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Nanoindentation of polydimethylsiloxane elastomers: Effect of crosslinking, work of adhesion, and fluid environment on elastic modulus

Published online by Cambridge University Press:  03 March 2011

Fernando Carrillo ,
Shikha Gupta ,
Mehdi Balooch ,
Sally J. Marshall ,
Grayson W. Marshall ,
Lisa Pruitt  and
Christian M. Puttlitz
Fernando Carrillo
Affiliation:
Department of Orthopaedic Surgery, University of California–San Francisco, San Francisco, California 94110; and Department of Chemical Engineering, EUETIT – Polytechnic University of Catalonia, Terrassa E-08222, Spain
Shikha Gupta
Affiliation:
Medical Polymers Group, Department of Applied Science and Technology, University of California–Berkeley, Berkeley, California 94720
Mehdi Balooch
Affiliation:
Department of Preventive and Restorative Dental Sciences, University of California–San Francisco, San Francisco, California 94143
Sally J. Marshall
Affiliation:
Department of Preventive and Restorative Dental Sciences, University of California–San Francisco, San Francisco, California 94143; andUniversity of California–Berkeley/University of California–San Francisco, Bioengineering Joint Graduate Group, San Francisco, California 94143
Grayson W. Marshall
Affiliation:
Department of Preventive and Restorative Dental Sciences, University of California–San Francisco, San Francisco, California 94143; andUniversity of California–Berkeley/University of California–San Francisco, Bioengineering Joint Graduate Group, San Francisco, California 94143
Lisa Pruitt
Affiliation:
Department of Mechanical Engineering, University of California–Berkeley, Berkeley, California 94720; andUniversity of California—Berkeley/University of California—San Francisco, Bioengineering Joint Graduate Group, San Francisco, California 94143
Christian M. Puttlitz*
Affiliation:
Department of Orthopaedic Surgery, University of California–San Francisco, San Francisco, California 94110 and, University of California—Berkeley/University of California—San Francisco, Bioengineering Joint Graduate Group, San Francisco, California 94143
*
a)Address all correspondence to this author. e-mail: puttlitz@engr.colostate.edu
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Abstract

With the potential to map mechanical properties of heterogeneous materials on a micrometer scale, there is growing interest in nanoindentation as a materials characterization technique. However, nanoindentation has been developed primarily for characterization of hard, elasto-plastic materials, and the technique has not been validated for very soft materials with moduli less than 5 MPa. The current study attempted to use nanoindentation to characterize the elastic moduli of soft, elastomeric polydimethylsiloxane (PDMS) samples (with different degrees of crosslinking) and determine the effects of adhesion on these measurements using adhesion contact mechanics models. Results indicate that nanoindentation was able to differentiate between elastic moduli on the order of hundreds of kilo-Pascals. Moreover, calculations using the classical Hertz contact model for dry and aqueous environment gave higher elastic modulus values when compared to those obtained from unconfined compression testing. These data seem to suggest that consideration of the adhesion energy at the tip-sample interface is a significantly important parameter and needs to be taken into account for consistent elastic modulus determination of soft materials by nanoindentation.

Keywords

Mechanical propertiesNanoindentationPolymer
Type
Articles
Information
Journal of Materials Research , Volume 20 , Issue 10 , October 2005 , pp. 2820 - 2830
Copyright
Copyright © Materials Research Society 2005

