Cohesive & Adhesive Failure and Contact Damage of Diamond- Like Carbon (DLC) Coated Titanium Substrates
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1 Research Collection Doctoral Thesis Cohesive & Adhesive Failure and Contact Damage of Diamond- Like Carbon (DLC) Coated Titanium Substrates Author(s): Bernoulli, Daniel Publication Date: 2014 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 Diss. ETH No Cohesive & Adhesive Failure and Contact Damage of Diamond-Like Carbon (DLC) Coated Titanium Substrates A thesis submitted to attain the degree of DOCTOR OF SCIENCES of ETH ZURICH (Dr. sc. ETH Zurich) Presented by Daniel Bernoulli MSc EPF in Materials Science & Engineering, EPFL & ETHZ born on citizen of Basel Accepted on the recommendation of Prof. Dr. Ralph Spolenak, examiner Prof. Dr. André R. Studart, co-examiner Prof. Dr. Karsten Durst, co-examiner 2014
3 Summary Thin surface layers are utilized in many modern technological applications for optimization of surface properties such as hardness or wear. Hydrogenated diamond-like carbon (DLC) is a hard and wear resistant material and is therefore already used as a surface layer in tribological applications. However, cohesive and adhesive failure as well as contact damage often limit the lifetime of the DLC-substrate combination. Knowledge of the factors and mechanisms influencing their failure are of profound importance for industrial applications and also for the further development of protective coating systems. DLC films on titanium substrates is, on the one hand, important for technical applications, e.g. for biomedical applications. On the other hand, from a scientific perspective, it is also an excellent model system for understanding the failure mechanisms of a hard and brittle film on a ductile metallic substrate. Thus, the cohesive and adhesive failure and the contact damage of DLC coated titanium substrates is studied in this thesis not only by analyzing the variation of the DLC film thicknesses, but also by investigating the role of the elastic-plastic deformation behavior of the titanium substrate. The cohesive and adhesive failure is studied under uniaxial loading conditions using microtensile testing, whereas the contact damage is induced by microindentation and complemented by finite-element analysis. From the uniaxial loading experiments, the critical energy release rates for cohesive and adhesive failure as well as the fracture toughness of DLC are determined quantitatively. Additionally, it is observed that the fracture strength and the onset strain of delamination increase significantly with decreasing DLC film thickness. However, the contact damage analysis reveals that the DLC film thickness, the elastic-plastic deformation behavior of the substrate, the applied pressure and the fracture toughness affect the contact damage creation, evolution and final morphology significantly. VII
4 The combined analysis of the cohesive and adhesive failure and contact damage results in a film thickness optimization process for DLC coated ductile metallic substrates. On the one side, the DLC film thickness needs to be as thin as possible to increase fracture strength and onset strain of delamination. On the other side, in order to minimize plastic deformation of the substrate upon indentation, the DLC film should be as thick as possible. To circumvent these opposing predictions of optimal film thicknesses, interlayers are deposited between the DLC film and the titanium substrate. The interlayer has to increase the mechanical stability of the DLC film and it also has to shield the titanium substrate from plastic deformation upon contact damage creation. To design an interlayer, which fulfills these requirements, the influence of the material structure, such as its phase, on the DLC film and titanium substrate should be known. The effect of phase can very well be studied with tantalum because it exists in the stable body-centered cubic α-phase and in the metastable tetragonal β-phase. To deposit the desired tantalum phase on titanium substrates, a method using a reactive sputter deposited tantalum nitride seed layer is developed. α- tantalum forms by depositing a 15 nm tantalum nitride seed layer while in its absence, β-tantalum forms. This deposition method additionally shows that, besides epitaxy, the surface chemistry of the base material substantially affects the growth of a particular phase. With this seed layer method DLC coated titanium substrates with interlayers of α- and β-tantalum are produced and the influence of the phase on the cohesive and adhesive failure and contact damage is examined. The analysis shows that the contact damage can be remarkably reduced with an α-tantalum interlayer due to plastic deformation of the ductile interlayer material. VIII
