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Indentation fracture of low-dielectric constant films: Part I. Experiments and observations

Published online by Cambridge University Press:  31 January 2011

Dylan J. Morris*
Affiliation:
Materials Science and Engineering Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899-8520
Robert F. Cook
Affiliation:
Materials Science and Engineering Laboratory, National Institute of Standards and Technology, Gaithersburg, Maryland 20899-8520
*
a)Address all correspondence to this author. e-mail: dylan.morris@nist.gov
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Abstract

Advanced microelectronic interconnection structures will need dielectrics of low permittivity to reduce capacitive delays and crosstalk, but this reduction in permittivity typically necessitates an increase in the porosity of the material, which is frequently accompanied by reduced mechanical reliability. Failure by brittle fracture remains a typical manufacturing and reliability hurdle for this class of materials. Part I of this two-part work explores the instrumented indentation and indentation fracture responses of a variety of organosilicate low-dielectric constant (low-κ) films. Three different chemical varieties of low-κ material were tested. The influence of film thickness on the fracture response is also explored systematically. Correlations are made between instrumented indentation responses and differing modes of fracture. It is demonstrated that the elastic response of the composite film + substrate systems can be simply tied to the fraction of the total indentation strain energy in the film. These results are then used in the companion paper, Part II [D.J. Morris and R.F. Cook, J. Mater. Res.23, 2443 (2008)], to derive and use a fracture mechanics model to measure fracture properties of low-κ films.

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Articles
Copyright
Copyright © Materials Research Society 2008