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References

REFERENCES

1Fung, Y.C.: Biomechanics: Mechanical Properties of Living Tissues (Springer-Verlag, New York, 1993).CrossRefGoogle Scholar
2Oliver, 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).Google Scholar
3Oliver, W.C. and Pharr, G.M.: Measurement of hardness and elastic modulus by intrumented indentation: advances in understanding and refinements to methodology. J. Mater. Res. 19, 3 (2004).Google Scholar
4Rho, J.Y., Zioupos, P., Currey, J.D. and Pharr, G.M.: Variations in the individual thick lamellar properties within osteons by nanoindentation. Bone 25, 295 (1999).Google Scholar
5Roy, M.E., Rho, J.Y., Tsui, T.Y., Evans, N.D. and Pharr, G.M.: Mechanical and morphological variation of the human lumbar vertebral cortical and trabecular bone. J. Biomed. Mater. Res. 44, 191 (1999).3.0.CO;2-G>CrossRefGoogle ScholarPubMed
6Zysset, P.K., Guo, X.E., Hoffler, C.E., Morre, K.E. and Goldstein, S.A.: Elastic modulus and hardness of cortical and trabecular bone lamellae measured by nanoindentation in the human femur. J. Biomech. 32, 1005 (1999).CrossRefGoogle ScholarPubMed
7Guo, X.E. and Goldstein, S.A.: Vertebral trabecular cone microscopic tissue elastic modulus and hardness do not change in ovariectomized rates. J. Orthop. Res. 18, 333 (2000).CrossRefGoogle Scholar
8Guo, L., Guo, X., Leng, Y., Cheng, J.C. and Zhang, X.: Nanoindentation study of interfaces between calcium phosphate and bone in an animal spinal fusion model. J. Biomed. Mater. Res. 54, 554 (2001).3.0.CO;2-9>CrossRefGoogle Scholar
9Rho, J.Y., Currey, J.D., Zioupos, P. and Pharr, G.M.: The anisotropic Young’s modulus of equine secondary osteones and interstitial bone determined by nanoindentation. J. Exp. Biol. 204, 1775 (2001).Google Scholar
10Swadener, J.G., Rho, J.Y. and Pharr, G.M.: Effects of anisotropy on elastic moduli measured by nanoindentation in human tibial cortical bone. J. Biomed. Mater. Res. 57, 108 (2001).Google Scholar
11Hengsberger, S., Kulik, A. and Zysset, P.: Nanoindentation discriminates the elastic properties of individual human bone lamellae under dry and physiological conditions. Bone 30, 178 (2002).CrossRefGoogle ScholarPubMed
12Marshall, G.W., Habelitz, S., Gallagher, R., Balooch, M., Balooch, G. and Marshall, S.J.: Nanomechanical properties of hydrated carious human dentin. J. Dent. Res. 80, 1768 (2000).CrossRefGoogle Scholar
13Balooch, M., Wumagidi, I.C., Balazs, A., Lundkvist, A.S., Marshall, S.J., Marshall, G.W., Siekhaus, W.J. and Kinney, J.H.: Viscoelastic properties of demineralized human dentin measured in water with atomic force microscope (AFM)-based indentation. J. Biomed. Mater. Res. 40, 539 (1998).3.0.CO;2-G>CrossRefGoogle Scholar
14Ebenstein, D.M., Kuo, A., Rodrigo, J.J., Reddi, A.H., Ries, M. and Pruitt, L.A.: Nanoindentation technique for functional evaluation of cartilage repair tissue. J. Mater. Res. 19, 273 (2004).Google Scholar
15Ebenstein, D.M. and Pruitt, L.A.: Nanoindentation of soft hydrated materials for application to vascular tissues. J. Biomed. Mater. Res. A 69A, 222 (2004).CrossRefGoogle Scholar
16Gupta, S., Carrillo, F., Balooch, M., Pruitt, L. and Puttlitz, C.M.: Simulated soft tissue nanoindentation—A finite element study. J. Mater. Res. 20, 1979 (2005).CrossRefGoogle Scholar
17Maugis, D.: Contact, Adhesion and Rupture of Elastic Solids (Springer, New York, 1999).Google Scholar
18Shull, K.R., Ahn, D., Chen, W.L., Flanigan, C.M. and Crosby, A.J.: Axisymmetric adhesion tests of soft materials. Macromol. Chem. Phys. 199, 489 (1998).Google Scholar
19Clarson, S.J. and Semlyen, J.A.: Siloxane Polymers (Prentice-Hall, Englewood Cliffs, NJ, 1993).Google Scholar
