Micro-scale abrasive wear testing of PVD coatings on curved substrates

A method is presented which enables a micro-scale abrasion test to be used to measure the wear performance of a coating over a small region, typically of millimetre dimensions, on a curved surface. The method is also applicable to studies of the wear resistance of any bulk material with a surface having complex curvature. The technique is illustrated by measurement of the intrinsic abrasion resistance of thin PVD coatings of TiZrN, ZrNbN and TiNbN on both flat and cylindrical tool steel and flat stainless steel substrates. The ability to measure the wear resistance of both a coating and its substrate, independently of each other and by a single test, is confirmed by experiment.     

Surface fatigue behaviour mapping of PVD coatings for mechanical purposes

Most mechanical components used for transmission of movement are subjected to repeated impacts or cyclic stress. If these elements are well designed and the materials well chosen, their durability is linked to surface fatigue mechanisms. In order to improve the fatigue behaviour of these parts, hard coatings, such as physical vapour deposition (PVD) or plasma‐assisted chemical vapour deposition (PACVD) coatings, can be appropriate. Unfortunately, such hard coatings cannot be used for elements whose replacement is more difficult than, say, cutting tools. An understanding of failure mechanisms should make it possible to optimise the fatigue behaviour of hard coatings. In order to study the surface fatigue behaviour of thin, hard PVD coatings, a special apparatus has been developed to carry out repeated impacts over a broad range of speeds. The possibility of mapping the fatigue behaviour of different coatings is illustrated through the examples of TiN and TiN/CrN multilayer coatings of different thicknesses deposited on several substrates.     

A method for the tribological testing of thin,hard coatings

A new method has been developed for tribological testing of thin, hard antiwear coatings, using a ball‐on‐disc tribosystem, under conditions of dry sliding. In this, an Al₂O₃ ball is pressed against a coated steel disc. Wear debris is removed from the contact zone by a stream of dry argon in this novel method. This improves the stability of the tribological properties and the repeatability of the test results. All test conditions are precisely defined, in particular: the type of motion, air relative humidity, ambient temperature, sliding speed, load, tribosystem spatial configuration, substrate material, substrate hardness and roughness, and coating thickness. The method developed has been used to test various physical vapour deposition coatings (deposited by the vacuum arc method), i. e., single‐layer TiN, Ti(C,N), CrN, and Cr(C,N), and multilayer Cr(C,N)/CrN/Cr and Cr(C,N)/(CrN+Cr₂N)/CrN/Cr. It is shown that CrN coatings exhibit the best antiwear properties, and Ti(C,N) the worst. Friction coefficients for CrN and Cr(C,N) coatings are much lower than for the more commonly used TiN. Multilayer coatings have better antiwear properties than single‐layer ones.     

Corrosion-wear behaviour of PVD Cr/CrN multilayer coatings for gear applications

At present, one of the most important problems in automobile engines and transmission components is due to tribological processes (friction and wear) that in many cases come accompanied by corrosion processes due to the environmental conditions to which these materials are exposed during their lifetime. Both mechanisms can be minimized by means of the development and the application of adequate coatings that combine low friction with a high corrosion and wear resistance.The new tendencies in industrial PVD coatings to improve their properties are focused in the development of new multilayer and nanostructured coatings. These structures allow in a relatively simple way enhancing their tribological properties and the corrosion resistance that can not be reached by means of the traditional monolayer coatings. The background of this type of coatings consists of the stacking up of several layers with good individual tribological and mechanical properties, but every individual layer has a thickness that can be from hundreds of nanometres down to only 5-10 nm. The properties of these nanostructured coatings depend strongly on the thickness modulation of every individual layer.Concerning PVD coatings, the chrome nitride coatings have demonstrated to possess excellent wear resistance properties. In this work, multilayer Cr/CrN coatings with different individual layer thickness have been deposited on substrates of steel F1272 and silicon. The deposition has been carried out by means of the cathodic arc method alternating an atmosphere of pure Ar with a reactive mixture of N₂/Ar. The multilayers obtained have been analyzed by means of Glow Discharge Optical Emission Spectroscopy (GD-OES) and in some cases by means of FE-SEM obtaining bilayer (Cr/CrN) periods of the order of 220 and 45 nm. The coating characterization has been complemented with hardness and composition measurements as well as by the performance of several wear and corrosion-wear tests.     

