11th National Congress on Theoretical and Applied Mechanics, 2-5 Sept.

2009, Borovets, Bulgaria

DETERMINATION OF MECHANICAL PROPERTIES OF ELECTROCHEMICALLY DEPOSITED THIN GOLD FILMS *

S. CHERNEVA
Institute of Mechanics, Bulgarian Academy of Sciences, BG-1113 Sofia, Bulgaria, Acad. G. Bonchev str., bl. 4 e-mail: sabina_cherneva@yahoo.com

R. IANKOV
Institute of Mechanics, Bulgarian Academy of Sciences, BG-1113 Sofia, Bulgaria, Acad. G. Bonchev str., bl. 4 e-mail: iankovr@yahoo.com

D. STOYCHEV
Institute of Physical Chemistry, Bulgarian Academy of Sciences, BG-1113 Sofia, Bulgaria, Acad. G. Bonchev str., bl. 11 e-mail: stoychev@ipchp.ipc.bas.bg ABSTRACT. In the present work the mechanical properties of thin gold film with known thickness were investigated. The film was deposited electrochemically over brass substratum with known thickness and mechanical properties. It was realized micro indentation experiment of the film and as a result of this the experimental load-displacement curve was obtained. After that the process of micro indentation was modeled numerically by means of finite element method and numerical loaddisplacement curve was obtained. Subsequently experimental and numerical loaddisplacement curves were compared. Results, which were obtained through numerical simulation, give good coincidence with the experimental results. Therefore the proposed method can be successfully applied for identification of material parameters of the accepted model. KEY WORDS: thin films, mechanical properties, microindentation, finite-element analysis

1. Introduction The processes of electrochemically deposition of thin films practically are used in all technical branches-from metallurgy and heavy machine-building to microelectronics and nanotechnology. Nowadays most intensive developed areas of application of the electrochemically deposited thin films are connected with electronics, computer technologies and instrument-building [1]. Electrochemically deposited gold films are fairly widespread, by reason of fact, that this is valuable
*

Authors gratefully acknowledge financial support from the EU Project INTERCONY, Contr. No. NMP4-CT-2006-033200, the Bulgarian National Science Fund under grants No. TK01/0185 and No. BG051PO001/07/3.3-02.

S. Cherneva, R. Iankov, D. Stoychev metal and besides because of its important technical characteristics. Advantages of thin gold films are very high electrical conductivity, very high plasticity, very high stability of corrosion and attractive outward appearance. In this connection gold films are used mainly for secure of high stability of corrosion of surfaces in different environments, for decorative purposes and in jewellery. Thickness of the gold films depending on outline purpose is from 0.15 m to 15m. In the present work we propose new method for determination mechanical properties of thin metal films. This method combine microindentation experiment and numerical simulations by means of finite element method. In most cases mechanical properties of thin films are determined by means of tensile tests or by means of nanoindentation experiments and mechanical properties of investigated gold film are obtained from the slope of unloading part of load-displacement curve. In contrast to aforementioned approach, we measured residual imprints diagonal d after unloading. Our approach gives possibility to be obtained not only hardness and Youngs modulus of investigated thin film, but it gives possibility to be obtained in addition yield strength, Poissons ratio, strength coefficient and strain hardening exponent. 2. Modeling of indentation process The material model used in present work is elastic-plastic with nonlinear hardening (Von Misses criterion for plasticity with isotropic hardening is used to model the plastic behaviour of the deformable body). The model involves the following material parameters: Youngs modulus E , Poissons ratio , yield strength p , strength coefficient K and strain hardening exponent n . The evolution of p during plastic deformation is given by: (2.1)

p (

) = (1 + K )
pn

0.2 p

,
p

where 0.2 is initial yield stress and p

is accumulated equivalent plastic strain .

