ICMCTF2009 Session E3-1: Tribology of Nanostructured and Amorphous Films

Thursday, April 30, 2009 1:30 PM in Room California

Thursday Afternoon

Time Period ThA Sessions | Abstract Timeline | Topic E Sessions | Time Periods | Topics | ICMCTF2009 Schedule

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1:30 PM E3-1-1 Friction Behavior of Nanocrystalline Diamond Coatings at Variable Sliding Speeds
N. Theodore (Naval Research Laboratory / North Carolina State University); K. Wahl (Naval Research Laboratory)
Tribology studies were performed on nanocrystalline diamond coatings to investigate changes in friction with sliding speed. Microstructure, surface morphology, and composition of the coatings were characterized using X-ray diffraction (XRD), atomic force microscopy (AFM), interferometry, and infrared and Raman spectroscopy. The nanocrystalline diamond coatings possessed crystallite sizes ranging from to 8 to 60 nm. These nanocrystalline diamond coatings produced similar visible wavelength Raman absorption bands with a peak at 1332 cm-1 typical of crystalline diamond bonding, strong peaks at 1340 cm-1 and 1580 cm-1 characteristic of the D and G peaks in sp2 hybridized carbon, and peaks at 1135 cm-1 and 1470 cm-1, which are commonly attributed to polyacetylene bonding. Reciprocating sliding tests, using sapphire and diamond counterfaces were performed in controlled air and nitrogen environments with variable humidity. The lo ad and track length were fixed at 3 N and 5 mm, respectively, and the sliding speed was varied between 100 µm/s to 2 mm/s. Sliding with either diamond or sapphire counterfaces resulted in low friction values, between 0.03 and 0.08. However, in diamond-on-diamond tests, slowing the oscillation speeds caused a subtle but noticeable reduction in the average friction value by about 5%. Fourier transform infrared (FTIR) and Raman spectroscopy were used to examine tribochemical changes on the worn surfaces.
1:50 PM E3-1-2 Tribology of Deuterated Diamond-Like Carbon Films : An Imaging TOF-SIMS Study
O.L. Eryilmaz, A. Erdemir, G. Kartal (Argonne National Laboratory)
In this study, we investigated friction and wear behavior of deuterated diamondlike carbon (DLC) films in dry nitrogen and hydrogen environments. The coatings were synthesized in a gas discharge plasma by applying 500 V rf. power to the substrates. Combination of deuterated methane, methane, hydrogen and/or deuterium mixtures with different ratios were used during deposition. The highly-hydrogenated or deuterated DLC films provided superlow friction (i.e., less than 0.01) regardless of the test environments, while the films that are hydrogen/deuterium-free or –poor had to be tested in hydrogen- and/or deuterium-containing test environments to attain low friction. When tested in dry nitrogen or vacuum, these hydrogen/deuterium-free films exhibited very high friction and wore out very quickly. All test were performed using pin-on-disk machines under 2-10 N loads and at 0.2 to 0.5 m/s sliding velocities. Near surface chemistry and depth profiles of sliding surfaces were analyzed by using time of flight secondary Ion Mass Spectroscopy (ToF-SIMS) and based on the results of surface analytical and tribological studies a mechanistic explanation was provided for the superlow friction behavior of hydrogen- and deuterium-rich DLC films.
2:10 PM E3-1-3 Super-Low Friction of Carbon-Based Coatings in Nitrogen Gas
K. Adachi (Tohoku University)
Carbon-based coatings such as carbon nitride (CNx)coatings exhibit a wide range of very attractive properties such as low friction and wear, good thermal and chemical stability which make them very suitable for demanding mechanical applications. In sliding of CNx-coatings in nitrogen (N2) gas stream and/or atmosphere, it provides super low friction. The beneficial effect of N2 gas on reducing friction of carbon-based coatings is much more enhanced by selection of counter material, coating condition, surface roughness of the coatings, atmospheric humidity and running-in condition, which is pre-sliding before introducing N2 gas to the sliding interface. In this presentation, comprehensive overviews of the unique lubricious effects of “Nitrogen” on friction with carbon-based coatings are introduced. Based on those attractive results high potential of carbon-based coatings for future successful tribological usage by controlling atmospheric gases is discussed.
2:50 PM E3-1-5 Tribological Behavior of DLC Coated Spinal Disk Implants
G. Thorwarth, U. Müller, C.V. Falub, R. Hauert, B. Weisse (Empa, Switzerland); C. Voisard (Synthes GmbH, Switzerland); M. Tobler (IonBond AG, Switzerland)

Coatings from diamond-like carbon (DLC) have been proven to be an excellent choice for wear reduction in many technical applications. Also, a multitude of attempts for adaption to the MedTech field has been undertaken. However, data gained from realistic in-vitro test setups are in short supply despite being quintessential for application development; the prediction of layer stability and failure mechanisms in the human body environment are important tasks still to be researched.

