ICMCTF2011 Session E2-3: Mechanical Properties and Adhesion

Friday, May 6, 2011 8:00 AM in Room California

Friday Morning

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8:00 AM E2-3-1 Optimization of the Scratch Test for Specific Coating Designs
Gregory Favaro (CSM Instruments SA, Switzerland); Nick Bierwisch (Saxonian Institute of Surface Mechanics, Germany); Quynh-Huong Duong, Philippe Kempe (CSM Instruments SA, Switzerland); Jürgen Ramm1 (Oerlikon Balzers AG, Switzerland); Norbert Schwarzer (Saxonian Institute of Surface Mechanics, Germany); Beno Widrig (OC Oerlikon Balzers AG, Germany)

The proper design of wear resistant coatings applied to cutting tools comprises the optimization of the mechanical properties (Young's modulus, yield strength, adhesion, intrinsic stresses, fracture, fretting and wear resistance etc.) of the coating-tool system.

The goal is to find material and structural solutions which keep the resulting stress strain field under typical application conditions below the stability limits of the system.

Based on nanoindentation measurements obtained from the coating-tool system which should be optimized, a scratch test is dimensioned with respect to load range and indenter geometry. The measured data from this “Physical Scratch Test” are used to simulate spatial stress profiles and to calculate the von Mises stress characteristics and the maximum tensile stresses in the scratch direction. In a further step, the simulations are used to suggest scratch parameters (“Fine Tuned Scratch Test”) which increase the sensitivity of the test for specific depth regions in the coating-tool architecture and allow improved and more sensitive investigations of critical interfaces, transition layers and surface-near substrate regions.

The tests were performed at PVD coated inserts (nitrides and oxides) and compared with the results obtained from cutting tests.

8:20 AM E2-3-2 A Modified Scratch Test for the Mechanical Characterization of Scratch Resistance and Adhesion of Thin Hard Coatings on Soft Substrates
Thomas Sander, Stephan Tremmel, Sandro Wartzack (University Erlangen-Nuremberg, Germany)

The scratch resistance of coatings and the adhesion between coating and substrate is usually determined in model experiments preceded with sharp diamond indenters. These common methods as described for example in EN 1071-3 often fail for the combination of hard coatings on soft substrates due to very small critical loads. Hence in the industry are used a lot of highly subjective and provisional test methods. On the one hand quantitative comparability is difficult with common methods since defects already occur at very small loads for ductile and relative soft substrate materials like plastics. On the other hand wear of the indenter in contact with hard coatings like pure diamond-coatings requires its cost-intensive replacement.

In this article a macroscopic tribological-mechanical test method is suggested which uses balls of hardened steel as indenters. A wide scope can be applied for both soft and hard coatings and different substrate materials. By variation of the ball-diameter, the normal contact force and the sliding speed different levels of stress and wear can be created to analyse the tribological and mechanical behaviour between body and counterpart as well as the interface of coating and substrate. The method is also suitable for timesaving pilot tests to find out the proper ball size and load for following ball-on-disk-tests on a tribometer. To determine scratch resistance close to reality as usual scratch conditions on consumer products are better represented by a small ball than a sharp diamond indenter. Another benefit of the presented test method is the cost saving acquisition of the balls for indentation in very high quality as they are standard parts in the ball bearing industry. For every test on very hard coatings a new ball can be used with the possibility to detect the wear both on the base object and the counterpart. The occurring failure modes of coating and substrate can be compared also with comparatively easy numerical models to verify the results. Additional to the test concept first results of different coatings will be presented in this paper and compared with the results of common scratch tests.

8:40 AM E2-3-3 The Plastic Deformation of Metallic Thin Films on Substrate Seen Through In Situ TEM Experiments
Marc Legros (CEMES-CNRS, France)
Thin metallic films on substrates exhibit a large resistance to deformation, and in the micron range, this dependence scales linearly with the inverse of the thickness. Such a linear increase of the films strength has been rationalized in term of confined dislocation motion (Nix, [1]). In this fairly simple, and thus popular model, the yield stress of a metallic film on a rigid substrate is attained when threading dislocations start to shear the film, increasing simultaneously the length of interfacial dislocations in their wake. This model leads to correct stress values for pseudo epitaxial metallic films (such as Al or Cu on sapphire) but falls short when it comes to metallic films that possess an amorphous interface with the substrate (Al on oxidized Si for instance) [2]. Considering the image forces seen by the interfacial dislocations in both systems, the opposite effect should be observed.

In films thinner than about 200 nm, yield stress plateaus or even decreases, clearly calling for an alternate relaxation mechanism. Parallel glide of dislocations, a potential symptom of enhanced grain boundary diffusion, is one of the possible substitution process, but so far, it has never been observed elsewhere than in Cu films [3].

