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Contents lists available at ScienceDirect

Mechanics of Materials

journal homepage: www.elsevier.com/locate/mechmat

**A hybrid model to determine mechanical properties of soft polymers by nanoindentation
**

Qinzhuo Liao 1, Jianyong Huang 1, Tao Zhu, Chunyang Xiong ⇑, Jing Fang

Department of Biomedical Engineering, Peking University, Beijing 100871, China Academy for Advanced Interdisciplinary Studies, Peking University, Beijing 100871, China

a r t i c l e

i n f o

a b s t r a c t

In nanoindentation tests for soft polymers, the elastic modulus estimated from the Hertz model varies with applied force, implying the effect of adhesion work needs to be considered in contact theory. In this article, a hybrid method of combining the Hertz model and the Johnson–Kendall–Roberts (JKR) model is presented, to analytically explain the descending phenomenon of the modulus estimation by considering adhesive effects. Thus both the force-independent elastic modulus and the adhesion work can be evaluated by ﬁtting the experimental data, without need to know the adhesive force in advance. The successful application to the measurement of polydimethylsiloxane (PDMS) material’s elastic modulus demonstrates the method is applicable to the mechanical characterization of soft polymers by nanoindentation. Ó 2010 Elsevier Ltd. All rights reserved.

Article history: Received 6 January 2010 Received in revised form 17 September 2010

Keywords: Nanoindentation Polymer Elasticity Adhesion

1. Introduction Soft polymeric materials are ﬁnding greater use in microdevices and biomedical engineering applications (McDonald and Whitesides, 2002). For instance, polydimethylsiloxane (PDMS) is one of the most widely used materials in microﬂuidics (Whitesides, 2006), and polyacrylamide can be used as a soft substrate (Pelham and Wang, 1997; Qin et al., 2007; Huang et al., 2009a,b). With size reduction to micro- and nano-scales, suitable methods to characterize local mechanical properties of soft materials have become more important. Nanoindentation, also known as instrumented or depth-sensing indentation, is increasingly being used to measure mechanical parameters at small scales (Van Landingham, 2003; Schuh, 2006). Even though the technique has been successfully applied to estimate elastic and elastic–plastic properties of hard materials, it still requires further validation and suitable correction for soft materials

⇑ Corresponding author at: Department of Biomedical Engineering, Peking University, Beijing 100871, China. Tel.: +86 10 62757940; fax: +86 10 62752513. E-mail address: cyxiong@pku.edu.cn (C. Xiong). 1 These authors contributed equally to this work.

0167-6636/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved. doi:10.1016/j.mechmat.2010.09.005

to obtain accurate and reproducible results (Zhao et al., 2003; Carrillo et al., 2005; Ebenstein and Pruitt, 2006; Gupta et al., 2007). In nanomechanics tests of hard materials, for instance, adhesion plays a negligible role in the sample and surface force can be neglected. Therefore, the classical Hertz model (Hertz, 1881) can be used to evaluate Young’s modulus of the elastic material. For soft materials such as polydimethylsiloxane (PDMS), many preliminary results have indicated that the adhesion energy at the tip-sample interface is a signiﬁcant factor for a consistent modulus determination by nanoindentation (Johnson et al., 1971; Lim and Chaudhri, 2003; Cao et al., 2005; Carrillo et al., 2005; Ebenstein and Wahl, 2006; Gupta et al., 2007). For the Hertz model without adhesive effect considerations, the contact area and effective force experienced by the substrate might be underestimated, so that the sample modulus of soft matter would be overestimated (Johnson et al., 1971; Lim and Chaudhri, 2003). Some results also present obvious negative forces on the force–displacement curve, which is a direct evidence of adhesion behavior (Cao et al., 2005; Carrillo et al., 2005; Ebenstein and Wahl, 2006). Another big problem is that the elastic moduli evaluated by the Hertz model show signiﬁcantly variation with the maximum indentation depth (or the peak indenter load) (Lim and