In our team’s efforts to develop DLC implant coatings with predictably stable layer adhesion in the human body, a new type of simulator has been developed for testing of spinal disk implants. Test results gained from this setup using coated and uncoated spinal disk replacements are presented and compared with conventional tribotests. The relevant differences and possible factors leading to implant failure are discussed. Requirements on the DLC and interfacial layers in the bio-tribo environment are suggested.

3:10 PM E3-1-6 Tribological and Mechanical Properties of Nanostructured Hydrogenated Amorphous Carbon and Titanium Diboride Films
B. Zhao, Y.W. Chung (Northwestern University)
Hydrogenated amorphous carbon films are of great interest due to their favorable ultra-low friction and low wear rate properties in dry environments. Our work demonstrated that sulfur doping of hydrogenated carbon films enabled them to achieve ultra-low friction performance in both dry and humid environments. However, these films have a hardness of 7 - 10 GPa and an elastic modulus around 80 GPa, which are too low for some high stress applications. Formation of nanostructured coatings is known to improve hardness. With the aim to produce hard, low-friction coatings, we synthesized nanolayered and nanocomposite films of sulfur-doped and undoped hydrogenated carbon and titanium diboride using dual-target magnetron sputtering. Titanium diboride deposited by this method had a hardness >30 GPa. This paper will discuss the film structure and how such structure correlates with its tribological and mechanical properties.
3:30 PM E3-1-7 When and Why a-c:H Films are Hydrophobic?
L.V Santos (National Institute for Space Research - INPE, Brazil); V.J. Trava-Airoldi, A.F. Azevedo, R.P.C.C. Statuti, P.A. Radi (INPE - Instituto Nacional de Pesquisas Espaciais, Brazil)
Lots of people have been working with a-c:H films for different kinds applications one of that is protective hydrophobic coatings. The development of a-c:H hydrophobic films have been studding through power supply system deposition range , surface roughness, and from nom metallic chemical elements interactions. In this paper we showed that the hydrofobicity or hydrophilic tendency from a-c:H films changes with the hydrogen content in the bulk of the film. To support our argument we showed the Raman, ERDA and AFM analyses from five different a-c:H content films correlated with contact angle results. All results were correlated with roughness films topography analyzed by atomic force microscopy. The results showed that a-c:H films hydrofobicity increase when hydrogen content decrease. When the content of bulk film has huge hydrogen connections these bonds connections increase the chemical structural disorder of amorphous carbon film them it increase the hydro-affinity. Th e carbon and hydrogen bonds provides aromatic rings groups formation and the aromatic rings are more hydrophobic them some aliphatic bonds. In addition treating the low hydrogenated content carbon films surface with oxygen plasma for two minutes the hydrophobicity increases. These results show that to produced a-c:H with hydrophobic tendency is necessary increased the c-H bonds and decreasing structural disorder of the film.
3:50 PM E3-1-8 Friction and Wear Behavior of Hydrogenated Amorphous Diamond-Like Carbon (a-C:H) by Reactive Magnetron Sputtering in Water Environment
B. Hilker, H.-R. Stock, M. Diesselberg (Stiftung Institut fuer Werkstofftechnik, Germany)
Amorphous hydrogenated carbon (a-C:H) films are known to have low friction coefficients and high wear resistance. However, the main problems in tribological applications are emerging heat and abrasion. For ecological and economic reasons there is a need to reduce the use of oil-based lubrications. Water lubrication is a promising candidate as an alternative. For this reason the main focus of this work was to improve a-C:H films which show very good tribological characteristics in humid environment. The films were developed with dc pulsed reactive magnetron sputtering (Cemecon CC 800/9). For depositing the films onto polished steel discs we produced a transition layer to improve adhesion by decreasing the voltage of a chromium target, using nitrogen gas flow and increase the voltage of a graphite target. The top a-C:H layer were deposited by sputtering from graphite targets and reactive deposition from acetylene. We examined bias voltage and acetylene flow as well as heating or plasma etching duration before starting the sputtering process and their impact on hardness and average surface roughness of the resulting coatings. One factor that had a major influence on wear was the thickness of the a-C:H films. The optimised a-C:H films had a total thickness of 2 µm and a plastic hardness of 25 Gpa. The tribological properties were investigated by a pin-on-disc test in water. Under an applied load of 20 N the coated samples were slid against 100Cr6 pins and also a-C:H coated 100Cr6 pins. The a-C:H films showed low friction coefficients against a-C:H coated 100Cr6 pins of μ = 0.06. These tribological tests illustrate the potential of a-C:H films to effectively reduce friction and wear in humid environment.
4:10 PM E3-1-9 Water Adsorption on Phosphorus Carbide Thin Films
E. Broitman (Carnegie Mellon University); A Furlan, G.K. Gueorguiev (IFM, Linköping University, Sweden); Zs Czigány (Research Institute for Technical Physics and Materials Science, Hungary); A.M. Tarditi (Universidad Nacional del Litoral, Argentina); A.J. Gellman (Carnegie Mellon University); S. Stafström (IFM, Linköping University, Sweden); L. Hultman (Linköping University, Sweden)