Here, we will show that in situ TEM can display the dislocation mechanisms while they operate in thin films and thus directly corroborate or contradict existing theories. Examples will be taken from Al and Cu films on rigid substrates. The stress is induced by the difference of CTE between the film and the substrate, as in wafer curvature experiments. We found that, for thicker films, amorphous interfaces play the role of dislocations sinks, similarly to free surfaces [4]. The increased strength of metallic films with amorphous interfaces is thus dictated by the nucleation of fresh dislocations. In thinner films, scarce dislocation activity is clearly replaced by other processes. Diffusion processes are harder to observe and quantify [5], but plasticity can also be carried out by grain boundary migration[6], similarly to what has been recently observed in nanocrystalline metals [7, 8], and despite the presence of the substrate.

[1] Nix WD. Metall. Trans. A 1989;20A:2217.

[2] Dehm G, Balk TJ, Edongue H, Arzt E. Microelectronic Engineering 2003;70:412.

[3] Balk TJ, Dehm G, Arzt E. Acta Mat 2003;51:4471.

[4] Legros M, Hemker KJ, Gouldstone A, Suresh S, Keller-Flaig RM, Arzt E. Acta Mat 2002;50:3435.

[5] Legros M, Dehm G, Balk TJ, Arzt E. Science 2008;319:1646.

[6] Mompiou F, Caillard D, Legros M. Acta Mat 2009;57:2198.

[7] Rupert TJ, Gianola DS, Gan Y, Hemker KJ. Science 2009;326:1686.

[8] Gianola DS et al. Acta Materialia 2006;54:2253.

9:20 AM E2-3-5 Correlation between Adhesion Strength and Coating/Substrate Mechanical Properties using the Scratch Test Technique
Bo Zhou, Nicholas Randall (CSM Instruments)
Scratch testing, as a mature technique for coating adhesion quantification, has been widely adopted by both industrial and academic fields over recent years. Following the urgent needs of very small materials characterization, nano-scratch testing has gradually replaced the traditional pull-off test for the study of ultra-thin film properties. In this research, the relationship between the adhesion strength and film/substrate mechanical properties was investigated to provide fundamental but crucial knowledge of the scratch mechanism. Five thin films were deposited using sputtering onto different polished substrate materials which span from soft silicon dioxide to hard sapphire. The surface roughness of the bare substrates was measured using Scanning Force Microscopy. Scratch tests were performed using a Nano Scratch Tester with a sphero-conical diamond indenter. A progressive load mode was employed to cause coating failure during scratch on the film surface. The critical values of different failure mechanisms, such as cracking, spallation, and delamination were accurately determined according to the scratch panorama image, penetration and residual depth data. In addition, the Hardness (H) and Modulus (E) values of the thin films and substrates were measured with an Ultra Nanoindentation Tester. The scratch critical failure loads were then plotted versus film/substrate H and E ratios. The relationship developed between these parameters was described in terms of the true mechanism behind scratch adhesion of such hard coatings.

9:40 AM E2-3-6 Numerical and Experimental Analyses of Scratch Tests Conducted on Coated Systems with Residual Stress Gradients
Newton Fukumasu, Roberto Souza (University of Sao Paulo, Brazil); Abel Recco (University of Santa Catarina, Brazil); André Tschiptschin (University of Sao Paulo, Brazil)

In this work, finite element (FEM) and experimental studies were conducted to understand adhesive and cohesive failures in coated systems with thin film residual stress gradients. The FEM analyses considered a rigid indenter applying normal and tangential loads on the coated systems. Three different cases of variation of film compressive stresses were considered. Stresses: (i) increased from the surface to the film/substrate interface; (ii) decreased from the surface to the film/substrate interface or (iii) were uniform along film thickness. In the numerical studies, the mechanical behavior of both coating and substrate was considered elastic-perfectly plastic. In the experimental portion of this work, a set of depositions of titanium nitride thin films was conducted varying the value of substrate bias during deposition, as an attempt to experimentally prepare specimens with the same trend of residual stress gradient as those analyzed numerically. These specimens were later submitted to scratch tests in order to analyze the critical loads obtained in each case. Numerical results provided a comparison of the distribution of stresses obtained in each simulation, indicating a trend of easier film debonding for the conditions where the stress values were more compressive at the interface and decreased towards the surface. This result is in qualitative agreement with the experimental study, in which lower critical loads were observed for the films where deposition started with high values of substrate bias and the bias was reduced as the deposition proceeded.

10:00 AM E2-3-7 Mechanical and Wear Characterization of Electroless Nickel-Boron Coatings
Véronique Vitry, Abdoul-Fatah Kanta, Fabienne Delaunois (Université de Mons, Belgium)

Nanocrystalline electroless nickel-boron deposits were synthesized on steel substrates and submitted to heat treatment under non-reactive atmosphere to enhance their properties. Their mechanical and tribological properties were investigated by various methods including nanoindentation, Taber wear testing and scratch tests. Their structural properties were also studied.