5 Zusammenfassung Beschichtung spielen in modernen technischen Anwendungen oftmals eine tragende Rolle, da damit Oberflächeneigenschaften wie Härte oder Verschleiss gezielt angepasst und verändert werden können. Wasserstoffhaltiger, diamantähnlicher Kohlenstoff (engl. hydrogenated diamond-like carbon (DLC)) ist ein hartes und verschleissarmes Beschichtungsmaterial und wird daher bereits in tribologischen Anwendungen verwendet. Kohäsives und adhäsives Versagen wie auch Kontaktschadenbildung limitieren aber oftmals die Lebensdauer oder führen zu plötzlichem Versagen solcher DLC Schichten. Kenntnisse über die Einflüsse und Mechanismen die zu deren Versagen führen können, sind daher sowohl von grosser Bedeutung für industrielle Anwendungen als auch für die Weiterentwicklung von Schichtsystemen. DLC auf Titan ist einerseits für technische Anwendungen von Interesse, z.b. für biomedizinische Anwendungen, andererseits ist es auch ein exzellentes Modellsystem für das allgemeine Verständnis von Versagensmechanismen einer harten und spröden Schicht auf einem duktilen, metallischen Grundmaterial. In dieser Dissertation wird daher das kohäsive und adhäsive Versagen wie auch der Kontaktschaden von DLC beschichteten Titansubstraten untersucht, unter Berücksichtigung der DLC Schichtdicke und dem elastisch-plastischen Verhalten des Titansubstrates. Das kohäsive und adhäsive Versagen wird mit uniaxialen Zugversuchen untersucht, wobei Mikroindentierung ergänzend mit der Finiten-Elementen Methode zur Kontaktschadenanalyse verwendet werden. Anhand der uniaxialen Zugversuche kann die kritische Energiefreisetzungsrate für kohäsives und adhäsives Versgagen sowie die Bruchzähigkeit des DLC quantitativ bestimmt werden. Dabei wird beobachtet, dass die Bruchfestigkeit und die Delaminationsdehnung mit abnehmender Schichtdicke signifikant zunehmen. Bei der Analyse der Kontaktschadenbildung zeigt sich hingegen, dass nicht nur die DLC Schichtdicke son- IX
6 dern auch die plastische Verformung des Substrates, der angelegte Druck und die Bruchzähigkeit der DLC Schicht den Kontaktschaden wesentlich mitbeeinflussen. Die Erkenntnisse über die kohäsiven und adhäsiven Versagensmechanismen und die Kontaktschadenbildung von DLC beschichteten Titansubstraten führen zu einem Schichtdickenoptimierungsprozess. Einerseits muss die DLC Schicht möglichst dünn gehalten werden, um Bruchfestigkeit und Delaminationsdehnung der Schicht zu erhöhen. Andererseits sollte, um plastische Verformung des Substrates bei Kontaktschadenbildung zu minimieren, die DLC Schicht möglichst dick sein. Um dieses Problem des DLC Schichtdickenoptimierungsprozess zu umgehen, werden zwischen dem DLC und dem Titansubstrat Zwischenschichten abgeschieden. Die Zwischenschichten müssen sowohl die mechanische Stabilität der DLC Schicht erhöhen als auch bei Kontaktschadenbildung vor plastischer Verformung des Substrates schützen. Um jedoch eine solche Zwischenschicht designen zu können, müssen die Einflüsse der Materialstruktur, z.b. der Phase, auf die DLC Schicht und das Titansubstrat bekannt sein. Der Einfluss der Phase kann mit Tantal sehr gut untersucht werden, da es sowohl in der kubisch-raumzentrierten α-phase als auch in der tetragonalen β-phase existiert. Damit die gewünschte Tantalphase auf dem Titansubstrat abschgeschieden werden kann, wird eine Methode mit einer reaktiv hergestellten Tantalnitridkeimschicht entwickelt. Bei der Verwendung einer solchen 15 nm Tantalnitridkeimschicht wächst Tantal in der α-phase. Wird jedoch eine solche Tantalnitridkeimschicht nicht verwendet, formt sich die β-phase. Diese Beschichtungsmethode zeigt zudem, dass neben Epitaxie, die Oberflächenchemie des Grundmaterials das Phasenwachstum wesentlich mitbeeinflusst. Mit dieser Keimschichtmethode werden DLC beschichtete Titansubstrate mit α- und β-tantal Zwischenschichten hergestellt und der Einfluss der Phase auf das kohäsive und adhäsive Versagen sowie die Kontaktschadenbilung untersucht. Es zeigt sich, dass durch die plastische Deformation einer α-tantal Zwischenschicht die Kontaktschadenbilung merklich reduziert werden kann. X
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