Amorphous phosphorus doped carbon (CxPy) thin films have been considered as a new tribological coating material with unique electrical properties. However, the material could not find practical applications so far since CxPy rapidly oxidizes, hydrolyzes, and delaminates when in contact with air. Recently, we demonstrated that phosphorus carbide (CPx , x≤0.15) thin solid films with a short range fullerene-like structure can be deposited by magnetron sputtering. Thus, the introduction of P atoms in the graphene structure induces the formation of bent and interlinked graphene planes1,2. In this work we compare the uptake of water of amorphous phosphorus-carbide (a-CPx) films, with fullerene-like phosphorus-carbide (FL-CPx) and amorphous carbon (a-C) films. Films with thickness in the range 100-300 nm were deposited onto silicon, quartz, and gallium orthophosphate substrates by reactive DC magnetron sputtering. The film mi crostructure was characterized by X-ray photoelectron spectroscopy, and transmission electron microscopy and diffraction. A piezoelectric crystal microbalance placed in a vacuum chamber was used to measure film water adsorption3. Results indicate that the amount of adsorbed water is highest for the pure a-C films and that the FL-CPx films adsorbed less water than a-CPx. To provide additional insight into the atomic structure of defects in the FL-CPx, a-CPx, and a-C compounds, we performed first-principles calculations within the framework of Density Functional Theory. Emphasis was put on the energy cost for formation of vacancy defects and dangling bonds in relaxed systems3. Cohesive energy comparison reveals that the energy cost for formation for dangling bonds in different structural configurations is considerable higher in FL-CPx than for the amorphous films. The simulations thus confirm the experimental results that dangling b onds are less likely in FL-CPx than in a-CPx and a-C films.

1A. Furlan, G.K. Gueorguiev, Zs. Czigány, H. Högberg, S. Stafström, and L. Hultman, Phys. Stat. Solidi RRL 2 (2008) 191.

2G. K. Gueorguiev, A. Furlan, H. Högberg, S. Stafström, and, L. Hultman, Chem. Phys. Lett. 426 (2006) 374.

3E. Broitman, G. K. Gueorguiev, A. Furlan, N. T. Son, A.J. Gellman, S. Stafström, and L. Hultman, Thin Solid Films, in press (2008).

4:30 PM E3-1-10 Measured and Simulated Wear and Friction Maps of DLCH20% and DLCH35% Films
P.A. Radi (INPE - Instituto Nacional de Pesquisas Espaciais, Brazil); L.V Santos (INPE - Instituto Nacional de Pesquisas Espaciais and Instituto Technologico da Aeronautica - ITA, Brazil); M.C.M Farias (Laboratório de Fenômenos de Superfície (LFS) Escola Politécnica/USP, Brazil); L.F. Bonetti (INPE - National Institute for Space Research, Brazil); V.J. Trava-Airoldi (INPE - Instituto Nacional de Pesquisas Espaciais, Brazil)
DLC (Diamond-Like Carbon) films exhibit unique mechanical and tribological properties and have applications on terrestrial and spatial environments. Depending on the hydrogen concentration on the DLC films and on the environment they can present high or low friction coefficient and wear rates. In this paper experimental results were extended to construct simulated wear and friction maps as a function of load and sliding speed in air and in vacuum to show the films behavior in different conditions as well as its potential for industrial and space application. Friction coefficient and wear rate of DLC films with 20% and 35% hydrogen content (DLCH20% and DLCH35%) produced under strictly controlled growth conditions on titanium alloy (Ti6Al4V) substrate were used to construct such maps. Additionally, the experimental results were used to develop a mathematical modeling of friction and wear of these films in order to identify the parameters that control friction and wear and to obtain the equation that describes these parameters. The techniques required to ensure high adhesion and film reproducibility are in the methodology. Hardness was measured and was considered as an additional reference in terms of DLC films quality. All tests were carried out at different loads and speeds. The results show the relationship between the DLC composition and the environment on the friction coefficient and wear of these films.
4:50 PM E3-1-11 Synthesis and Characterization of Nanocomposite and Nanolaminate Multilayers by High-Power Ion Beam Ablation*
T.J. Renk, T.E. Buchheit, S. Prasad (Sandia National Laboratories)