含Mo的PVD涂层结构及其摩擦学特性的研究进展

从含Mo元素的代表性涂层入手,综述了二元、三元再到多元含Mo系列PVD涂层的研究现状和进展,探究了不同元素添加、不同制备参数等对涂层微观结构、力学性能和摩擦学性能等的影响。在涂层组分从二元发展到多元的过程中,改变掺杂元素种类、含量,制备参数会引起涂层微观结构的变化进而提升涂层力学性能和摩擦学性能。涂层性能的改善,有利于增强对机械设备中关键传动零部件的保护,延长机械设备使用寿命,对军工及社会发展具有重大意义。     

Tribological testing of some potential PVD and CVD coatings for steel wire drawing dies

The aim of this study was to investigate the possibility to replace cemented carbide wire drawing dies with CVD or PVD coated steel dies. Material pick-up tendency, friction and wear characteristics of four different commercial coatings – CVD TiC and PVD (Ti,Al)N, CrN and CrC/C – in sliding contact with ASTM 52100 bearing steel were evaluated using pin-on-disc testing. The load bearing capacity of the coating/substrate composites was evaluated using scratch testing. The results show that the friction characteristics and material pick-up tendency of the coatings to a large extent is controlled by the surface topography of the as-deposited coatings which should be improved by a polishing post-treatment in order to obtain a smooth surface. Based on the results obtained in this study, three different coatings – CrC/C, TiC and dual-layer TiC/CrC/C – are recommended to be evaluated in wire drawing field tests. CrC/C and TiC are recommended due to their intrinsic low friction properties and material pick-up tendency in sliding contact with steel. The dual-layer is recommended in order to combine the good properties of the two coatings CrC/C (low shear strength) and TiC (high hardness).     

Comparative tribological behaviors of TiN, CrN and MoNCu nanocomposite coatings

The purpose of this study is to investigate comparative tribological behaviors of Cu-doped TiN, CrN, and MoN coatings under a wide range of dry sliding conditions. TiN and CrN coatings have been developed and used by industry in numerous tribological applications including, machining, manufacturing and transportation. In contrast, MoN has attracted very little attention as a tribological coating in the past, despite being much harder than both TiN and CrN. In this paper, we will mainly concentrate on the Cu-doped versions of these coatings whose tribological properties have not yet been fully explored. The results of this study have confirmed that the addition of Cu into TiN, CrN and MoN coatings has indeed modified the grain size and morphology, but had a beneficial effect only on the friction and wear behavior of MoN. The tribological behavior of CrN did not change much with the addition of Cu but that of TiN became worse after Cu additions. Raman spectroscopy technique was used to elucidate the structural and chemical natures of the oxide films forming on sliding surfaces of Cu-doped TiN, CrN and MoN films. The differences in the friction and wear behavior of Cu-doped TiN, CrN, and MoN is fully considered and a mechanistic explanation has been provided using the principles of a crystal chemical model that can relate the lubricity of complex oxides to their ionic potentials.     

Functional behaviour of PVD coatings under sliding and rolling stress conditions

Whereas wear-resistant PVD coatings are well established in the field of metalcutting, and the functional and tribological behaviour of these coatings is well known under such conditions, PVD coatings are used only occasionally in mechanical engineering. The reason for this seems to be the lack of information concerning the functional behaviour of these coatings in closed tribosystems. To evaluate new areas of application together with optimised coating compounds, model wear tests were performed under sliding, rolling and slip-rolling stress conditions. In addition, the test parameters, such as sliding speed, load, ambient temperature, and number of revolutions were varied, as were the coating compounds and their thicknesses. The results obtained show that friction and wear of PVD coatings are both strongly influenced by the kind of stress and the test parameters themselves. Coatings that perform well under certain test conditions can break down quickly under some other stress conditions. TiN coatings, for example, which display low friction and wear under sliding friction, fail under rolling conditions very shortly afterwards.     

