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.     

Investigation of antiwear coatings deposited by the pvd process

The tribological properties of various PVD‐deposited coatings (vacuum arc method) have been tested, both single‐layer coatings (TiN, CrN, Ti(C,N), and Cr(C,N)) and multilayer coatings (Cr(C,N)/CrN/Cr and CR(C,N)/(CrN+Cr₂N)/CrN/Cr). An unlubricated ball‐on‐disc tribosystem was used in which an Al₂O₃ ball is pressed against a coated steel disc rotating in the horizontal plane. A novelty of the method is the removal of wear debris from the contact zone using a draught of dry argon. This improves the repeatability of the test results and the stability of the tribological characteristics. It is shown that CrN coatings exhibit the best antiwear properties and Ti(C,N) the worst. Multilayer coatings have better antiwear properties than single‐layer ones. The friction coefficients for CrN and Cr(C,N) coatings are much smaller than for the commonly used TiN. A correlation has also been found between the physical properties of the coatings tested (adhesion of the coating to the substrate assessed in scratch tests, and coating hardness) and their antiwear properties. An improvement in coating‐substrate adhesion results in wear reduction, while greater hardness (causing a coating embrittlement increase and a change in the wear mechanism) brings about greater wear. There is no correlation between the physical properties and the friction coefficients of the coatings tested.     

Low Friction CrNMPP/TiNDCMS Multilayer Coatings

Transition metal nitrides like CrN and TiN are widely used in automotive applications due to their high hardness and wear resistance. Recently, we showed that a multilayer architecture of CrN and TiN, deposited using the hybrid—high power impulse magnetron sputtering (HIPIMS) and direct current magnetron sputtering (DCMS)—HIPIMS/DCMS deposition technique, results in coatings which indicate not only increased mechanical and tribological properties but also friction coefficients in the range of diamond-like-carbon coatings when tested at RT and ambient air conditions. The modulated pulsed power (MPP) deposition technique was used to replace the HIPIMS powered cathode within this study to allow for a higher deposition rate, which is based on the complex MPP pulse configuration. Our results on MPP/DCMS deposited CrN/TiN multilayer coatings indicate excellent mechanical and tribological properties, comparable to those obtained for HIPIMS/DCMS. Hardness values are around 25 GPa with wear rates in the range of 2 × 10⁻¹⁶ Nm/m³ and a coefficient of friction around 0.05 when preparing a superlattice structure. The low friction values can directly be correlated to the relative humidity in the ambient air during dry sliding testing. A minimum relative humidity of 13% is necessary to guarantee such low friction values, as confirmed by repeated tests, which are even obtained after vacuum annealing to 700 °C. Our results demonstrate that the co-sputtering of high metal ion sputtering techniques and conventional DC sputtering opens a new field of applications for CrN/TiN coatings as high wear resistance and low friction coatings.     

Interlayer thickness influence on the tribological response of bi-layer coatings

The present work deals with the influence of coating thickness on the tribological response of bi-layer model coatings consisting of CrN with Cr interlayer with varying Cr/CrN thickness ratios on high-speed steel. Ball-on-disc experiments were carried out in ambient air at room temperature and alumina balls as counterbodies. The mechanical stresses in both layers generated during the tests were calculated with the software package Elastica. Wear tracks on the samples were characterised using both scanning electron microscopy and optical profilometry. The results show that the interlayer thickness plays a determinant role in the tribological response of the coatings provided that the CrN layer thickness exceeds a critical value to withstand mechanical wear.     

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.     

Multilayer thin film CrN coating on aerospace AL7075-T6 alloy for surface integrity enhancement

Chromium nitride (CrN) coating has emerged as a new alternative in machining applications. CrN has good thermal stability, low deposition temperature, and excellent wear and corrosion resistance. However, no precise information exists yet regarding the ideal coating parameter conditions that lead to higher surface integrity. For this reason, an optimization study is desired—a study on the parameters of CrN coating on aerospace Al7075-T6 alloy using physical vapor deposition magnetron sputtering. The present research work investigates the effects of temperature as well as nitrogen flow rate and DC power on coated samples’ surface hardness, adhesion, surface roughness, and microstructure. To carry out the investigation, the Taguchi optimization method with L₁₆ (3⁴) orthogonal array was applied. However, to obtain optimum parameters for superior surface integrity, signal/noise (S/N) response analysis method was employed. Finally, confirmation tests with the best parameter combinations attained in the optimization process were carried out to demonstrate the progress made. Ultimately, surface hardness of coated Al7075-T6 was enhanced by 15.33 %, adhesion by 24.3 %, and surface roughness by 7.22 %.     

