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ICMCTF 2012! - CD-Lab Application Oriented Coating Development

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in the mechanical properties indicate bad adhesive properties for one<br />

coating. For quantitative measurement of the interfacial fracture strength<br />

and fracture toughness, micro-cantilevers with a length of about 1.5 µm and<br />

a thickness of about 0.5 µm were prepared by focused ion beam so that the<br />

highest bending stress or stress intensity occurs right at the interface. Using<br />

a force measurement systems, the micro-cantilevers were loaded inside the<br />

SEM and the fracture properties were evaluated. The interfacial fracture<br />

strength of the different interfaces is discussed in terms of the<br />

microstructure, the local mechanical properties and the chemical gradients<br />

in the adhesion layer. It is found that a reduction in the bending strength of<br />

the interface of ~40% results on a macroscopic scale in a change from good<br />

to bad adhesion properties. Furthermore the results of fracture toughness<br />

and bending strength of the interface are compared to the properties of pure<br />

a-c:H.<br />

Using these different approaches, a better understanding on the damage<br />

behavior of thin brittle coatings on ductile substrates is achieved and the<br />

local adhesion strength is correlated to the coating microstructure and<br />

chemical composition.<br />

Funding by DFG Cluster of Excellence Engineering of Advanced Materials<br />

(EAM)<br />

9:20am E2-1-5 Study of adhesion and cracking of TiO2 coatings on a<br />

Ti alloy using an impact-sliding testing instrument, X. Nie<br />

(xnie@uwindsor.ca), University of Windsor, Canada<br />

Different thickness and surface porosity of TiO2 coatings on Ti alloys<br />

appear to have a different combination of bioactivity and chemical stability.<br />

For bio-implants of dentals, the coating thickness and surface morphology<br />

would also influence mechanical integrity. There is a need in further study<br />

on fatigue cracks and wear property of the coatings under simulated load<br />

conditions of dental surgery operations and implant applications. In this<br />

paper, a newly-developed impact-sliding testing instrument is used to<br />

simulate those dental applications under a variety of forces where impacts,<br />

scratch, fretting, and other relevant wear behaviour occur. The research<br />

result showed that the wear behaviour was significantly affected by the<br />

coating thickness and surface porosity. The impact-sliding instrument can<br />

be used as a tool in study of coating adhesion and cracking for dental<br />

implant applications.<br />

9:40am E2-1-6 Influence of oxide film properties on the adhesion<br />

performance of epoxy-coated aluminium, Ö Özkanat<br />

(o.ozkanat@tudelft.nl), Delft University of Technology, Netherlands;<br />

Materials innovation institute (M2i), Netherlands, J.M.C. Mol, J.H.W. de<br />

Wit, Delft University of Technology, Netherlands, H. Terryn, Vrije<br />

Universiteit Brussel, Materials innovation institute (M2i), Belgium<br />

Adhesion of organic coatings and corrosion resistance of<br />

polymer/(hydr)oxide/aluminium interfaces plays pivotal role in the<br />

engineering of lightweight components. Interfacial bonds at the<br />

polymer/metal joints have to withstand high mechanical forces and<br />

corrosive attack to protect the functional properties of coated metals.<br />

Therefore, it is crucial to understand and to control the delamination of<br />

organic coatings and the molecular adhesion forces originating at the<br />

interface in order to achieve the long-term stability of these composites.<br />

Adhesion strength is both influenced by the functionality of the organic<br />

molecules at the interface and the surface properties of thin oxide film e.g.<br />

hydroxyl content, oxide thickness and surface morphology. In this work, we<br />

present how the surface properties affect the adhesion performance of<br />

coated systems. First, different pretreatments (acid, alkaline and immersion<br />

in boiling water) were given in order to create variations in the surface<br />

properties of aluminium substrate. Then differently pretreated bare surfaces<br />

were characterized by means of surface sensitive techniques [1] in which<br />

Scanning Kelvin Probe (SKP), X-Ray Photoelectron Spectroscopy (XPS),<br />

Visible Spectroscopic Ellipsometry (VISSE) and Fourier Transform<br />

Infrared Spectroscopy (FTIR) were utilized in order to evaluate Volta<br />

Potential, hydroxyl fraction, oxide thickness and chemical composition,<br />

respectively. Since the oxide properties of aluminium might be extremely<br />

sensitive to the small changes in the environmental conditions, effect of<br />

ambient humidity (40% RH or 90% RH) and aging (40min vs 240min) on<br />

the oxide film properties was also revealed. Results showed [1] that<br />

pseudoboehmite oxide exhibited the highest hydroxyl fraction and oxide<br />

thickness; it was also shown that all differently pretreated surfaces along<br />

with the reference surface were influenced by both ageing and humidity.<br />

This was followed by the molecular bonding of functional groups -<br />

representative interfacial adhesive molecules- on differently pretreated<br />

surfaces by means of Volta potential shift [2] (SKP) and affinity (XPS).<br />

Finally, the influence of the oxide film properties on macroscopic adhesion<br />

of epoxy-coatings was investigated by means of mechanical testing to<br />

evaluate the performance of coated systems. It was observed from Shear<br />

testing and Bell Peel testing that variations in the thin oxide film properties<br />

resulted in different adhesion performance. This research presents a relation<br />