... (5). expressed as a2 1 þ h¼ 0 R pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!4 3 1 À P=Padh 2 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!1 3 1 À P=Padh a2 þ h0 À 0 2 3 ð4Þ 2a2 1 þ À 0 3R where h0 is the apparent displacement when the indentation force is zero (P = 0). 1881). Ebenstein and Wahl. These large variations are in disagreement with the actual properties of PDMS as a linearly elastic polymer. while the adhesive forces need not be known in advance.. 2. the reduced modulus EHertz of the sample material can be expressed as r EHertz r sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ S3 ¼ 6RP max ð1Þ where R is the nominal radius of the indenter tip curvature.. Carrillo et al. Nanoindentation tests were carried out using a Hysitron TriboIndenter (Hysitron Inc. on the other hand. given by S¼ dP dh h¼hmax ð2Þ As the sample is much softer than the indenter. and then combining Eq. needs to input a suitable adhesive force in advance. Minneapolis. the difference in elastic moduli resulting from different peak loads can be reconciled (Gupta et al. and the objective of data processing from the Hertz analysis is to obtain the modulus–force relation from multiple load– displacement curves. This correction. with a displacement-controlled closed loop feedback mode. on the other hand. 1999))... is measured from the force–displacement curve of nanoindentation in the maximum depth. 2005. After cooling. the samples were cut from the bulk elastomer with dimensions 2 Â 2 Â 1 cm3. The effect of interfacial adhesion between probe tip and sample surface of the soft matter. 3. the indentation depth h is evaluated by taking account of both the applied force P and the adhesive force Padh (Cao et al. The contact stiffness S (i. The tip was then indented to the maximum displacement with a constant rate. MN). however. / Mechanics of Materials 42 (2010) 1043–1047 Chaudhri. which is commonly difﬁcult to be accurately measured and different authors provide various values for soft materials (Cao et al. All indents were produced by a sapphire spherical probe with a nominal radius of 400 lm. Experimental procedure The PDMS samples were prepared by mixing the elastomer base with the curing agent (Sylgard 184. The mixed solutions were poured into plastic containers to cure for 2 h at 85 °C. (normally set h0 = 0 in the tests) and a0 is the radius of the contact area at zero load. Basically. the slope of the initial portion of the unloading curve). the relation of the Young’s modulus EHertz and the reduced modulus is EHertz ﬃ EHertz ð1 À m2 Þ r ð3Þ where m is the Poisson’s ratio of the sample (m % 0. 2005. 2006). Theory According to the Hertz model (Hertz. three locations were chosen on the sample surface and each location had eight indents applied.e. is taken into account by introducing the JKR model to this approach. Gupta et al. related to the adhesive force Padh by a3 ¼ À 0 3RP adh EJKR r ð5Þ From the adhesive force Padh. 2007). by considering the Young’s modulus and the adhesion work as two inherent properties of the soft material and evaluating them as two constant parameters to ﬁt the experimental data. 2005).1044 Q. (4)] into that in the Hertz model [Eq. The Hertz theory is a classical method used in most nanoindentation tests of elastic materials. which was suitable for soft materials with small indentation depths. For every specimen.. the phenomenon of depth-dependence of Young’s modulus in the Hertz analysis can be described by the hybrid method and both the elastic modulus and the adhesion work can be obtained from the modulus–load curves. a hybrid method of combining the Hertz model and the JKR model is presented to simultaneously determine both the Young’s modulus and adhesion work by nanoindentation. Indentations with eight different maximum indentation depths were implemented ranging from about 500 to 4000 nm and the rate of loading and unloading was kept at 100 nm/s. Speciﬁcally. and then drawn to unload with the same rate as loading.5 for PDMS (Mark. Prior to indentation a small preload was applied for surface detection. Liao et al. (2)]. 1971). and Pmax is the maximum applied force corresponding to the maximum indentation depth hmax. 2003. Dow Corning. In this way. By the JKR model. the Hertz analysis does not consider the behavior of adhesive force that exists in most interfaces between the soft material and the indenter. held there for 5 s. the contact ﬂexibility is derived as . By considering adhesive interactions within the Johnson–Kendall–Roberts (JKR) adhesion contact model (Johnson et al. the adhesion work Dc (the interfacial energy per unit area) can be expressed as Dc ¼ À 2 Padh 3 pR ð6Þ Substituting the depth h expressed by the JKR model [Eq. MI) in two different ratios (10:1 and 20:1) respectively. In this study. 2007). Midland.