The hardness of the deposits increased from 900 to 1250 hv100 due to optimal crystallization of the nanocrystalline coating while the Taber wear index was halved after heat treatement.

The scratch tests resistance of the coatings was good in both as-deposited and heat treated conditions.

The mechanisms inducing the modification of the mechanical and tribological properties were discussed and they were linked to the structural state of the material.
10:20 AM E2-3-12 Micro-Scratch Testing for Interface Characterizations of Diamond-Coated Tools
Ping Lu (University of Alabama); Xingcheng Xiao, Michael. Lukitsch (General Motors Research and Development Center); Kevin Chou (The University of Alabama)

Interface adhesion is one of the foremost important properties of diamond-coated tools, critically linked to their machining performance. Despite of significant advances in diamond deposition technologies that can produce superior diamond properties, coating-substrate adhesion remains the major challenge to extend tool life and understanding the adhesion characteristics are of primary interests to coated-tool makers and users.

In this study, a micro-scratch tester was applied to evaluate the adhesion of diamond coated carbide tools, about 4 µm thickness, at the room temperature. A diamond indenter with a tip radius of 50 µm was employed. The scratch speed was 2 mm/min with the progressive loading method. The scratch length for each test was 5 mm. The maximum normal forces applied were 30 N. During the testing, tangential force, acoustic emission (AE) signals, and depth of the scratch were acquired. Scratch marks and delamination areas were examined by digital microscopy, white-light interferometery and scanning electron microscopy.

The results indicate that the onset of delamination can be clearly captured from the force and AE signals. Though scratch testing may provide information such as critical loads, the interface characteristics cannot be directly utilized when evaluating interface behaviors of a diamond-coated tool subject to tribological loading. Therefore, a finite element analysis (FEA) model was developed to simulate the scratch process with the interface modeled by a cohesive zone. The results indicate that it is feasible to use FEA combined with scratch tests to evaluate the interface properties, i.e., the cohesive zone strength and characteristic length.

10:40 AM E2-3-8 Investigation of the Mechanical Properties of Hierarchically Structured Gold Nanoparticles
Adam Smith, Yaowu Hao, Efstathios Meletis (University of Texas at Arlington)
Due to the superior properties of nanoparticles over their bulk counterparts, the development of new, novel nanoparticles remains an area of intense investigation. Recent research in our laboratory has resulted in the synthesis of spherical hollow gold nanoparticles (HGNPs) showing three degrees of hierarchy (particle diameter ~100 nm, wall thickness ~20 nm and grain size ~5 nm). Such HGNPs can display very unique mechanical properties. Recent characterization of hierarchically structured CdS hollow nanoparticles has shown them to have a shear strength approaching the theoretical strength of the material. [1] Synthesis of HGNPs in our laboratory provides a golden opportunity to further investigate the mechanical response of such hierarchically structured nanomaterils and develop a broader understanding of their behavior. In the present study, we report results from nanoindentation experiments that were conducted on a series of HGNPs to explore their mechanical response.

[1] Shan, Z. W. et al. Ultra high stress and strain in hierarchically structured hollow nanoparticles. Nature Materials 7, 947-952 (2008).