Architecture of Multilayer Cr/CrN Coatings for Wear Protection in Seawater: Cr/CrN Ratio and Total Thickness

Cr/CrN multilayer coatings with various Cr/CrN thickness ratios and total thicknesses were deposited on 316L stainless steel by multi-arc ion plating. The coatings were systematically characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), and nanoindentation. Tribological behaviors were investigated using a ball-on-disk tribometer in artificial seawater. The results showed that the multilayer coating phases changed from Cr₂N + CrN to Cr + Cr₂N + CrN phases with an increase in Cr/CrN thickness ratio. The adhesion showed a slight difference for the coatings with different thickness ratios but significantly increased with total thickness. The hardness was also slightly improved by thickening the coatings. The friction coefficient and wear rate were lowest at a thickness ratio of about 0.3. However, there was no large difference in the friction coefficient between coatings with different thicknesses. The wear rate was lower for the thicker coatings under various loads. The load-bearing capacity was also improved by thickening the coatings.     

Friction and wear properties of duplex MAO/CrN coatings sliding against Si3N4 ceramic balls in air, water and oil

It is evident that the micro-arc oxidation (MAO) ceramic coatings often exhibit relatively high friction coefficients as sliding against many mating materials. To reduce the friction coefficient for the MAO coatings, the duplex MAO/CrN coatings were deposited on 2024Al alloy using combined micro-arc oxidation and reactive radio frequency magnetron sputtering. The microstructure and phase of the duplex coatings were observed and determined using scanning electron microscope (SEM) and X-ray diffraction (XRD), respectively. The friction and wear behaviors of the duplex coatings sliding against Si₃N₄ balls in air, water and oil were investigated using a ball-on-disk tribometer. The wear rate of the duplex coating was determined by non-contact optical profilometer and the wear tracks on the duplex coatings were observed by SEM. The results showed the CrN coatings mainly consisted of Cr, CrN and Cr₂N phases. The duplex coatings/Si₃N₄ tribopair exhibited the highest friction coefficient in air, while displayed the lowest friction coefficient in oil. When the normal load and the sliding speed increased, the friction coefficient in air increased from 0.65 to 0.72, whereas decreased from 0.58 to 0.36 in water and 0.20 to 0.08 in oil. The specific wear rates for the duplex coatings in air were higher than those in oil. In comparison to the MAO coatings, the duplex MAO/CrN coatings displayed excellent tribological properties under the same conditions.     

Formation of nanostructured TiAlN,TiCrN, and TiSiN coatings using reactive magnetron sputtering

The effect of the additive of the third element (Al, Cr or Si) to titanium nitride coatings deposited using reactive magnetron sputtering on their hardness and tribological behavior is studied. The regularities of the formation of the coatings, as well as the influence of conditions of deposition on their final composition and characteristics, are considered; recommendations on producing the TiN-based coatings with the enhanced performance characteristics are given. The tribotests of these coatings are performed and discussed. When using the aluminum additive and keeping optimum conditions of deposition, the effect of enhancing the performance characteristics of the TiN coating is observed.     

Optical Detections From Worn and Unworn Titanium Compound Surfaces

Wear-induced roughness in terms of grooves, sharp ridges, and edges leads to scattering of the reflected light and leads unavoidably to a reduction of the optical signals in a standard specular geometry. However, by using a double-layer system consisting of titanium aluminum nitride (TiAlN) on top of a titanium nitride (TiN) layer we obtain an increase in the reflected light as a result of wear. The relative change of reflectance of light from the tribological TiAlN coated surface to the underlying layer of TiN is similar for non-worn surfaces and for surfaces exposed to an abrasive wear process. The induced roughness reduces the signals from worn samples, in a standard specular geometry, by up to 30% compared with unworn samples. Our model system of TiAlN coatings on top of ‘optical’ signal layers of TiN deposited on a 100Cr6 steel substrate, was exposed to a reciprocating wear process with up to 10⁵ repetitive cycles in a linear tribometer. The worn TiAlN layers of thicknesses up to 3 μm, with strongly developed grooves and ridges, were subsequently used for the reflectance measurements. The results show that optical reflectance monitoring is a potential technique for intelligent determination of a residual thickness of realistic tribological coatings prior to complete wear.     

Tribological and electrochemical performances of Cr/CrN and Cr/CrN/CrAlN multilayer coatings deposited by RF magnetron sputtering

CrN/CrAlN and Cr/CrN/CrAlN multilayers were grown with dual RF magnetron sputtering. The application of these multilayers will be wood machining of green wood. That is why ball-on-disc and electrochemical tests in NaCl aqueous solution were realized to elucidate the tribological and corrosion behavior of these coatings as they will be exposed to wear and corrosion during wood machining process. The samples/alumina and samples/WC coupling showed different wear mechanisms. The 300 nm thick Cr/CrN/CrAlN multilayer demonstrated the best tribological behavior and corrosion resistance. The influence of growth defects on corrosion resistance has been shown.     