.

Pmax Þ ¼ 1 ¼ dh. a2 1 1 ~ JKR . Padh .

pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ ¼ 0 SðE .

S dP P¼Pmax R Padh 1 À P max =Padh 2 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!À2 3 1 1 þ 1 À Pmax =Padh Â4 2 18 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!1 3 3 1 1 þ 1 À Pmax =Padh 5 À 2 3 sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ 2 3 1 3 1 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ ¼ RP adh EJKR 1 À Pmax =Padh .

varies with the maximum applied force corresponding to the maximum indentation depth which ranged from 500 to 4000 nm. showing negative forces near zerodisplacement indicating the existence of adhesive forces. by substituting Eq.Q. The adhesion work Dc. (1) and (3). 1 and 2 plot data from eight indents of one location on each sample and that the results from the other two indent locations are similar and not shown. where the various amounts of adhesive work produce different estimations of the elastic modulus as the indents are shallow. Using the hybrid model to evaluate the modulus–force relation with Eq. as given in Fig. Fig. 1 shows the force–displacement curves of two PDMS specimens with different base-agent ratios. Results and discussion Fig. (8). representing the inﬂuence of adhesive force Padh on the indentation contact. (7) into Eqs. 3a. (8) of the hybrid model. The Young’s moduli estimated from the Hertz model. as dominated by (a) the adhesion work Dc. . Pmax Þ3 SðE ð8Þ 4. as shown in Fig. Illustration of theoretical EHertz À Pmax relation evaluated by Eq. 2. Fig. 3. determines the descending rate of the modulus with the applied force. showing variation with the maximum applied indentation force. Padh . The modulus EHertz evaluated by the Hertz method. 1. 3b where the adhesive work is kept at a certain level. where the slopes of the initial unloading curve are used to obtain the elastic moduli. Liao et al. 3 presents the theoretical descriptions for the decreasing variation of the modulus EHertz with the maximum applied force Pmax. Negative forces can be observed in both the initial loading and the unloading near the zero-displacement position. Fig. These force-dependent results of EHertz values are in accordance with those reported by Gupta et al. 2. It should be pointed out that Figs. as shown in Fig. EJKR. especially when the indentation depth is shallow or the applied force is small. 20:1). / Mechanics of Materials 42 (2010) 1043–1047 1045 1 1þ Â4 18 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!À2 3 1 À Pmax =P adh 2 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ!1 3 3 1 1 þ 1 À Pmax =Padh 5 À 2 3 2 ð7Þ Therefore. This effect is more obvious when the maximum applied force is relatively small in these Dc-dominated curves. showing that the adhesion is an important factor which interferes with the estimation of sample modulus. Force–displacement curves of two PDMS samples with different base-agent ratios (10:1. mainly determines the modulus levels of EHertz evaluation. indicating the existence of adhesive force between the indenter and the sample in their contact zone. and (b) the modulus EJKR. with maximum displacement of 500 nm in nanoindentation. Padh . (2007). Pmax Þ sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ 1 ¼ ð1 À m2 Þ 6RP max Â ~ JKR . Fig. The other independent parameter. an analytical expression of combining the two models is obtained to relate the two types of elastic modulus given by EHertz ¼ f ðEJKR .

