Optimization of the mechanical properties of magnetron sputtered diamond-like carbon coatings

Diamond-like carbon coatings containing hydrogen, a-C:H, were deposited by use of reactive DC magnetron sputtering with an industrial deposition system. The reactive gas C₂H₂ was used in combination with carbon targets. Using Raman spectroscopy, nanoindentation and Rockwell C indentation, the mechanical properties of the coatings were optimized. Excessively high compressive stresses, which were measured with Raman spectroscopy, were found in the coatings with high hardness, resulting in poor adhesion to the substrates. By thermal annealing, these compressive stresses were reduced without altering the hardness, resulting in diamond-like carbon coatings with good adhesion.     

Adhesion and fatigue resistance of Ta-doped MoS2 composite coatings deposited with pulsed-DC magnetron sputtering

MoS₂–Ta composite coatings were deposited using the pulsed-DC magnetron sputtering technique. X-ray diffraction (XRD), scanning electron microscopy, energy dispersive spectroscopy, and atomic force microscopy were used to determine the structural properties of the MoS₂–Ta composite coatings. The hardness values and adhesion and fatigue features of the coatings were determined using a microindentation hardness test and a scratch test, respectively. The scratch tests were evaluated using two modes: a standard mode (under a progressive load) and a multimode (sliding-fatigue with a constant sub-critical load within the same scratch track). Failure mechanisms of the scratch tracks were determined by examining the resulting micrographs. The MoS₂–Ta coatings have a dense columnar microstructure. XRD patterns of the coatings revealed MoS₂ (0?0?2), MoS₂ (1?0?0), MoS₂ (1?0?3), and α-Ta (1?1?0) reflections. The thickness, roughness, hardness, and elemental ratio values of the coatings were significantly affected by the target currents. The adhesion of the coatings dramatically increased with an increase in the thickness, hardness, and Ta/Mo ratio and with decreases in the roughness. The MoS₂–Ta composite coatings with a high load-bearing capacity exhibited excellent fatigue resistance.     

Scratch and wear resistance of hydrophobic CeO2-x coatings synthesized by reactive magnetron sputtering

CeO_2-x coatings were deposited under variable oxygen flow ratios (%f_O2) onto Si substrates by reactive magnetron sputtering. Nanoindentation testing revealed an increase in the hardness, elastic modulus, H/E and H³/E² ratio with increasing oxygen flow ratio, which in turn increased the adhesion and tribological performance of the coatings. Scratch testing yielded the highest critical load (L_C2 = 28.8 N) and CPR_S = 103 for the coating deposited with the highest oxygen flow ratio (57 %f_O2). Cracking events during scratch testing were initiated by tensile forces behind the scratch stylus, which led to the formation of semi-circular ring cracks. As the normal load increased, transverse cracks emerged extending outwards from the scratch track towards the edge causing the exposure of substrate. Beyond L_C2, severe spallation of the CeO_2-x coatings led to coating failure. Furthermore, the specific wear rates of the CeO_2-x coatings were determined to be within the ~10⁻¹⁵ m³/Nm range influenced by three-body abrasive wear. In-depth analyses from scratch and wear data indicates that these coatings possess good adhesion and durability.     

Investigation of the adhesion of NbN coatings deposited by pulsed dc reactive magnetron sputtering using scratch tests

Scratch tests have been used to investigate the adhesion of niobium nitride (NbN) coatings that were deposited by pulsed dc reactive magnetron sputtering at target currents of 1.5, 2.5, and 3.5 A onto M2 tool steel and silicon wafer. The coating adhesion on each material substrate was investigated using a progressive load scratch tester (PLST) and a multi-pass scratch tester (MPST). Microhardness tests and scanning electron microscopy (SEM) were also used to examine the hardness and microstructure of the NbN coatings. These results have indicated that the structural, mechanical, and adhesion properties of the NbN coatings improve with increasing target currents. While performing PLST and MPST tests, the highest adhesion and lowest friction force were obtained for the coatings deposited at a target current of 3.5 A. In addition, the triboscobic behaviors that were observed from the MPST of the coatings indicated that the target currents affect the friction behavior of the coatings.     

