Comptes Rendus
Surface mechanics: facts and numerical models
Characterization of the adhesion of thin film by Cross-Sectional Nanoindentation Analysis of the substrate edge chipping and the film delamination
Comptes Rendus. Mécanique, Volume 339 (2011) no. 7-8, pp. 443-457.

Cross-Sectional Nanoindentation (CSN) is a recent method for adhesion measurement of nanoscale thin films in Ultra-Large Scale Integrated circuits. In the case of ductile thin films, the motion of the substrate chip implies significant plastic deformation of the film and complex geometry of delaminated areas. This article recalls first the experimental procedure and the two main features observed in this test performed on various plane copper films deposited on silicon: the critical force producing silicon edge chipping increases linearly with the distance of the indenter to the interface; on the section the delaminated length of the film (ab) is proportional to the residual silicon chip displacement uf and the ratio S=uf/(ab) depends on the manufacturing process of the film, and is so related to its adhesion to the substrate. One proposes a simple analysis of the silicon edge chipping. Then a model of pull-off of an elastic-strain hardening plastic film is developed, which suggests an explanation for the delamination process. Application of the model to experimental results starting from films plastic properties deduced from nanoindentation measurements provides plausible results. Some improvements for performing the CSN test are proposed in order to make easier its interpretation.

Published online:
DOI: 10.1016/j.crme.2011.05.003
Keywords: Adhesion, Nanoindentation, Thin films, Microelectronic, Copper, Mechanical analysis

Eric Felder 1; Sébastien Roy 1; Evelyne Darque-Ceretti 1

1 CEMEF, UMR CNRS/MINES ParisTech 7635, BP 207, 06904 Sophia-Antipolis, France
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Eric Felder; Sébastien Roy; Evelyne Darque-Ceretti. Characterization of the adhesion of thin film by Cross-Sectional Nanoindentation Analysis of the substrate edge chipping and the film delamination. Comptes Rendus. Mécanique, Volume 339 (2011) no. 7-8, pp. 443-457. doi : 10.1016/j.crme.2011.05.003. https://comptes-rendus.academie-sciences.fr/mecanique/articles/10.1016/j.crme.2011.05.003/

[1] E. Darque-Ceretti; E. Felder Adhésion et adhérence. Sciences et techniques de lʼingénieur, CNRS Editions, Paris, 2003 (pp. 246–251)

[2] A.A. Volinsky; N.R. Moody; W.W. Gerberich Interfacial toughness measurements for thin films on substrates, Acta Mater., Volume 50 (2002), pp. 441-466

[3] G.J. Klingenmaier; M. Dobrash Adhesion Measurement of Thin Films, Thick Films and Bulk Coatings (K.L. Mittal, ed.), ASTM STP, vol. 640, ASTM, Philadelphia, 1978, pp. 369-390

[4] A. Bagchi; G.E. Lucas; Z. Suo; A.G. Evans A new procedure for measuring the decohesion energy for thin ductile films on substrate, J. Mater. Res., Volume 9 (1994) no. 7, pp. 1734-1741

[5] A. Bosseboeuf; M. Dupeux; M. Doutry; T. Bourouina; D. Bouchier; D. Debarre Characterization of W films on Si and SiO2/Si substrates by X-ray diffraction, AFM and blister test adhesion measurements, Microsc. Microanal. Microstruct., Volume 8 (1997), pp. 261-272

[6] R.H. Dauskardt; M. Lane; Q. Ma; N. Krishna Adhesion and debonding of multi-layer thin film structures, Eng. Fract. Mech., Volume 61 (1998), pp. 141-162

[7] Z. Gan; S.G. Mhaisalkar; Z. Chen; S. Zhang; Z. Chen; K. Prasad Study of interfacial adhesion energy of multilayered ULSI thin film structures using four-point bending test, Surf. Coat. Technol., Volume 198 (2005), pp. 85-89

[8] C.S. Litteken; R.H. Dauskardt Adhesion of polymer thin-films and patterned lines, Int. J. Fract., Volume 119/120 (2003), pp. 475-485

[9] S.S. Chiang; D.B. Marshall; A.G. Evans A simple method for adhesion measurements (J.A. Pask; A.G. Evans, eds.), Surfaces and Interfaces in Ceramics and Ceramics–Metal Systems, Plenum, New York, 1981, pp. 603-617

[10] P.R. Jindal; D.T. Quinto; G.J. Wolfe Adhesion measurements of chemically vapor deposited and physically vapor deposited hard coatings on WC–Co substrates, Thin Solid Films, Volume 154 (1987), pp. 361-375

[11] P.K. Mehrotra; D.T. Quinto Techniques for evaluating mechanical properties of hard coatings, J. Vac. Sci. Technol. A, Volume 3 (1985) no. 6, pp. 2401-2405

[12] M.D. Drory; J.W. Hutchinson Measurement of the adhesion of a brittle film on a ductile substrate by indentation, Proc. R. Soc. Lond. A, Volume 452 (1996), pp. 2319-2341

[13] A.A. Volinsky; N.I. Tymiak; M.D. Kriese; W.W. Gerberich; J.W. Hutchinson Quantitative modeling and measurement of copper thin film adhesion, Mat. Res. Soc. Symp. Proc., Volume 539 (1999), pp. 277-290

[14] A.A. Volinsky; J.B. Vella; W.W. Gerberich Fracture toughness, adhesion and mechanical properties of low-K dielectric thin films measured by nanoindentation, Thin Solid Films, Volume 429 (2003), pp. 201-210

[15] J.B. Vella; S.M. Smith; A.A. Volinsky; I.S. Adhihetty Adhesion quantification of post-CMP copper to amorphous SiN passivation by nanoindentation, Mat. Res. Soc. Symp. Proc., Volume 649 (2001)

[16] P. Laeng, P.A. Steinmann, Adhesion testing of hard C.V.D. coatings using the scratch test, in: Proc. of the 8th Int. Conf. C.V.D., Electrochem. Soc., Pennington, 1981, pp. 723–735.