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References

REFERENCES

1International Technology Roadmap for Semiconductors, 2006 Update, Assembly and Packaging., http://www.itrs.net (accessed 2006), p. 2.Google Scholar
2Anstis, G.R., Chantikul, P., Lawn, B.R.Marshall, D.B.: A critical evaluation of indentation techniques for measuring fracture toughness. I. Direct crack measurements. J. Am. Ceram. Soc. 64, 533 1981CrossRefGoogle Scholar
3Lawn, B.R.: Fracture of Brittle Solids Cambridge University Press Cambridge, UK 1993CrossRefGoogle Scholar
4Arora, A., Marshall, D.B., Lawn, B.R.Swain, M.V.: Indentation deformation/fracture of normal and anomalous glasses. J. Non-Cryst. Solids 31, 415 1979CrossRefGoogle Scholar
5Morris, D.J.Cook, R.F.: Indentation fracture of low-dielectric constant films: Part II. Indentation fracture mechanics model. J. Mater. Res. 23, 2443 2008CrossRefGoogle Scholar
6Morris, D.J., Myers, S.B.Cook, R.F.: Sharp probes of varying acuity: Instrumented indentation and fracture behavior. J. Mater. Res. 19, 165 2004CrossRefGoogle Scholar
7Lucas, B.N., Oliver, W.C., Pharr, G.M.Loubet, J.L.: Time dependent deformation during indentation testing in Thin Films: Stresses and Mechanical Properties VI, edited by W.W. Gerberich, H. Gao, J-E. Sundgren, and S.P. Baker (Mater. Res. Soc. Symp. Proc. 436, Pittsburgh, PA, 1997), p. 233CrossRefGoogle Scholar
8Oliver, W.C.Pharr, G.M.: An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7, 1564 1992CrossRefGoogle Scholar
9Lucas, B.N., Oliver, W.C.Swindeman, J.E.: The dynamics of frequency-specific, depth-sensing indentation testing in Fundamentals of Nanoindentation and Nanotribology, edited by N.R. Moody, W.W. Gerberich, N. Burnham, and S.P. Baker (Mater. Res. Soc. Symp. Proc. 522, Warrendale, PA, 1998), p. 3CrossRefGoogle Scholar
10Oliver, W.C.Pharr, G.M.: Measurement of hardness and elastic modulus by instrumented indentation: Advances in understanding and refinements to methodology. J. Mater. Res. 19, 3 2004CrossRefGoogle Scholar
11Ikezawa, K.Maruyama, T.: Sharp tip geometry and its effect on hardness in nanoindentation experiments. J. Appl. Phys. 91, 9689 2002CrossRefGoogle Scholar
12Pharr, G.M., Harding, D.S.Oliver, W.C.: Measurement of fracture toughness in thin films and small volumes using nanoindentation methods in Mechanical Properties and Deformation Behavior of Materials Having Ultra-Fine Microstructures, edited by M. Nastasi, D.M. Parkin, H. Gleiter (NATO ASI, Boston, MA, 1993), p. 449CrossRefGoogle Scholar
13Kese, K.Rowcliffe, D.J.: Nanoindentation method for measuring residual stress in brittle materials. J. Am. Ceram. Soc. 86, 811 2003CrossRefGoogle Scholar
14Morris, D.J.Cook, R.F.: In situ cube-corner indentation of soda-lime glass and fused silica. J. Am. Ceram. Soc. 87, 1494 2004CrossRefGoogle Scholar
15Lathabai, S., Rodel, J., Dabbs, T.Lawn, B.R.: Fracture mechanics model for subthreshold indentation flaws. I. Equilibrium fracture. J. Mater. Sci. 26, 2157 1991CrossRefGoogle Scholar
16Maschio, R. Dal: Application of the Hagan model for crack nucleation to radial cracks in glass. J. Mater. Sci. Lett. 4, 948 1985CrossRefGoogle Scholar
17Lawn, B.R.Evans, A.G.: A model for crack initiation in elastic/plastic indentation fields. J. Mater. Sci. 12, 2195 1977CrossRefGoogle Scholar
18Cook, R.F.Braun, L.M.: Trapped cracks at indentations. II. Fracture mechanics model. J. Mater. Sci. 29, 2192 1994CrossRefGoogle Scholar
19Morris, D.J.Cook, R.F.: Radial fracture during indentation by acute probes: I, Description by an indentation wedging model. Int. J. Fract. 136, 237 2005CrossRefGoogle Scholar
20Kim, S., Toivola, Y., Cook, R.F., Char, K., Chu, S-H., Lee, J-K., Yoon, D.Y.Rhee, H-W.: Organosilicate spin-on glasses. I. Effect of chemical modification on mechanical properties. J. Electrochem. Soc. 151, 37 2004CrossRefGoogle Scholar
21Toivola, Y., Suhan, K., Cook, R.F., Char, K., Lee, J-K., Yoon, D.Y., Rhee, H-W., Kim, S.Y.Jin, M.Y.: Organosilicate spin-on glasses. II. Effect of physical modification on mechanical properties. J. Electrochem. Soc. 151, 45 2004CrossRefGoogle Scholar
22Toivola, Y., Thurn, J.Cook, R.F.: Structural, electrical, and mechanical properties development during curing of low-k hydrogen silsesquioxane films. J. Electrochem. Soc. 149, 9 2002CrossRefGoogle Scholar
23Cook, R.F.Pharr, G.M.: Direct observation and analysis of indentation cracking in glasses and ceramics. J. Am. Ceram. Soc. 73, 787 1990CrossRefGoogle Scholar
24Volinsky, A.A.Gerberich, W.W.: Nanoindentaion techniques for assessing mechanical reliability at the nanoscale. Microelectron. Eng. 69, 519 2003CrossRefGoogle Scholar
25Huang, X.Pelegri, A.A.: Nanoindentation measurements on low-k porous silica thin films spin coated on silicon substrates. J. Eng. Mater.-T. ASME 125, 361 2003CrossRefGoogle Scholar
26Shen, L.Zeng, K.: Comparison of mechanical properties of porous and non-porous low-k dielectric films. Microelectron. Eng. 71, 221 2004CrossRefGoogle Scholar
27Joslin, D.L.Oliver, W.C.: A new method for analyzing data from continuous depth-sensing microindentation tests. J. Mater. Res. 5, 123 1990CrossRefGoogle Scholar
28Yoffe, E.H.: The elastic compliance of a surface film on a substrate. Philos. Mag. Lett. 77, 69 1998CrossRefGoogle Scholar
29Kim, M.T.: Influence of substrates on the elastic reaction of films for the microindentation tests. Thin Solid Films 283, 12 1996CrossRefGoogle Scholar
30Gao, H., Chiu, C-H.Lee, J.: Elastic contact versus indentation modeling of multi-layered materials. Int. J. Solids Struct. 29, 2471 1992Google Scholar
31Song, H., Pharr, G.M.Rar, A.: Assessment of new relation for the elastic compliance of a film-substrate system in Thin Films: Stresses and Mechanical Properties IX, edited by C.S. Ozkan, L.B. Freund, R.C. Cammarata, and H. Gao (Mater. Res. Soc. Symp. Proc. 695, Warrendale, PA, 2002), p. 431CrossRefGoogle Scholar
32Mencik, J., Munz, D., Quandt, E., Weppelmann, E.R.Swain, M.V.: Determination of elastic modulus of thin layers using nanoindentation. J. Mater. Res. 12, 2475 1997CrossRefGoogle Scholar
33Perriot, A.Barthel, E.: Elastic contact to a coated half-space: Effective elastic modulus and real penetration. J. Mater. Res. 19, 600 2004CrossRefGoogle Scholar
34Xu, H.Pharr, G.M.: An improved relation for the effective elastic compliance of a film/substrate system during indentation by a flat cylindrical punch. Scr. Mater. 55, 315 2006CrossRefGoogle Scholar
35Morris, D.J.: Indentation fracture of low-dielectric constant materials.Ph.D. Thesis, University of Minnesota, Minneapolis, MN,2004Google Scholar