4 shows two analytical curves that ﬁt well with our experimental data of EHertz À Pmax relations. The difference of results is due to several reasons: the curing/cooling time and temperature of materials. showing that the force-dependent phenomenon of the Hertzian modulus keeps its appearance in the results (Fig.. Through statistical analysis of indentation results of PDMS tests.0005). the measured E was found to increase with the increasing loading/unloading rate. / Mechanics of Materials 42 (2010) 1043–1047 This means these two parameters dominate a family of theoretical curves which cover the relation of EHertz À Pmax as estimated by the Hertz model. similar to the conclusion drawn by Lim and Chaudhri (2003).05. In addition. is within the range of the typical values (100–500 mJ/m2) reported by Bietsch and Michel (2000). tests with different preloads (from 0. Also for this case of base-agent ratio. 2005) and 1. Results of the Young’s modulus and adhesion work for the 10:1 PDMS with different loading/unloading rates.. Lim and Chaudhri. Furthermore.0875) is slightly larger than 0.9 ± 0. the solution of the elastic modulus EJKR for the soft materials becomes a process of ﬁnding an appropriate curve from Eq. For these two sorts of PDMS samples with different cross-linker. the estimated modulus EJKR = 1. changes less than 6% and the adhesion work Dc varies less than 2%. the sample-tip system. the p-value of Dc (p = 0. et al. The loading/unloading rates used in our experiment were smaller than the rate of 250 nm/s that was used by Gillies and Fig. Statistical results of the Young’s modulus and adhesion work for the PDMS with different base-agent ratios. for different base-agent ratios of the polymer. The elastic modulus EJKR. However. The two estimated values of EJKR. 4. 2007). in which the adhesion work Dc can also be evaluated without special measurement of adhesive force. before further investigation is carried out. Besides. 1971.5 MPa (Gupta et al. Fig. But it is still too early to say there is no signiﬁcant difference between Dc. implying that the surface adhesive energy of PDMS material may be more consistent with the property Fig. Taking the 10:1 ratio as an example. The analytical curves determined by the appropriate parameters Dc and EJKR to ﬁt the experimental data of EHertz À Pmax. 5. to represent the intrinsic mechanical behaviors of the PDMS material. 2003).1046 Q. (8). 6).. which proves that the Hertz analysis without adhesion consideration normally overestimates the sample modulus (Johnson et al. which suggests that the results are basically independent of the preload forces.3 MPa (Cao et al. indicating that the effect of surface adhesion becomes less in the cases of larger forces or deeper indents. where the curve parameters EJKR and Dc are attached as the force-independent elastic modulus and the adhesion work. of the base component. 5 gives the mean values of the Young’s modulus EJKR with small standard deviations.02 MPa is between the values of 1. Fig. however. show that EHertz tends to converge to EJKR as the maximum applied force becomes larger. Liao et al. Fig. 6. EHertz will usually always be higher than EJKR for any indentation depths. with two constant parameters to ﬁt the data of EHertz À Pmax from the nanoindentation test. . different loading/unloading rates from 50 to 200 nm/s have been implemented in our tests. signiﬁcant difference is observed in EJKR (p = 0. Therefore. which shows that the viscoelastic property has not much inﬂuence on the results. the adhesion work Dc = 209 ± 9. as illustrated by the dashed lines of constants.74 ± 0.1 mJ/m2 obtained from our PDMS-sapphire tip system.1 to 2 lN) in nanoindentation show that the measured moduli vary less than 1%. In spite of this.

Carrillo et al. 491–499. Chaudhri. 90607004.. 156–171. Review of instrumented indentation. 2000. D. Polymer Data Handbook... Carrillo. Determination of cellular tractions on elastic substrate based on an integral Boussinesq solution.. Shi. 2005). can be evaluated as two constant parameters by ﬁtting the experimental data... Fang. 13661–13665. Peng. 2006. K. C.H. S.W..M. Y. 2009b. Puttlitz.. 1971.. Conformal contact and pattern stability of stamps used for soft lithography. Hertz. 10872008.C.L.F. The research is supported by the National Basic Research Program of China through Grant Nos... Cao. L. Zhu.. 5. Zhao. 2005.. Cellular traction force recovery: an optimal ﬁltering approach in two-dimensional Fourier space. 2009a.M. A comparison of JKR-based methods to analyze quasi-static and dynamic indentation force curves. Qiang for technical assistance in nanoindentation tests. Nano Today 1 (3). C. Qin. 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