Tribological behaviour of W‐alloyed carbon‐based coatings in dry and lubricated sliding contact

Carbon‐based coatings with different W contents were deposited by direct current magnetron sputtering in reactive and non‐reactive atmospheres. All deposited coatings have compact morphologies with amorphous (tungsten‐free) or nanocrystalline structures (tungsten‐doped). The latter one was indicated by very broad peaks in X‐ray Diffraction spectra in the position of tungsten carbide suggesting W‐carbide nanoparticles embedded in an amorphous carbon matrix. The hardness increased from 10 to 15 GPa with increasing W content. The coatings were tribological tested at dry and lubricated conditions with increasing temperature in a coating/steel configuration. In dry sliding, the friction coefficient increases with the increase of the temperature reaching values higher than 1.0. The friction is significantly lower in lubricated contact using three different oils: poly‐alpha‐olefin, paraffin and olive oil. The olive oil shows promising lubricating properties at the temperature lower than 70°C; however, at higher temperature, the coatings were quickly worn through. Copyright © 2014 John Wiley & Sons, Ltd.     

Surface performances of PVD ZrN coatings in biological environments

Zirconium nitride (ZrN) thin films were deposited by reactive RF magnetron sputtering on Ti-6Al-4V and Si (100) substrates for potential use in biomedical applications. The tribological behaviour was evaluated against bovine bone in dry condition using a pin-on-disc apparatus. Abrasion is the primary wear mechanism observed in ZrN/bone contact. The corrosion properties were determined through two electrochemical techniques: potentiodynamic polarization and electrochemical impedance spectroscopy. The coatings with reduced oxygen content provided: (i) good resistance against corrosion when exposed to physiological solution and (ii) better anti-bioadhesion against Staphylococcus aureus bacteria.     

An overview of the potential of quantitative coating adhesion measurement by scratch testing

The scratch test has been used to assess the adhesion of thin hard coatings for some time now and is a useful tool for coating development or quality assurance. However, the test is influenced by a number of intrinsic and extrinsic factors which are not adhesion-related and the results of the test are usually regarded as only semi-quantitative. The stress state around a moving indenter scratching a coating/substrate system is very complex and it is difficult to determine the stresses which lead to detachment. Furthermore, the interfacial defect state responsible for failure is unknown. However, by a careful analysis of the observed failure modes in the scratch test (not all of which are related to adhesion) it is possible to identify adhesive failures and in some cases these occur in regions where the stress state is relatively simple and quantification can be attempted.Ideally engineers would like a material parameter (such as work of adhesion or interfacial toughness) which can be used in an appropriate model of the coating-substrate system stress state to determine if detachment will occur under the loading conditions experienced in service. This data is not usually available and the development of such models must be seen as a long-term goal. In modern indentation and scratch systems the work of friction (or indentation) can be directly measured and the relationship between this parameter and adhesive failure can be demonstrated in some cases. This paper reviews the main adhesion-related failure modes and the stresses responsible for them and indicates where quantification is possible illustrating this with results from hard coatings on steel, thermally grown oxide scales and optical coatings on glass. The use of empirical calibration studies, directly measured work of friction and quantification by finite element methods is discussed.     