Effect of microstructure on the adhesion strength of TiBx coating on Ti6Al4V substrate

TiB_x coatings were deposited on Ti6Al4V and Si (100) wafer substrates by D.C. magnetron sputtering with various target-to-substrate distances (T.S. distances) from 50 mm to 200 mm. The influence of T.S. distance on the microstructure, hardness and adhesion strength of TiB_x coatings and Ti6Al4V substrate system was investigated. Results showed that the microstructure of TiB_x coatings transformed from dense to fibre columnar grain with the increase in T.S. distance, whilst the hardness decreased from 20.9 GPa to 9.4 GPa. The Rockwell-C indentation adhesion strength grade was also improved from HF6 to HF1. An adhesion evaluation factor G, which is related to the mechanical properties and the microstructure of TiB_x coating, is proposed based on the test results. The adhesion strength increased with G, which corresponded well with the results of indentation test. The high-speed rubbing test with a sliding speed of 300 m/s was performed to check the Al-adhesion resistance of the TiB_x coating against Al–hBN seal coating.     

Characterization of (Ti1−xAlx)N films prepared by radio frequency reactive magnetron sputtering

(Ti_1−xAl_x)N films were deposited by radio frequency reactive magnetron sputtering on a high speed steel substrate. The structure and composition of the coatings were analysed by various techniques. Hardness and adhesion of the films were investigated using Vickers micro-indentation and scratch test respectively, whereas their tribological properties were studied using a pin-on-disk tribometer. The results show that increasing aluminium content leads to increase hardness of the films and to decrease their wear resistance when sliding against a magnesia-stabilized zirconia ball. On the contrary, no clear dependence of the film adhesion on the aluminium concentration was detected.     

Corrosion and friction resistance of TiVCrZrWNx high entropy ceramics coatings prepared by magnetron sputtering

High entropy alloy coatings have attracted much attention because of their high hardness, low-level fault energy, and chemical stability. Nevertheless, this type of coating would inevitably suffer from wear, corrosion, aging, and so on. Hence, a novel coating with corrosion and friction resistance would be constructed for broadening its application scenarios. In this work, TiVCrZrWN_x high entropy ceramics coatings were prepared by reactive magnetron sputtering. The microstructure, mechanical properties, friction, and corrosion resistance of the coatings deposited at different nitrogen flow rates have been studied. The microstructure of TiVCrZrWN_x coatings is strongly dependent on the nitrogen flow rate and forms a stable FCC structure when the nitrogen flow rate reaches 24 sccm. The pure TiVCrZrW coating is 15.65 GPa, with the increase of nitrogen flow rate (24 sccm), the coating hardness reaches 21.27 GPa. The corrosion resistance of the coatings also increases continuously. According to the results of the impedance spectrum and polarization curve, the charge transfer resistance value of the coating gradually increases with the content of nitrogen, the current density rapidly decreases to a minimum as the potential increases. In terms of tribological behavior, the formation of V₂O₅ during the sliding in seawater could significantly reduce the coefficient of friction from 0.603 to 0.383. Therefore, TiVCrZrWN_x HECs coatings simultaneously possess high hardness, toughness, and excellent resistance to friction and corrosion, which is expected to provide a new and reliable method for the research field of coatings in the maritime field.     

Evaluation of hardness, tribological behaviour and impact load of carbon-based hard composite coatings exposed to the influence of humidity

Diamond-like composite coatings were deposited by PACVD with an interface magnetron sputtered metallic layer prepared by d.c. unbalanced magnetron sputtering onto HSS substrates. The focus of the present work was on the study of the humidity effect on the tribological properties, hardness and impact resistance of the deposited coatings. The coatings were tested under both dry and humid conditions using several testing methods, like the pin-on-disc test equipped with linear reciprocating movement, impact test and depth sensing indentation test. It was found that the humidity may substantially influence not only the results of tribological tests, but surprisingly, also the results of the dynamic wear and hardness tests. By increasing the relative humidity, the value of dynamic impact resistance increased at an equivalent stress of 1.6 GPa more than three times. On the other hand, the wear rate of the coated part increased by more than four orders of magnitude. The results of the indentation test were influenced by humidity mainly at nanometre scales. The hardness measured at dry conditions was higher by 25% than the values obtained by the measurements under humid conditions.     