The boundary value problem is defined under the following assumptions: a) the indentation process is quasistatic; b) the deformable axis symmetric specimen is composed by an isotropic linear elasticplastic with linear hardening substrate and elastic-power law plastic film; d) the indenter is modeled as a rigid body; e) full adhesion between the film and the substrate is assumed; f) the friction forces in the contact area are neglected; g) no stress-strain prehistory is taken into account. Because of the axial symmetry the boundary condition on G1 is (see Fig.1): (2.2)

u y G1 = 0 .
u x G5 = 0 .

The deformable body is imposed on a rigid base and this gives the following boundary condition on the surface G5 : (2.3) Because of the acceptance for full adhesion between the film and the substrate, the displacement filed u on G6 is continuous:

Determination of mechanical properties of thin gold films (2.4)

u 1 = u 2 , ( x, y ) G6 .

Fig.1. Scheme of the boundary value problem for substrate and thin layer. 3. Experimental part

Fig.2. Scanning electron microscopy (SEM) micrograph of the structure of investigated gold layer.

We realized microindentation experiment of the gold film with thickness 10m, which was electrochemically deposited on brass substratum with 0.5 mm thickness. Fig.2 shows the microstructure of the gold film.Mechanical properties of the brass (CuZn36) substratum are known from our previous investigations [2]. The indentation was implemented through Vickers microhardness tester Leitz Wetzlar (Germany) with indenter - tetrahedral diamond pyramid with angle 136. Pressing of the specimen with the indenter was realized within 10 seconds, while the applied loads are respectively 0.049N, 0.1471N, 0.1961N, 0.2942N, 0.5393N, 1.03N, 2.01N, 2.991N, 4.952N. We measured residual imprints diagonal d through a microscope. Seven measurements for each of pointed loadings have been done, from which minimum and maximum values were eliminated. The indentation depth was determined according to [3] through the formula: (3.1) h = 0.14285d In this study, indentation data points are obtained after the indenter is removed. This way the displacement h is the depth of the residual imprint. As a result of experimental measurements was built load-displacement curve P h . 4. Numerical simulations The above described indentation process of microindentation is modelled numerically by means of finite-element code MSC.MARC. The boundary value problem is based on the model described in section 2. The rectangular area from substrate and thin film is approximated by 2200 4-nodes isoparametric finite

S. Cherneva, R. Iankov, D. Stoychev elements. The geometry of the domain is given in figure 1: l1 = 0.51mm, l 4 = 2mm and the thickness of the bright gold film is l5 = 0.01mm. The Vickers indenter is replaced by equivalent cone with angle 70.3. As initial values for the thin layer material properties are taken the material characteristics of the bulk gold taken from literature (see Table1). We realized a series of numerical simulations where we compared the experimental and calculated load-displacement curves.
Table 1. Mechanical properties of gold type of material method of material parameters determination the gold film from this work with thickness 10 m gold films with thickness 0.5 m [4] [5] bulk gold [5] standard tensile test 0.11 0.15 [6] 78 by microindentation and trialerror approach based on finite element simulation by tensile test and transmission electron microscopy 0.33 52 5 5 -

p
[GPa]
0.30

[GPa] []
55 0.5

n []

0.2

This way we performed trialerror procedure in order to obtain the material parameter set that gives the best fit to the experimental data. The criterion for good coincidence between numerical and experimental results is following:

100 10%, (4.1) where N are number measurements, u iFEM are displacements, which are obtained
N

u FEM u exp = i exp i u max i =1

from numerical simulations at each of aforementioned nine loadings, u iexp are experimental obtained displacements at each of aforementioned nine loadings and exp u max is the maximum measured displacement. Fig.3 shows the comparison between the experimental and numerical results for the process of microindentation.

Determination of mechanical properties of thin gold films

140
6 5

Experimental points Experimental curve

2

120 100 80 HV 60
1

4 P [N ] 3 2 1

2d-simulations for the thin film

40 20 0 0.00E+0 2.00E-06 4.00E-06 6.00E-06 8.00E-06 1.00E-05 1.20E-05 0 h[m]

0 0.00E+ 2.00E- 4.00E- 6.00E- 8.00E- 1.00E- 1.20E- 1.40E00 06 06 06 06 05 05 05 h[m]

Fig.3. Comparison between experimental and numerical results, that were obtained from 2D-model of the process of microindentation.

