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Fatigue in thin films Lifetime and damage formation.pdf

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920<br />

O. Kraft et al. / Materials Science <strong>and</strong> Eng<strong>in</strong>eer<strong>in</strong>g A319–321 (2001) 919–923<br />

It is the aim of this paper to elucidate the fatigue<br />

mechanisms <strong>in</strong> constra<strong>in</strong>ed volumes <strong>and</strong> to determ<strong>in</strong>e<br />

fatigue lifetimes under these conditions. We present<br />

two methods, which we developed to study the fatigue<br />

behavior of th<strong>in</strong> metal <strong>films</strong> on substrates: The<br />

first technique <strong>in</strong>volves tensile test<strong>in</strong>g of Cu <strong>films</strong> deposited<br />

onto elastic polyimide substrates. Tensile test<strong>in</strong>g<br />

of these specimen results <strong>in</strong> tension–compression<br />

cycles <strong>in</strong> the plastically deformed th<strong>in</strong> film while the<br />

substrate is elastically deformed only. The second<br />

technique utilizes the cyclic deflection of th<strong>in</strong> Ag <strong>films</strong><br />

deposited onto micromach<strong>in</strong>ed SiO 2 cantilever beam<br />

us<strong>in</strong>g a nano<strong>in</strong>dentation system.<br />

2. Experimental<br />

2.1. Tensile test<strong>in</strong>g<br />

For process<strong>in</strong>g of the tensile specimen, shown <strong>in</strong><br />

Fig. 1a, the 125 m thick polyimide substrates (Kapton,<br />

Du Pont) were <strong>in</strong>itially cleaned by r<strong>in</strong>s<strong>in</strong>g with<br />

ethanol <strong>and</strong> pressurized CO 2 . Then, the sample was<br />

mounted <strong>in</strong> the deposition system (base pressure of<br />

5×10 −7 mbar) <strong>and</strong> activated by an oxygen plasma<br />

(O 2 pressure 1×10 −2 mbar, power 100 W, bias<br />

−300 V). Without break<strong>in</strong>g vacuum, 3 m thick Cu<br />

<strong>films</strong> were then sputter deposited at a substrate temperature<br />

of 300°C, a rate of 60 nm per m<strong>in</strong> with an<br />

Ar pressure of 2×10 −3 mbar, a power of 150 W<br />

<strong>and</strong> a bias of −80 V. After deposition, the samples<br />

were annealed <strong>in</strong> a vacuum furnace (6×10 −6 mbar)<br />

at a temperature of 400°C.<br />

The tensile tests were performed <strong>in</strong> an electromechanical<br />

tensile tester (Zwicki 1120, Zwick) under<br />

load control. Samples were cyclically loaded between<br />

a m<strong>in</strong>imum load of 2 N to maximum loads <strong>in</strong> the<br />

range of 15–60 N. Under these conditions, the film is<br />

stra<strong>in</strong>ed with constant total stra<strong>in</strong> ranges between 0.7<br />

<strong>and</strong> 2.1% as determ<strong>in</strong>ed from the crosshead displacement<br />

<strong>and</strong> monitored as a function of the number of<br />

cycles. It is not possible to determ<strong>in</strong>e the film stress<br />

us<strong>in</strong>g this configuration because the externally applied<br />

force is predom<strong>in</strong>antly governed by the mechanical<br />

properties of the substrate. However, microtensile<br />

tests on comparable samples us<strong>in</strong>g an X-ray diffraction<br />

technique enabled the measurements of stress–<br />

stra<strong>in</strong> behavior dur<strong>in</strong>g such experiments as<br />

exemplified <strong>in</strong> Fig. 1b [11]. On load<strong>in</strong>g <strong>and</strong> unload<strong>in</strong>g,<br />

the film is plastically deformed <strong>in</strong> tension <strong>and</strong> <strong>in</strong><br />

compression for a total <strong>and</strong> plastic stra<strong>in</strong> range of 0.5<br />

<strong>and</strong> 0.15%, respectively.<br />

2.2. Microbeam bend<strong>in</strong>g<br />

Fig. 1. Microtensile test<strong>in</strong>g; (a) Sample geometry of the 125 m thick<br />

polyimide foil substrate <strong>and</strong> the Cu film sputtered <strong>in</strong> the middle<br />

section of the dog-bone shaped sample. (b) Typical stress-stra<strong>in</strong><br />

behavior for a Cu film on a polyimide substrate dur<strong>in</strong>g cyclic load<strong>in</strong>g<br />

as measured by X-ray diffraction (second cycle of 0.7 m thick Cu<br />

film, from [11]). The total applied stra<strong>in</strong> range of the cycle is 0.5%,<br />

whereas the plastic stra<strong>in</strong> range amounts only to about 0.15% as<br />

<strong>in</strong>dicated by the arrow with<strong>in</strong> the hysteresis loop.<br />

The microbeam samples are shown schematically <strong>in</strong><br />

Fig. 2a. They consist of a 2.83 m thick SiO 2 layer<br />

<strong>and</strong> a th<strong>in</strong>ner Ag film. The Ag <strong>films</strong>, rang<strong>in</strong>g from<br />

0.2 to 1.5 m <strong>in</strong> thickness, were sputter deposited at<br />

a temperature of about −190°C <strong>and</strong> annealed at +<br />

100°C. A detailed description of film deposition <strong>and</strong><br />

the test<strong>in</strong>g procedure is given <strong>in</strong> [12]. The test<strong>in</strong>g procedure<br />

is briefly described as follows, the beams are<br />

deflected by a commercial nano<strong>in</strong>dentation system<br />

(Nano II, MTS Corp.), which applies a cyclic load<br />

P=P mean +P o cos(2t), where P mean is the mean<br />

load, P o the load amplitude <strong>and</strong> the frequency,<br />

which was chosen to be 45 Hz. In this configuration,<br />

the largest stra<strong>in</strong> occurs at the fixed end of the beam<br />

(as <strong>in</strong>dicated <strong>in</strong> Fig. 2a). Based on elastic beam bend<strong>in</strong>g<br />

theory, this stra<strong>in</strong> can be calculated from the<br />

lever length L <strong>and</strong> the applied load as:<br />

= P(L−x) (z−q) (3)<br />

IE<br />

where I is the moment of <strong>in</strong>ertia, E the Young’s<br />

modulus of the substrate material, q the position of<br />

the neutral axis, <strong>and</strong> x <strong>and</strong> z the coord<strong>in</strong>ates along<br />

the length <strong>and</strong> the thickness of the beam. The mo-

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