Adhesion and tribological properties of TiTaBN coatings with a graded interlayer deposited by pulsed DC biased and continuous dc biased magnetron sputtering

The properties of TiBN-based coatings are significantly affected by adding alloying elements and coating parameters. Therefore, in this study, TiTaBN coatings with graded interlayer (CWGIL) were deposited on D2 steel substrates by pulsed DC biased (PDCB) and continuously DC biased (CDCB) closed field unbalanced magnetron sputtering (CFUBMS). The structural, mechanical, adhesion and tribological properties of the coatings were analysed with EDS, SEM, XRD, microhardness, scratch testing and a pin-on-disc tribo-tester (under various atmospheric conditions). TiTaBN CWGIL deposited by PDCB magnetron sputtering (MS) had a very dense microstructure, high hardness and a high critical load value. TiTaBN CWGIL deposited by PDCB MS had a lower friction coefficient, the wear rate and the penetration depth in all atmospheric conditions. In conclusion, the application of a PDCB substrate instead of a CDCB one dramatically increases the performance of CFUBMS-deposited TiTaBN coatings.     

Wear-resistant Ti–Al–Ni–C–N coatings produced by magnetron sputtering of SHS-targets in the DC and HIPIMS modes

The hard wear-resistant nanocomposite Ti–Al–Ni–C–N coatings were deposited by direct current magnetron sputtering (DCMS) and high power impulse magnetron sputtering (HIPIMS) in the Ar, Ar+15%N_2, and Ar+25%N₂ atmospheres. The structure of coatings was analyzed using the X-ray diffraction analysis, glow discharge optical emission spectroscopy, and scanning electron microscopy. Mechanical and tribological properties were measured using the nanoindentation and scratch testing as well as by tribological testing using the “pin-on-disc” scheme. Electrochemical corrosion resistance and oxidation resistance of coatings were investigated. The results suggest that the coatings are based on the FCC phases TiCN and Ni₃Al with crystallites size ~3 and ~15 nm, correspondingly. DCMS coatings with optimal composition were characterized by hardness 34 GPa, stable friction coefficient <0.26 and wear rate <5 × 10^-6 mm³N^-1m^-1. Application of HIPIMS mode allowed the increase of adhesion strength, tribological properties and corrosion resistance of coatings.     

Methods for studying the mechanical and tribological properties of hard and soft coatings with a nano-indenter

This study illustrates the capabilities of a nanoindentation/nanoscratch tester to assess mechanical and tribological properties of coating films. Properties such as hardness, elastic modulus, mar and scratch resistance, and critical force for cracking can be accurately measured. Operation of the Nano-Indenter is described in detail. A scanning probe microscope (SPM) is shown to be a valuable supplement to the Nano-Indenter. Well-characterized thermoset acrylic clearcoats and thermoplastic latex films were studied. For the first time, operating parameters are described for measurement of relatively soft coatings, such as films cast from a latex with a glass transition temperature (T_g) of 8°C. Thus, the method is made available for study of most types of coatings. The method can easily discriminate between coatings with different T_gs and crosslink densities. Once operating parameters are established, it takes about 10 minutes for an indentation test and 10 minutes for a scratch test with the Nano-Indenter, and with further automation this time could be reduced. Each indentation test accurately measures hardness and elastic modulus as a function of depth within the coating, and each scratch test provides additional insight into the material’s behavior. The method is sensitive to small changes in polymer composition and formulation, and results are highly reproducible. Presented at the 81st Annual Meeting of the Federation of Societies for Coatings Technology, November 12–14, 2003, in Philadelphia, PA.     

