. C. Zhang, W. C. D. Cheong and T. X. Yu, “The difference of
phase distribution in silicon after indentation with Berkovich and
spherical indenters,” Acta Mater. 53, 4795-4800 (2005).
[6] W. C. D. Cheong and Zhang L .C., “Effect of repeated nano-indentations
on the deformation in monocrystalline silicon,” Mater. Sci. Lett. 19,
439-442 (2000).
[7] 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).
[8] J. Jang, M. J. Lance, S. Wen, T. Y. Tsui and G. M. Pharr,
“Indentation-induced phase transformation in silicon: influences of load,
rate and indenter angle on the transformation behaviour,” Acta Mater. 53,
1759-1770 (2005).
[9] Y. Gogots C. Baek, and F. Kirscht, “Raman microspectroscopy study of
processing-induced phase transformations and residual stress in silicon,”
Semicond. Sci. Technol. 14, 936-944 (1999).
[1] S. G. Kaplan and L. M. Hanssen, “Silicon as a standard material for
infrared reflectance and transmittance from 2 to 5,” Infrared Phys.
Techno. 43, 389-396 (2002).
[2] W. C. Oliver and G. M. Pharr, “An improved technique for determining
hardness and elastic modulus using load and displacement sensing
indentation experiments,” Mater. Res. 7, 1564-1583 (1992).
[3] D. Beegan, S. Chowdhury and M. T. Laugier, “Work of indentation
methods for determining copper film hardness,” Surf. Coat. Technol. 192,
57-63(2005).
[4] 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, 4679-4684 (1986).
[5] I. Zarudi, L. C. Zhang, W. C. D. Cheong and T. X. Yu, “The difference of
phase distribution in silicon after indentation with Berkovich and
spherical indenters,” Acta Mater. 53, 4795-4800 (2005).
[6] W. C. D. Cheong and Zhang L .C., “Effect of repeated nano-indentations
on the deformation in monocrystalline silicon,” Mater. Sci. Lett. 19,
439-442 (2000).
[7] 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).
[8] J. Jang, M. J. Lance, S. Wen, T. Y. Tsui and G. M. Pharr,
“Indentation-induced phase transformation in silicon: influences of load,
rate and indenter angle on the transformation behaviour,” Acta Mater. 53,
1759-1770 (2005).
[9] Y. Gogots C. Baek, and F. Kirscht, “Raman microspectroscopy study of
processing-induced phase transformations and residual stress in silicon,”
Semicond. Sci. Technol. 14, 936-944 (1999).
@article{"International Journal of Chemical, Materials and Biomolecular Sciences:70197", author = "Woei-Shyan Lee and Shuo-Ling Chang", title = "Nanoindentation Behaviour and Microstructural Evolution of Annealed Single-Crystal Silicon", abstract = "The nanoindentation behaviour and phase
transformation of annealed single-crystal silicon wafers are examined.
The silicon specimens are annealed at temperatures of 250, 350 and
450ºC, respectively, for 15 minutes and are then indented to maximum
loads of 30, 50 and 70 mN. The phase changes induced in the indented
specimens are observed using transmission electron microscopy
(TEM) and micro-Raman scattering spectroscopy (RSS). For all
annealing temperatures, an elbow feature is observed in the unloading
curve following indentation to a maximum load of 30 mN. Under
higher loads of 50 mN and 70 mN, respectively, the elbow feature is
replaced by a pop-out event. The elbow feature reveals a complete
amorphous phase transformation within the indented zone, whereas
the pop-out event indicates the formation of Si XII and Si III phases.
The experimental results show that the formation of these crystalline
silicon phases increases with an increasing annealing temperature and
indentation load. The hardness and Young’s modulus both decrease as
the annealing temperature and indentation load are increased.", keywords = "Nanoindentation, silicon, phase transformation,
amorphous, annealing.", volume = "9", number = "7", pages = "799-5", }