Study of wear resistance of thermal-diffusion boron nitride coatings on titanium

The wear resistance of commercially pure titanium VT1-0 covered with boron nitride coatings in pair with steel U8 is studied. It is found that the boron nitride coatings deposited from amorphous boron by thermal-diffusion saturation in molecular nitrogen at temperatures of 800?C850°C using the noncontact method improve the wear resistance of titanium during boundary sliding friction. Their characteristics are compared with those of boride coatings on titanium deposited by the same method. It is shown that the high-gradient strengthened layers formed during contact thermal-diffusion boronitriding within the 900?C950°C temperature range affect adversely the tribological performance of the boron nitride coating-steel pair.     

Wear behaviour of flame sprayed NiCrBSi coating remelted by flame or by laser

Flame spray coatings are widely used in industry because of low cost and process simplicity. However, high porosity and poor adherence to the substrate means that quality is poor, though it can nevertheless be improved by subjecting coatings to a remelting using a technique that usually involves an oxyacetylene flame. The study that follows is an attempt to evaluate a laser technique as an alternative to the more traditional flame remelting of flame spray layers, using grey cast iron (DIN GG30) as the substrate and a NiCrBSi alloy as the coating material. Coatings obtained by laser remelting exhibited a practically pore-free microstructure with good adherence to the substrate. The limited control of process parameters during flame remelting led in some cases to incomplete melting of the full thickness of the layers. Hardness of the remelted coatings was very similar in both cases, with values that were slightly lower than for flame-spray layers. The tribological behaviour of both coating types was then compared in dry sliding wear tests (block-on-ring tests) at various loads (30–100 N) and sliding speeds (0.65–2.62 m/s). Both coatings wear rates and wear rate coefficients k (mm³/Nm) were calculated. No significant differences in wear performance between the two coatings were found. A severe wear regime with adhesion as the principal component was observed at the higher test loads. The predominant wear mechanism at the lower test velocities was oxidation.     

Cr2N/CrN multilayer coatings for wood machining tools

The present paper describes results from a recent research project aimed at forming a wear resistant coating based on chromium on tools to wood machining. Cr₂N/CrN multilayer coatings deposited on HS6-5-2 steel substrates using cathodic arc evaporation were tested. These coatings were formed from 7 bilayers being ca. 340 nm thick and equally thick Cr₂N and CrN layers. For comparison, Cr₂N and CrN monolayer coatings were also prepared. Hardness measurements, indentation and scratch tests, friction and wear were performed to characterize the mechanical properties. The wear tracks and Rockwell indentations enable to assess wear mechanisms of the coatings. The results of the Cr₂N/CrN coatings investigated show high hardness: ca. about 22 GPa and a critical force being higher than 95 N and a low wear rate.The industrial tests of planer knives with Cr₂N/CrN multilayer coatings were carried out on a down-spindle milling machine to determine the durability of tools with wear resistant coatings for woodworking. These tools show increase of “life time” two times. Another positive feature of the use of such tools is the increase of the quality of wood surface machined when compared with uncoated tools.     

沉积参数对磁控溅射CrN_x膜结构和性能的影响

本文采用非平衡直流磁控溅射方法制备CrN_x薄膜,研究沉积参数对膜结构和性能的影响。结果表明沉积过程中增加N_2的分压,薄膜的组成由Cr_2N相转变成CrN相,膜的表面形貌也由胞状转化为正四面体。增加样品台的负偏压,沉积膜层更加致密,表面更加平坦。     

Fretting fatigue life evaluation of multilayer Cr–CrN-coated Al7075-T6 with higher adhesion strength—fuzzy logic approach

In this research work, an experimental evaluation was conducted to explore the fretting fatigue life of multilayer Cr–CrN-coated AL7075-T6 alloy specimens with higher adhesion strength to substrate as the coating adhesion strength is one of the most critical issues in magnetron sputtering technique. Physical vapor deposition (PVD) magnetron sputtering technique was used for coating purpose, and a fuzzy rule-based system was established to investigate how to achieve higher adhesion of Cr–CrN coating on AL7075-T6 with respect to changes in input process parameters, direct current power, nitrogen flow rate, and temperature. Close assent was obtained between the experimental results and fuzzy model predicted values. Experimental result analysis was performed with Pareto–ANOVA variance as an alternative analysis. The fretting fatigue lives of coated AL7075-T6 alloy were improved 70 % and 22 % at high and low cyclic fatigue, respectively, compared with uncoated specimens.     