20Livermore, C. and Voldman, J.: Material properties database. http://www.mit.edu/~6.777/matprops/matprops.htm (2005).Google Scholar
21White, C.C., Drzal, P.L. and VanLandingham, M.R. Viscoelastic characterization of polymers using dynamic instrumented indentation, in Fundamentals of Nanoindentation and Nanotribology III, edited by Wahl, K.J., Huber, N., Mann, A.B., Bahr, D.F., and Cheng, Y-T. (Mater. Res. Soc. Symp. Proc. 841, Warrendale, PA, 2005), R5.3 p. 187.Google Scholar
22Lötters, J.C., Olthuis, W., Veltink, P.H. and Bergveld, P.: Polydimethylsiloxane as an elastic material applied in a capacitive accelerometer. J. Micromech. Microeng. 6, 52 (1996).Google Scholar
23Lötters, J.C., Olthuis, W., Veltink, P.H. and Bergveld, P.: The mechanical properties of the rubber elastic polymer polydimethylsiloxane for sensor applications. J. Micromech. Microeng. 7, 145 (1997).Google Scholar
24Sharp, K.G., Blackman, G.S., Glassmaker, N.J., Jagota, A. and Hui, C.Y.: Effect of stamp deformation on the quality of microcontact printing: Theory and experiment. Langmuir 20, 6430 (2004).Google Scholar
25Sedin, D.L. and Rowlen, K.L.: Influence of tip size on AFM roughness measurements. Appl. Surf. Sci. 182, 40 (2001).Google Scholar
26Hertz, H.: On the contact of elastic solids. J. Reine Angew. Math. 92, 156 (1881).Google Scholar
27Johnson, K.L.: Contact Mechanics (Cambridge University Press, Cambridge, U.K., 1987).Google Scholar
28Sneddon, I.N.: The relation between load and penetration in the axisymmetric Boussinesq problem for a punch of arbitrary profile. Int. J. Eng. Sci. 3, 47 (1956).CrossRefGoogle Scholar
29Johnson, K.L., Kendall, K. and Roberts, A.D.: Surface energy and the contact of elastic solids. Proc. R. Soc. London A324, 301 (1971).Google Scholar
30Derjaguin, B.V., Muller, V.M. and Toporov, Y.P.: Effect of contact deformations on the adhesion of particles. J. Colloid Interface Sci. 53, 314 (1975).Google Scholar
31Tabor, D.: Surface forces and surface interactions. J. Colloid Interface Sci. 58, 2 (1977).Google Scholar
32Maguis, D.: Adhesion of spheres: the JKR-DMT transition using a Dugdale model. J. Colloid Interface Sci. 150, 243 (1992).CrossRefGoogle Scholar
33Johnson, K.L. and Greenwood, J.A.: An adhesion map for the contact of elastic spheres. J. Colloid Interface Sci. 192, 326 (1997).Google Scholar
34Carpick, R.W., Ogletree, D.F. and Salmeron, M.: A general equation for fitting contact area and friction vs load measurements. J. Colloid Interface Sci. 211, 395 (1999).Google Scholar
35Sun, Y.J., Akhremitchev, B. and Walker, G.C.: Using the adhesive interaction between atomic force microscopy tips and polymer surfaces to measure the elastic modulus of compliant samples. Langmuir 20, 5837 (2004).Google Scholar
36Galliano, A., Bistac, S. and Schultz, J.: Adhesion and friction of PDMS networks: Molecular weight effects. J. Colloid Interface Sci. 265, 372 (2003).Google Scholar
37Gent, A. N. and Schultz, J.: Effect of wetting liquids on the strength of adhesion of viscoelastic materials. J. Adhes. 281 (1972).CrossRefGoogle Scholar
38Tambe, N.S. and Bhushan, B.: Scale dependence of micro/nano-friction and adhesion of MEMS/NEMS materials, coatings and lubricants. Nanotechnology 15, 1561 (2004).CrossRefGoogle Scholar
39Muller, V.M., Yushenko, V.S. and Derjaguin, B.V.: On the influence of molecular forces on the deformation of an elastic sphere and its sticking to a rigid plane. J. Colloid Interface Sci. 77, 91 (1980).Google Scholar
40VanLandingham, M.R., Drzal, P.L. and White, C.C. Indentation creep and relaxation measurement of polymers, in Fundamentals of Nanoindentation and Nanotribology III, edited by Wahl, K.J., Huber, N., Mann, A.B., Bahr, D.F., and Cheng, Y-T. (Mater. Res. Soc. Symp. Proc.841, Warrendale, PA, 2005), R5.5, p. 193.Google Scholar