Fig.4. Alteration of the Vickers hardness HV [kg / mm 2 ] of the gold film with increasing of the indentation depth h.

Curve 1 was obtained from numerical simulations with material parameters for bulk gold, that were taken from the literature [5]. Material properties for thin gold layer obtained in the present study are given in Table 1 together with values for bulk gold and thin layer material properties reported by other authors. We obtained quadratic error = 0.3% . The results show that the Youngs modulus of the thin gold film is lower from that of the bulk gold (by reason of the fact that during the process of electrodeposition of the film there are inclusions of carbon, nitrogen, etc.), but the yield stress of the thin gold film is higher than the yield stress of bulk gold (by reason of the fact that our electrodeposited thin gold film is strongly fine grained one, because of the presence of surface-active addends during the process of electrodeposition). Our film has microhardness 126.5 kg / mm 2 . Alteration of the Vickers hardness HV of the gold film with increasing of the indentation depth h is shown of Fig.4. It is obviously that microhardness is almost constant. Therefore the substratum doesnt influence when we determine mechanical properties of the gold film. 5. Conclusions This work is focused on determination of mechanical properties of thin electrochemically deposited gold films. The identification of the elastic-plastic parameters involved in a previously chosen by us model [7] is done by numerical simulation of microindentation experiment and comparison between the model prediction and the measured data. The constitutive model used in the finite element model of the substrate is based on the Von Mises yield criterion in combination with

S. Cherneva, R. Iankov, D. Stoychev a linear hardening law and for the film we used power hardening law. It was realized microindentation experiment of the film and as a result of this the experimental loaddisplacement curve was obtained. After that the process of microindentation was modeled numerically by means of finite element method and numerical loaddisplacement curve was obtained. Subsequently experimental and numerical loaddisplacement curves were compared. The best fit was achieved using trial-error approach. The set of film material parameters which gives the best fit to the experimental data is given in first row of Table 1. For these material parameters we obtained almost full coincidence (difference from 0.3%) between experimental and numerical curves. Therefore the proposed approach can be successfully applied for identification of material parameters of the accepted model. REFERENCES [1] GAMBURG, U. D. Galvanic films, Technosphera Publ. House, Moskow, 2006. [2] CHERNEVA, S. CH. , R. ZL. IANKOV, D. S. STOYCHEV, V. I. KAVARJIKOV. Numerical modeling of microindentation experiment for determination mechanical characteristics of metals and alloys. Journal of Theoretical and Applied Mechanics , 37 (2007), No. 2, 4558. [3] TUSHINSKY, L. , I. KOVENSKY, A. PLOKHOV, V. SINDEYEV, P. RESHEDKO. Coated metal: structure and properties of metal coating compositions. Springer-Verlag, Berlin, 2002. [4] HAQUE, M. , M. SAIF. Deformation mechanisms in free-standing nanoscale thin films: A quantitative in situ transmission electron microscope study. PNAS, 101( 2004), No. 17, 63356340. [5] ESPINOSA, H. , B. PROROK. Size effects on the mechanical behaviour of gold thin films. Journal of Materials Science , 38 (2003), No. 20, 41254128. [6] LEE, D. , X WEI, X. CHEN, M. ZHAO, S. JUN, J. HONE, E. HERBERT, W. OLIVER, J. KYSAR. Microfabrication and mechanical properties of nanoporous gold at the nanoscale. Scripta Materialia, 56 (2007), 437440. [7] IANKOV, R. ZL., S. CH. CHERNEVA, D. S. STOYCHEV. Investigation of material properties of thin copper films through finite element modelling of microindentation test. Applied Surface Science, 254 (2008), No. 17, 5460 5469.