11:00 AM E2-3-10 Influence of the Nitriding and TiAlN/TiN Coating Thickness on the Mechanical Properties and Adhesion of Duplex Treated AISI H13 Steel
Ricardo Torres, Paulo Soares (Pontifícia Universidade Católica do Parana, Brazil); Carlos Lepienski (Universidade Federal do Parana, Brazil); Roberto Souza, Maria Faria, André Tschiptschin (University of Sao Paulo, Brazil)
AISI H13 die steel substrates were low pressure gas nitrided to different thickness and hardness value. Nitrided and non nitrided samples were subsequently coated with bi-layer TiAlN/TiN to two different thicknesses: 3 and 8 µm. The hardness was measured across the sample thickness and observed to be higher when a thinner coating was deposited over nitrided substrates. The hardness behavior across relatively thin coating was not affected by the nitrided surface hardness or thickness of the nitrided layer in the range of values examined here (80-150 µm). On the other hand, the hardness behavior of thicker coating was affected by the nitrided layer. Moreover, the adhesion of the coating system over nitrided and non nitrided substrates was tested through scratch tests. The adhesion of a thinner coating is better than the adhesion of a thicker coating at given nitrided substrate condition. The adhesion of a thicker coating is influenced by the nitrided case features. A harder and thicker nitrided case improves the adhesion of a thicker coating system. Spallation is the failure mode a thinner coating system while chipping was observed to be the failure mode of a thicker coating system.
11:20 AM E2-3-11 Microstructure and Characterization of Ternary Sputtering Ni-Ru-P Coatings
Yu-Cheng Hsiao, Fan-Bean Wu (National United University, Taiwan)
In the study, the ternary Ni-Ru-P alloy coatings were fabricated by magnetron dual-gun co-sputtering technique. The chemical composition variation of the coatings in terms of sputtering input power was investigated. The Ni-Ru-P coatings exhibited a Ru content ranged from 3.3 to 64.6 at.% as the Ru deposition input power was controlled at 15 to 100W. The phase transformation of the Ni-Ru-P coatings with respect to annealing treatment was analyzed by X-ray diffraction technique. The Ni-Ru-P coatings exhibited an amorphous/nanocrystalline feature under a vacuum annealing temperature up to 450oC. Ni(Ru) and Ni-P precipitation phases under annealing temperature above 500oC were observed. The influence of Ru on the thermal stability of Ni-P-based alloy coating was discussed. The variation in roughness of the alloy coatings attributed by the Ru contents was also analyzed. The sputtered Ni-Ru-P coatings exhibited superior mechanical and anti-oxidation characteristics as compared to the Ni-P coating. The introduction of Ru significantly strengthened the Ni-P-based coating. The Ni-Ru-P coating systems were also compared with Ni-Ru binary coating in order to understand the effect of P in Ni-based coatings.
11:40 AM E2-3-13 Adhesive Interlayers' Effect on the Entire Structure Strength of Glass Molding Tools" Pt-Ir Coatings by Nanotests Determined
F. Klocke (RWTH Aachen University, Germany, CERTH, Greece & IPT, Germany); Konstantinos-Dionysios Bouzakis (Aristoteles University of Thessaloniki, Greece, CERTH, Greece & IPT, Germany); Kyriakos Georgiadis (IPT, Germany); Stefanos Gerardis, G. Skordaris, Maria Pappa (Aristoteles University of Thessaloniki, Greece, CERTH, Greece & IPT, Germany)
Precision glass molding is a medium to large scale production technology of complex optical components with high surface quality and form accuracy. However, the process is only economically viable if a long lifetime of the molding tools can be guaranteed. This can be achieved by using protective coatings on the optical surfaces of the molding tools. The most commonly used coatings for this application are based on noble metals, as they show reduced interaction with the glass during molding. The coatings must have excellent mechanical and chemical properties at high temperatures to withstand the stresses during molding and simultaneously extreme low surface roughness and defects density. The form accuracy of the molding tools is in the nm range and must be maintained even after the coating deposition. Therefore, very thin films of approximately 300 nm thickness are used. High film adhesion and strength properties are necessary for preventing surface defects and coating delamination.

In the described investigations, platinum (Pt)- iridium (Ir) coatings were deposited directly on cemented carbide samples by Physical Vapour Deposition (PVD) process. Moreover, for improving the adhesion, different materials such as of Ni and Cr were employed as adhesive interlayers at various thicknesses. These interlayers were deposited on the substrate before the Pt-Ir film, during the same PVD process. Appropriate experimental procedures were conducted for characterizing the coatings’ mechanical and adhesion properties such as nanoindentations, nano-impact and nano-scratch tests. FEM calculations simulating the films’ loadings during nano-impact test explain the effect of the adhesive interlayer on the entire coating substrate structure strength.

12:00 PM E2-3-9 A Study on the Microstructures and Mechanical Properties of Ti-Al-Cr-Si-N Nanocomposite Thin Films Prepared by Pulsed DC Reactive Magnetron Sputtering System
Po-Chi Huang (Tungnan University); Jyh-Wei Lee (Mingchi University of Technology, Taiwan); Hsin-Pei Chen (Tungnan University, Taiwan); Yu-Chen Chan, Hsien-Wei Chen, Jenq-Gong Duh (National Tsing Hua University, Taiwan)
Surface modification technology can be used to deposit a foreign hard coating material onto the surface of interest to achieve specific properties, such as high strength, adequate adhesion, wear and corrosion resistance. In this study, the Ti-Al and Cr-Si targets were used to fabricate the Ti-Al-Cr-Si-N nanocomposite thin films with various Cr and Si contents by a pulsed DC magnetron sputtering system. The crystalline structure of coatings was determined by a glancing angle X-ray diffractometer. The surface roughness of thin films was explored by an atomic force microscopy (AFM). The surface and cross-sectional morphologies of thin films were examined by a scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The adhesion, hardness and nanotribological properties of thin films were evaluated by a nanoindenter and scratch tester respectively. It was observed that the hardness and nanotribological properties was strongly influenced by the Cr and Si contents of Ti-Al-Cr-Si-N nanocomposite thin films in this work.
Time Period FrM Sessions | Abstract Timeline | Topic E Sessions | Time Periods | Topics | ICMCTF2011 Schedule