Two-body abrasive wear of electroless nickel composite coatings

The two-body abrasive wear of electroless nickel (EN), EN-silicon carbide, and EN-alumina composite coatings have been investigated using a scratch test with a diamond indenter. The coatings were heat treated at temperatures of 100–500° C. The hardness of the coatings increased with heat treatment temperature from 500 HV100 for the as-deposited condition to 1008 HV100 when fully hardened. Scratch testing showed that the as-deposited coating had scratch tracks with a high degree of plasticity, signs of microploughing and tensile cracking and was characterised as a ductile failure. On the other hand, the heat-treated coatings showed chipping and cracking on the edge of the scratch tracks, failing in a brittle manner. The heat-treated EN-silicon carbide coatings, however, exhibited no cracking nor chipping, believed to be due to its higher fracture toughness than the other heat-treated coatings, attributable to its lower phosphorus content. The volume of material removed from the silicon carbide scratch track was 1/3 of the volume removed from the steel substrate at a 20 N load, and showed the best wear/ scratch resistance of any of the coatings tested.     

Evaluation of wear and tribological properties of coatings rubbing against copper

A new crossed-cylinders tribo-tester is proposed. This tribo-tester can decrease the tendency of the chatter vibration. The tribological properties of coatings against copper is evaluated with this tribo-tester. The wear rate of TiN, TiC and TiCN rubbing against copper is higher than the substrate high speed tool steel: SKH51 (JIS). The catalytic action of copper for oxidation of Ti-based coatings is a main reason of this high wear rate of TiN, TiC and TiCN rubbing against copper. The wear rate of CrN rubbing against copper is in a very low level because CrN shows the excellent oxidation resistance and Cr₂O₃ film formation decreases the wear loss of CrN coating.     

Structure and water-lubricated tribological properties of Cr/a-C coatings with different Cr contents

The Cr containing amorphous carbon coatings (Cr/a-C) with varying Cr content were deposited using unbalanced magnetron sputtering. The results revealed that the chromium carbide nano-clusters were formed when the Cr content exceeded 4.9 at%. The critical load increased while the hardness decreased after the Cr element incorporation. Although the low Cr containing Cr/a-C coatings (≤4.9 at%) exhibited similar friction coefficient with a-C coatings, but the initial friction coefficient, running-in distance and wear rate of SUS440C balls all decreased. However, the Cr/a-C coatings with high Cr content (11.98–14.09 at%) would worsen the tribological properties because chromium carbides acted as abrasive wear particles during tribotests.     

Erosion, corrosion and erosion–corrosion of EB PVD thermal barrier coatings

Electron beam (EB) physical vapour deposited (PVD) thermal barrier coatings (TBCs) have been used in gas turbine engines for a number of years. The primary mode of failure is attributed to oxidation of the bond coat and growth of the thermally grown oxide (TGO), the alumina scale that forms on the bond coat and to which the ceramic top coat adheres. Once the TGO reaches a critical thickness, the TBC tends to spall and expose the underlying substrate to the hot gases. Erosion is commonly accepted as a secondary failure mechanism, which thins the TBC thus reducing its insulation capability and increasing the TGO growth rate. In severe conditions, erosion can completely remove the TBC over time, again resulting in the exposure of the substrate, typically Ni-based superalloys. Since engine efficiency is related to turbine entry temperature (TET), there is a constant driving force to increase this temperature. With this drive for higher TETs comes corrosion problems for the yttria stabilised zirconia (YSZ) ceramic topcoat. YSZ is susceptible to attack from molten calcium–magnesium–alumina–silicates (CMAS) which degrades the YSZ both chemically and micro-structurally. CMAS has a melting point of around 1240 °C and since it is common in atmospheric dust it is easily deposited onto gas turbine blades. If the CMAS then melts and penetrates into the ceramic, the life of the TBC can be significantly reduced. This paper discusses the various failure mechanisms associated with the erosion, corrosion and erosion–corrosion of EB PVD TBCs. The concept of a dimensionless ratio D/d, where D is the contact footprint diameter and d is the column diameter, as a means of determining the erosion mechanism is introduced and discussed for EB PVD TBCs.     