The Repetitive High Energy Pulse Power (RHEEP) facility at Sandia National Laboratories was used to generate ion-beams of 10 J/cm2 energy. Ablating targets with the high energy ion-beams makes this facility a unique tool for low-stress multilayer thin film deposition. In the first part of this study, Mo-based films were grown on Si wafers, while keeping the substrate at 300°C during the deposition process with the intent of investigating MoS2 films with improved tribological characteristics. Friction and wear measurements were performed using a Si3N4 ball in dry nitrogen and air with 50% relative humidity. Characterization of the films was performed on cross-sections of wear scars suitable for TEM analyses prepared using focused ion beam (FIB) microscopy. Results showed that dual target ablation of MoS2 and Ti or V onto heated substrates permitted self-assembly of Mo species into 50 nm size boulders in the film structure. Consequen tly, unlike pure MoS2 which oxidizes in humid air, the nanocomposites exhibited extremely low wear even when tested in air with 50%RH. Thus, we demonstrated that the nanostructure comprising of relatively hard particles of Mo metal in a matrix of softer MoS2 provided a low friction and highly wear-resistant film that is also resistant to moisture.

By ablating different multiple metal targets, the RHEEP facility also demonstrated the capability for synthesizing a wide range of metal nanolaminate films, providing opportunities to understand fundamental mechanisms driving strength, stiffness and wear characteristics of this category of films. The metal laminate systems we investigated include Mo-Ir, Mo-Ti, and Mo-W. In these cases, nanolaminate films consisted of at least 100 alternating material layers, each layer less than 10 nm thick. Films were deposited on Silicon and Al2O3 substrates. The mechanical response of these nanolaminates was in vestigated using instrumented indentation. The role of layer thickness and shear modulus difference on the strength and wear characteristics of the nanolaminate films will be discussed.

1Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy’s National Nuclear Security Administration under Contract DE-AC04-94AL85000.

5:10 PM E3-1-12 Wear-Resistant and Low-Friction Diamond-Like-Carbon (DLC)-Layers for the Wood Machining Industry
W. Tillmann (Technische Univeristaet Dortmund, Germany); E. Vogli, F. Hoffmann (Technische Universitaet Dortmund, Germany)
Forestry, timber-, and paper-industry in Europe have a production value of approximately 400 billion Euros per year. For this reason, the supplying industry is very conscious to develop highly efficient tools. Especially wear and high friction of cutting tools are limiting factors in the processing of wood and wood-based products. Excellent wear and friction properties increase the tool life just as affecting the power consumption, the surface finish of the workpiece and the production rate in a positive way. To facilitate higher productivity at lower operating cost, it is of particular importance to use tools with enhanced wear and friction attributes. Novel amorphous diamond-like-carbon (DLC) coated tools provide these properties in dry and even in humid environment. This work is focused on the development of a DLC-system with high wear and friction resistance also under humid conditions which especially exist during the processing of wood and wood-based products. Usi ng the Physical Vapor Deposition (PVD)-process different DLC-coating systems have been deposited, in which the layer properties have been designed related to the humidity conditions. Wooden counterparts were used during wear and friction tests to analyse the tribological behaviour of the coatings. Furthermore Raman spectroscopy was applied to characterize the layers microstructure. The layer properties and coating parameters have been systematically analyzed with special emphasis on tribological attributes. Correlations between layer structure and corresponding wear and friction properties have been scrutinized.
Time Period ThA Sessions | Abstract Timeline | Topic E Sessions | Time Periods | Topics | ICMCTF2009 Schedule