Thursday Morning, April 26, <strong>2012</strong> 78<br />

between the adhesion performance and the oxide film properties of the<br />

aluminium substrates.<br />

[1] Ö. Özkanat, B. Salgin, M. Rohwerder, J. M. C. Mol, J. H. W. de Wit ,<br />

H. Terryn, Journal of Physical Chemistry C <strong>2012</strong>, 116, 1805.<br />

[2] Ö. Özkanat, B. Salgin, M. Rohwerder, J. H. W. de Wit , J. M. C. Mol,<br />

H. Terryn, Surface and Interface Analysis <strong>2012</strong>, Accepted.<br />

10:00am E2-1-7 Adhesion and fatigue properties of TiB2-MoS2<br />

composite coatings deposited by closed-field unbalanced magnetron<br />

sputtering, F.B. Bidev, Ö. Baran (obaran@erzincan.edu.tr), E. Arslan, Y.<br />

Totik, İ. Efeoglu, Ataturk University, Turkey<br />

In this work, TiB2-MoS2 composite coatings deposited by closed-field<br />

unbalanced magnetron sputtering (CFUBMS) technique using Taguchi<br />

L9(3 4 ) experimental method.The structural properties of TiB2-MoS2<br />

composite coatings were analyzed SEM and XRD.The hardness of coatings<br />

were measured using microhardness tester.Adhesion and fatique properties<br />

of coatings have been scratch tested in two modes. A multi-mode operation<br />

was used as sliding-fatigue, like multi-pass scratching in the same track at<br />

different fractions of critical load (unidirectional sliding) and a standard<br />

mode using progressive load operation. Failure mechanisms were discussed<br />

according to SEM examinations of the scratch tracks.<br />

Key Words:TiB2-MoS2 ,Taguchi method, Adhesion, Multi-pass scratch<br />

10:20am E2-1-8 <strong>Coating</strong> thickness and interlayer effects on CVDdiamond<br />

film adhesion to cobalt-cemented tungsten carbides, P. Lu,<br />

The University of Alabama, US, H. Gomez, University of South Florida,<br />

US, X. Xiao, M.J. Lukitsch, A. Sachdev, General Motors, US, D. Durham,<br />

A. Kumar, University of South Florida, US, K. Chou (kchou@eng.ua.edu),<br />

The University of Alabama, US<br />

In this study, diamond coating adhesion on cobalt-cemented tungstencarbide<br />

(WC-Co) substrates was investigated using scratch testing. In<br />

particular, the methodology was applied to evaluate the effects of the<br />

coating thickness and interlayer on coating delaminations. In the coating<br />

thickness effect study, substrate surface preparations, to remove the surface<br />

cobalt, prior to diamond depositions was common chemical etching using<br />

Murakami solutions . On the other hand, to study the interlayer effect, by<br />

halting the catalytic effect of the cobalt binder, two different interlayers,<br />

Cr/CrN/Cr and Ti/TiN/Ti, were deposited to WC-Co substrate surfaces (no<br />

chemical etching) by using a commercial physical vapor deposition (PVD)<br />

system in a thickness architecture of 200nm/1.5µ m/1.5µ m, respectively.<br />

Diamond films were synthesized by using a hot-filament chemical vapor<br />

deposition (HFCVD) reactor at a gas mixture of 6 sccm of CH4 and 60 sccm<br />

of H2, with varied deposition times.<br />

Scratch testing was conducted on the fabricated specimens using a<br />

commercial machine, at a maximum normal load of 20 N and a speed of 2<br />

mm/min. It is noted that the onset of coating delamination can be clearly<br />

identified by high-intensity acoustic emission (AE) signals when such<br />

events occur, which can be used to determine the critical load. Scratched<br />

track geometry was also characterized by white-light interferometry and<br />

scanning electron microscopy.<br />

The results show that the adhesion of the diamond coating increases with<br />

the increased coating thickness, with a nearly linear relation, in the range<br />

tested. In a previous investigation, finite element (FE) simulations of<br />

scratching on a diamond-coated carbide were developed, using a cohesive<br />

zone model, to evaluate coating delaminations related to interface<br />

characteristics. The FE model was applied in this study to investigate the<br />

coating thickness effect on delamination critical loads and the results<br />

suggest a linear relation too. For the two types of interlayer materials tested,<br />

either of them seems to be effective and the diamond coating with Tiinterlayer<br />

shows poorer adhesion comparing to the Cr-interlayer coating.<br />

10:40am E2-1-9 On the effect of pressure induced change of Young's<br />

modulus, hardness and yield strength, N. Schwarzer<br />

(n.schwarzer@siomec.de), Saxonian Institute of Surface Mechanics,<br />

Germany<br />

It will be shown how relatively simple models simulating the bond<br />

interaction in solids applying effective potentials like Lennard-Jones and<br />

Morse can be used to investigate the effect of pressure induced changes of<br />

Young's modulus and yield strength of these solids. Relatively simple<br />

dependencies of the bulk-modulus B on the pressure P being completely<br />

free of microscopic material parameters are derived wherever the solid bond<br />

interaction can be described or at least partially described by Lennard-Jones<br />

potentials. Instead of bond energies and length only specific integral<br />

constants like Young's modulus and Poisson's ratio are of need. The<br />

influence of the pressure induced Young's modulus change B(P) is<br />

discussed especially with respect to mechanical contact experiments.<br />

Thereby it is also shown how the extraction of critical decomposition

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