Residual stress measurement in PVD optical coatings by microtopography

Residual stress in optical plasma vapor deposited coatings must be carefully measured. The topographic inspection of the coatings’ surface at microlevel allows the assessment of its residual stress. In the present work we will report on the optical non-destructive and non-invasive microtopographic inspection of WO₃ PVD thin films for residual stress evaluation. The MICROTOP.06.MFC system, an active optical triangulation sensor developed at the Universidade do Minho, was employed. It allows depth resolutions down to 2 nm and lateral resolutions down to 1 μm. The three dimensional coordinate set obtained on the inspection allow the calculation of the stress distribution over the film.     

Comprehensive tribological characterization of thin TiN-based coatings

Innumerable papers have been published so far describing tribological investigations of thin hard coatings based on TiN. Analysis of the presented results demonstrates a large dispersion of measured friction and wear numbers, whereas TiN-coated pieces and tools have proved their benefits in a broad area of application. Therefore an attempt was made to clarify the influences on friction and wear test results by varying the coating process, the tribological stresses due to sliding, fretting and rolling motion and by changing the surrounding medium. The results reveal that machining of substrate surfaces and type of tribological stresses due to sliding, fretting and rolling have an important influence. The formation of reaction layers is dominating the tribological behaviour in most cases.     

Use of ethyl-dimethyl-2-methoxyethylammonium tris(pentafluoroethyl)trifluorophosphate as base oil additive in the lubrication of TiN PVD coating

This paper discusses and compares the use of ethyl-dimethyl-2-methoxyethylammonium tris(pentafluoroethyl)trifluorophosphate ionic liquid [(NEMM)MOE][FAP] and the traditional zinc dialkyldithiophosphate (ZDDP) as 1 wt% additives to a polyalphaolefin (PAO 6) in the lubrication of TiN PVD coating. Tribological tests performed using a ball-on-plate reciprocating tribometer showed how both additives improve the anti-friction and anti-wear behaviors of the base oil for the two loads tested. However, the traditional additive ZDDP showed the lowest friction coefficient in all cases. Interferometry and XPS analyses showed that the formation of tribofilms resulting from the interaction of the ionic liquid with the surface contributed to the tribological improvement.     

The scanning micro-sclerometer: a new method for scratch hardness mapping

A new surface engineering research tool, called a scanning microsclerometer (SMS), has been developed. It uses nano-indentation technology and a piezoelectric transducer positioning system to generate high-precision scratch patterns on the surfaces of metals and, by monitoring the instantaneous displacement of the stylus tip, can generate scratch hardness and scratching force maps of the surface. A dual-stroke process is used. The first stroke at low load profiles the surface to establish a reference datum and the second pass, in the opposite direction and at higher load, produces the indentation scratch. Examples of micro-scratch hardness mapping experiments, using scratch spacings of 1·0 μm, on a silicon carbide-based ceramic composite are used to illustrate the capabilities of the SIVIS. Using end-on fibers in the rectangular stylus scanning area, the difference in scratch hardnesses of the fibers, the matrix, and even the thin carbon coatings in the fiber-matrix interface could be detected. The SMS was originally developed to produce scratch hardness maps, but it is also useful for conducting accurately controlled, single-point micro-machining patterns and in studies of differential material abrasion.     

Analytical models of scratch hardness

The ability of one material to abrade or scratch another has a long history as the basis of a scale of hardness and is clearly related to the now more common measure of hardness as the resistance of a material to indentation. However, there is no simple relation between the values of hardness from these two tests. Producing an abraded groove in the surface of a specimen involves large plastic strains, and a number of analytical models have been proposed for this process based on such techniques as slip line field theory and the theorems of plastic load bounding. While there is reasonable agreement between the predicted and measured values of the loads, these methods are much less satisfactory in providing estimates of the patterns of deformation or strain around the groove and these limitations may be associated with some of the idealizations relatively simple models make about material behaviour — such as isotropy and a neglect of elastic effects. The scratch testing of brittle solids can also involve plastic behaviour facilitated by the high local hydrostatic compressive stresses generated close to the tip of a sharp indenter. Scratch hardness is also finding applications as a test for the integrity of coated substrates, although the modes of failure here may be more complex than those observed in homogeneous materials.