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Effects of substrate on determination of hardness of thin films by nanoscratch and nanoindentation techniques

Published online by Cambridge University Press:  03 March 2011

Noureddine Tayebi
Affiliation:
Department of Mechanical and Industrial Engineering, and Department of General Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
Andreas A. Polycarpou*
Affiliation:
Department of Mechanical and Industrial Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
Thomas F. Conry
Affiliation:
Department of General Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
*
a)Address all correspondence to this author. e-mail: polycarp@uiuc.edu
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Abstract

A comparative study on the effects of the substrate on the determination of hardness of thin films by the use of the nanoscratch and nanoindentation techniques was conducted. Gold films deposited on fused quartz substrates and silicon dioxide films deposited on aluminum substrates with variant film thicknesses were investigated. These two systems correspond to a soft film on a hard substrate and a hard film on a soft substrate, respectively. The effect of substrate interaction on the measurement of hardness using the nanoscratch technique was found to be less pronounced compared to that of the nanoindentation technique due to: (i) the lower normal loads applied to achieve the penetration depths that occur at higher loads when using the nanoindentation method; (ii) the direct imaging of the residual deformation profile that is used in the nanoscratch technique, which allows for the effects of pileup or sink-in to be taken into account, whereas in the nanoindentation technique the contact area is estimated from the load-displacement data, which does not include such effects; and (iii) the account of elastic recovery of the plastically deformed surfaces from scratch tests. The film thickness did not appear to have any effect on the hardness of Au and SiO2 films obtained from nanoscratch data. This observation allowed, for the case of SiO2 films, the determination of the “free substrate effect region” and the derivation of an empirical relationship that relates the composite hardness of the film/substrate system to the contact-depth-to-film-thickness ratio, even when the indenter penetrates into the substrate. Such findings can allow for the determination of the intrinsic hardness of ultrathin hard films (∼1–5 nm thick), where the substrate effect is unavoidable.

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Articles
Copyright
Copyright © Materials Research Society 2004