[17] E. Felder; C. Angélélis; M. Ducarroir; M. Ignat; P. Mazot Propriétés mécaniques des films minces : Problématiques et moyens de mesure, Ann. Chim. Sci. Mat., Volume 23 (1998), pp. 791-819

[18] S. Roy, Mesure de lʼadhérence et des propriétés mécaniques de couches minces sub-microniques. Application aux procédés de dépôt Alchimer pour la microélectronique et au biomédical, Ph.D. Dissertation, Ecole des Mines de Paris, 2008.

[19] J. Lesage; P.H. Demarecaux; O. Bartier; G. Mesmacque Détermination de lʼadhérence de revêtements par le test dʼindentation interfaciale, Rev. de Métall. – CIT, Volume 90 (1993) no. 12, pp. 1655-1663

[20] J.M. Sanchez; S. El-Mansy; B. Sun; T. Scherban; N. Fang; D. Pantuso; W. Ford; M.R. Elizalde; J.M. Martinez-Esnaola; A. Martin-Meizoso; J. Gil-Sevillano; M. Fuentes; J. Maiz Cross-sectional nanoindentation: a new technique for thin film interfacial adhesion characterization, Acta Mater., Volume 47 (1999) no. 17, pp. 4405-4413

[21] M.R. Elizalde; J.M. Sanchez; J.M. Martinez-Esnaola; D. Pantuso; T. Scherban; B. Sun; G. Xu Interfacial fracture induced by cross-sectional nanoindentation in metal–ceramic thin film structures, Acta Mater., Volume 51 (2003), pp. 4295-4305

[22] T. Scherban; D. Pantuso; B. Sun; S. El-Mansy; J. Xu; M.R. Elizalde; J.M. Sanchez; J.M. Martinez-Esnaola Characterization of interconnect interfacial adhesion by cross-sectional nanoindentation, Int. J. Fract., Volume 119/120 (2003), pp. 421-429

[23] J.M. Molina-Aldareguia; I. Ocaña; D. González; M.R. Elizalde; J.M. Sánchez; J.M. Martínez-Esnaola; J. Gil-Sevillano; T. Scherban; D. Pantuso; B. Sun; G. Xu; B. Miner; J. He; J. Maiz Adhesion studies in integrated circuit interconnect structures, Eng. Fail. Anal., Volume 14 (2006) no. 2, pp. 349-354

[24] I. Ocana; J.M. Molina-Aldareguia; D. Gonzalez; M.R. Elizalde; J.M. Sanchez; J.M. Martinez-Esnaola; J. Gil Sevillano; T. Scherban; D. Pantuso; B. Sun; G. Xu; B. Miner; J. He; J. Maiz Fracture characterization in patterned thin films by cross-sectional nanoindentation, Acta Mater., Volume 54 (2006), pp. 3453-3462

[25] S. Roy; E. Darque-Ceretti; E. Felder; H. Monchoix Cross-sectional nanoindentation for copper adhesion characterization in blanket and patterned interconnect structures: experiments and three-dimensional FEM modeling, Int. J. Fract., Volume 144 (2007), pp. 21-33

[26] H. Chai; B.R. Lawn A universal relation for edge chipping from sharp contacts in brittle materials: A simple means of toughness evaluation, Acta Mater., Volume 55 (2007), pp. 2555-2561

[27] J. Lankford; D.L. Davidson The crack-initiation threshold in ceramic materials subject to elastic/plastic indentation, J. Mater. Sci., Volume 14 (1979), pp. 1662-1668

[28] J.-I. Jang; G.M. Pharr Influence of indenter angle on cracking in Si and Ge during nanoindentation, Acta Mater., Volume 56 (2008), pp. 4458-4469

[29] B.R. Lawn; A.G. Evans A model for crack initiation in elastic/plastic indentation fields, J. Mater. Sci., Volume 12 (1977), pp. 2195-2199

[30] D.B. Marshall; B.R. Lawn Indentation of brittle materials (P.J. Blau; B.R. Lawn, eds.), Microindentation Techniques in Materials Sciences and Engineering, ASTM STP, vol. 889, ASTM, Philadelphia, 1986

[31] B.R. Lawn; A.G. Marshall Hardness, toughness and brittleness: an indentation analysis, J. Am. Ceram. Soc., Volume 62 (1977), pp. 347-350

[32] A.N. Gent New and improved tests for adhesion, J. Adhesion, Volume 23 (1987), pp. 115-122

[33] P. Baqué; E. Felder; J. Hyafil; Y. DʼEscatha Mise en forme des métaux. Calculs en plasticité, Dunod, Paris, 1974

[34] W.C. Oliver; G.M. Pharr An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments, J. Mater. Res., Volume 7 (1992) no. 6, pp. 1564-1583

[35] D. Tabor The Hardness of Metals, Clarendon Press, Oxford, 1951

[36] D. Lebouvier, P. Gilormini, E. Felder, Theoretical and experimental study of the flow pressure and deformation of hard and soft coatings during plastic indentation, in: Proceedings of the 5th International Congress on Tribology, Eurotrib ʼ89, Helsinki, vol. 2, 1989, pp. 116–121.

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