Substrate Effects on the Micro/Nanomechanical Properties of TiN Coatings

Nanoindentation and nanoscratch tests were performed for titanium nitride (TiN) coatings on different tool steel substrates to investigate the indentation/scratch induced deformation behavior of the coatings and the adhesion of the coating–substrate interfaces and their tribological property. In this work, TiN coatings with a thickness of about 500 nm were grown on GT35, 9Cr18 and 40CrNiMo steels using vacuum magnetic-filtering arc plasma deposition. In the nanoindentation tests, the hardness and modulus curves for TiN/GT35 reduced the slowest around the film thickness 500 nm with the increase of indentation depth, followed by TiN/9Cr18 and TiN/40CrNiMo. Improving adhesion properties of coating and substrate can decrease the differences of internal stress field. The scratch tests showed that the scratch response was controlled by plastic deformation in the substrate. The substrate plays an important role in determining the mechanical properties and wear resistance of such coatings. TiN/GT35 exhibited the best load-carrying capacity and scratch/wear resistance. As a consequence, GT35 is the best substrate for TiN coatings of the substrate materials tested.     

Structural and tribological characterization of tungsten nitride coatings at elevated temperature

Transition metal nitrides exhibit excellent mechanical properties (hardness and Young's modulus), high melting point, good chemical stability and high electrical conductivity. However, tungsten nitrides still stand aside of the main attention. In our previous study, tungsten nitride coatings with different nitrogen content showed excellent wear resistance at room temperature. Nevertheless, many engineering applications require good tribological properties at elevated temperature. Thus, the present study is focused on the tribological behaviour (friction coefficient and wear rate) of tungsten nitride coatings at temperature up to 600 °C.

The structure, hardness, friction and wear of tungsten nitride coatings with nitrogen content in the range 30–58 at.% prepared by dc reactive magnetron sputtering were investigated. The tribological tests were performed on a pin-on-disc tribometer in terrestrial atmosphere with Al₂O₃ balls as sliding partner. The coating wear rate was negligible up to 200 °C exhibiting a decreasing tendency; however, the wear dramatically increased at higher temperatures. The coating peeled off after the test at 600 °C, which is connected with the oxidation of the coating.     

Effects of sliding velocity and normal load on friction and wear characteristics of multi-layered diamond-like carbon (DLC) coating prepared by reactive sputtering

Friction and wear tests were performed to investigate effects of sliding velocity and normal load on tribological characteristics of a multi-layered diamond-like carbon (DLC) coating for machine elements. The DLC coatings which consist of sequentially deposited gradient Cr/CrN, W-doped DLC (a-C:H:W) and DLC (a-C:H) layers were formed on carburized SCM 415 Cr–Mo steel disks using a reactive sputtering system. The tests against AISI 52100 steel balls were performed under various sliding velocities (0.0625, 0.125, 0.25, 0.5, 1 and 2 m/s) and normal loads (6.1, 20.7 and 49.0 N) in ambient air (relative humidity=26±2%, temperature=18±2 °C). Each test was conducted for 20 km sliding distance without lubricating oil. The results show that friction coefficients decrease with the increase in sliding velocity and normal load. Wear rates of both surfaces decrease with the increase in normal load. The increase in sliding velocity leads initially to the increase in wear rates up to the maximum value. Then, they decrease, as the sliding velocity increases above specific value that corresponds to the maximum wear rate. Through surface observation and analysis, it is confirmed that formation of transfer layers and graphitized degree of wear surfaces of DLC coatings mainly affect its tribological characteristics.     

Influence of layer thickness on hardness and scratch resistance of Si-DLC/CrN coatings

Abstract

Multifunctional coatings, widely used in tribological applications, have their properties strongly influenced by the interaction of the system coating/substrate. The use of multilayered coatings has been pointed out as a solution for the problem of high internal stresses that can be generated in coated systems, in particular in the case of soft substrates. In multilayered coatings, a decrease in the stress gradient between substrate and coating improves adhesion. Moreover, the thickness of the coating has shown a strong influence on the tribological behaviour of the coated system. This paper, through widely used and efficient techniques, seeks to assess the influence of the thickness of different layers (DLC and CrN) on the response of a multifunctional coating. Si rich DLC and CrN coatings with different thicknesses were deposited on a steel substrate (AISI 1020) by Plasma Enhanced Magnetron Sputtering (PECVD). Scanning electron microscopy (SEM) and Raman spectroscopy (RS) were used in order to characterize the chemical composition and microstructure of the coatings. Instrumented indentation and scratch test techniques were used to measure hardness, elastic modulus, and adhesion of each layer. Critical loads were determined by visual analysis, using SEM in conjunction with the curves obtained in the scratch tests. The evaluation of the effect of the thicknesses of the layers allowed an optimised design of the multifunctional coated systems with improved durability.