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References

REFERENCES

1Pethica, J.B., Hutchings, R. and Oliver, W.C.: Hardness measurement at penetration depths as small as 20 nm. Phil. Mag. A 48, 593 (1983).CrossRefGoogle Scholar
2Doerner, M.F. and Nix, W.D.: A method for interpreting the data from depth-sensing indentation instruments. J. Mater. Res. 1, 601 (1986).CrossRefGoogle Scholar
3Oliver, W.C. and Pharr, G.M.: An improved technique for determining hardness and elastic modulus using load and displacement sensing indentation experiments. J. Mater. Res. 7, 1564 (1992).CrossRefGoogle Scholar
4Bhattacharya, A.K. and Nix, W.D.: Analysis of elastic and plastic deformation associated with indentation testing of thin films on substrates. Int. J. Solids Structures 24, 1287 (1988).CrossRefGoogle Scholar
5Tsui, T.Y., Oliver, W.C. and Pharr, G.M.: Influences of stress on the measurement of mechanical properties using nanoindentation: Part I. Experimental studies in an aluminum alloy. J. Mater. Res. 11, 752 (1996).CrossRefGoogle Scholar
6Tsui, T.Y. and Pharr, G.M.: Substrate effects on nanoindentation mechanical property measurement of soft films on hard substrates. J. Mater. Res. 14, 292 (1999).CrossRefGoogle Scholar
7Saha, R. and Nix, W.D.: Effects of the substrate on the determination of thin film mechanical properties by nanoindentation. Acta Mater. 50, 23 (2002).CrossRefGoogle Scholar
8Chen, X. and Vlassak, J.J.: Numerical study on the measurement of thin film mechanical properties by means of nanoindentation. J. Mater. Res. 16, 2974 (2001).CrossRefGoogle Scholar
9Sawa, T., Akiyama, Y., Shimamoto, A. and Tanaka, K.: Nanoindentation of a 10 nm thick thin film. J. Mater. Res. 14, 2228 (1999).CrossRefGoogle Scholar
10Pharr, G.M. and Bolshakov, A.: Understanding nanoindentation unloading curves. J. Mater. Res. 17, 2660 (2002).CrossRefGoogle Scholar
11Tsui, T.Y., Ross, C.A. and Pharr, G.M.: A method for making substrate-independent hardness measurements of soft metallic films on hard substrates by nanoindentation. J. Mater. Res. 18, 1383 (2003).CrossRefGoogle Scholar
12Randall, N.X.: Direct measurement of residual contact area and volume during the nanoindentation of coated materials as an alternative method of calculating hardness. Phil. Mag. A 82, 1883 (2002).CrossRefGoogle Scholar
13McGurk, M.R. and Page, T.F.: Using the P -δ2 analysis to deconvolute the nanoindentation response of hard-coated systems. J. Mater. Res. 14, 2283 (1999).CrossRefGoogle Scholar
14Kral, E.R., Komvopoulos, K. and Bogy, D.B.: Hardness of thin-film media: Scratch experiments and finite element simulations. ASME J. Tribology 118, 1 (1996).CrossRefGoogle Scholar
15Tayebi, N., Conry, T.F. and Polycarpou, A.A.: Determination of hardness from nanoscratch experiments: Corrections for interfacial shear stress and elastic recovery. J. Mater. Res. 18, 2150 (2003).CrossRefGoogle Scholar
16Mohs, F.: Grundriss der Mineralogie, (1824), English Translation by W. Haidinger, Treatise of Mineralogy, (Constable, Edinburgh, 1825).Google Scholar
17Li, X. and Bhushan, B.: Micro/nanomechanical and tribological characterization of ultrathin amorphous carbon coatings. J. Mater. Res. 14, 2328 (1999).CrossRefGoogle Scholar
18Consiglio, R., Randall, N.X., Bellaton, B. and von Stebut, J.: The nano-scratch tester (NST) as a new tool for assessing the strength of ultrathin hard coatings and the mar resistance of polymer films. Thin Solid Films 332, 151 (1998).CrossRefGoogle Scholar
19 B. Bhushan, Handbook of Micro/Nanotribology , 2nd ed. (CRC, Boca Raton, FL, 1999).Google Scholar
20Goddard, J. and Wilman, H.: A theory of friction and wear during the abrasion of metals. Wear 5, 114 (1962).CrossRefGoogle Scholar
21Tsukizoe, T. and Sakamoto, T.: Friction in scratching without metal transfer. Bull. JSME 18, 65 (1975).CrossRefGoogle Scholar
22Komvopoulos, K., Saka, N. and Suh, N.P.: The mechanism of friction in boundary lubrication. ASME J. Tribology 107, 452 (1985).CrossRefGoogle Scholar
23Love, A.E.H.: Stress produced in a semi-infinite solid by pressure on part of the boundary. Phil. Trans. Royal Soc. A228, 377 (1929).Google Scholar
24Sneddon, I.N.: Relation between load and penetration in axisymmetric Boussinesq problem for punch of arbitrary profile. Int. J. Eng. Sci. 3, 47 (1965).CrossRefGoogle Scholar
25Pharr, G.M., Oliver, W.C. and Brotzen, F.R.: On the generality of the relationship among contact stiffness, contact area, and elastic modulus during indentation. J. Mater. Res. 7, 613 (1992).CrossRefGoogle Scholar
26Cheng, C-M. and Cheng, Y-T.: On the initial unloading slope in indentation of elastic-plastic solids by an indenter with an axisymmetric smooth profile. Appl. Phys. Lett. 71, 2623 (1997).CrossRefGoogle Scholar
27Boussinesq, J.: Application des potentials a l’etude de l’equilibre du movement des solides elastiques (Gauthier-Villars, Paris, 1885 , in French).Google Scholar
28Johnson, K.L., Contact Mechanics (Cambridge University Press, Cambridge, U.K., 1985).CrossRefGoogle Scholar
29Yu, N., Polycarpou, A.A. and Conry, T.F.: Tip-radius effect in finite element modeling of sub-50 nm shallow indentation. Thin Solid Films 450, 295 (2004).CrossRefGoogle Scholar
30 Hysitron, Inc., Nanoindentation User Manual , Minneapolis, MNGoogle Scholar
31Kuhn, L., Corcoran, S., and Wyrobek, T.: Data storage, 55, Penn Well, Tulsa, OK (July 1998).Google Scholar
32 Hysitron, Inc., Nanoscratch User Manual , Minneapolis, MN, (2001)Google Scholar
33Bucaille, J., Felder, E. and Hochstetter, G.: Mechanical analysis of the scratch test on elastic and perfectly plastic materials with the three-dimensional finite element modeling. Wear 249, 422 (2001).CrossRefGoogle Scholar
34Callister, W.D. Jr., Materials science and engineering—An introduction , 3rd ed. (John Wiley and Sons, New York, 1994).Google Scholar