Mechanical properties and thermal stability of tungsten boride films deposited by radio frequency magnetron sputtering

Tungsten and boron compounds belong to the group of superhard materials since their hardness could exceed 40?GPa. In this study, the properties of the tungsten boride WB_x coatings deposited by radio frequency magnetron sputtering were investigated. The sputtering was performed from specially prepared targets that were composed of boron and tungsten mixed in a molar ratio of 2.5 and sintered in Spark Plasma Sintering (SPS) process. WB films were deposited on silicon (100) and stainless steel 304 substrates at temperatures of 23 ÷ 770?°C. Microstructure, chemical and phase composition were investigated by using Scanning Electron Microscope (SEM), X-Ray Photoelectron Spectroscopy (XPS) and X-Ray Diffraction (XRD), respectively. The mechanical properties like Vickers hardness and Young's modulus were obtained by using nanoindentation test at a load of 5 ÷ 100 mN. The friction coefficient and wear resistance of αWB coatings were investigated in scratch test and reciprocal sliding wear instrumentation. Moreover, in order to investigate thermal properties, the αWB films were annealed at 1000?°C in argon/air for 1?h and at 250?°C for 2?h in air atmosphere. Results of our research confirm that αWB coatings can be considered as an alternative to superhard materials in the production of wear resistant, long-lasting tools.     

Mechanical properties and adhesion of TiN monolayer and TiN/TiAlN nanolayer coatings

In this work, TiN monolayer and TiN/TiAlN nanolayer coatings were deposited on 100C6 (AISI 52100) steel substrate by Physical vapor deposited (PVD) magnetron sputtering system. The morphological characterization was evaluated using an atomic force microscopy. The mechanical properties were determined by nanoindentation test. The adhesion was investigated by both microindentation and scratch test. The results show that the TiN/TiAlN nanolayer coating have the more rough surface and the better mechanical properties and adhesion compared to TiN monolayer coating. The effect of microstructural and mechanical proprieties on the adhesion behavior was further discussed. It was found that the improvement in adhesion of nanolayer system is in part due to the increase in plastic deformation resistance and the enhancement of mechanical properties (hardness and elastic modulus) and to the structure with a small grain size and a high number of interfaces.     

Adhesion of diamond coatings on steel and copper with a titanium interlayer

Adherent diamond coatings on steel and copper were obtained by using a titanium interlayer. The adhesion of the coatings was evaluated by scratch tests and micro-indentation tests. The diamond coating on steel exhibited a much higher critical load than on copper, as revealed by the scratch tests. However, an observation on the back of the scratch-delaminated film and on the corresponding substrate surface showed that the detachment occurred between the diamond film and the titanium interlayer. Therefore, the difference in the critical scratch load is due mainly to a substrate effect, making it difficult to compare the adhesion of different coatings.On the other hand, Knoop indentation tests showed interesting results: a small indentation load causes round spallation in the film with no observable crack. An exponential sink-in deformation under the indentation is proposed, y=−a exp(−bx). The coating adhesion is considered to be equivalent to the deformation stress at the edge of the spallation zone. The adhesion of diamond coatings on steel and copper with a titanium interlayer is evaluated quantitatively using this model. Furthermore, a thermal quench method is proposed to estimate the coating adhesion. The results found are in agreement with the indentation model.     

Investigation of the mechanical properties of electrodeposited nickel and magnetron sputtered chromium nitride coatings deposited on mild steel substrate

Electrodeposition and magnetron sputtering techniques have been employed for the deposition of Ni and bilayer NiCrN coatings, respectively, on mild steel substrate. Ni electrodeposition was performed using sulfate Watt’s bath, while magnetron sputtering was performed on electrodeposited Ni using DC power 350 W and base pressure of 3 × 10^?5 Torr in order to prepare bilayer NiCrN coatings. Structural and mechanical properties of Ni and bilayer NiCrN coatings have been investigated using various characterization techniques such as SEM-EDX, XRD, hardness, adhesion testing, etc. SEM analysis reflects the formation of spherical/nodular particles of varying sizes in NiCrN coating whereas Ni coating shows irregular, agglomerated, and non-uniform distribution of particles. Formation of hard CrN phase in NiCrN coating has been confirmed by XRD and EDX. NiCrN coating exhibits better hardness in comparison with Ni coating due to the formation of nitride phase. Micro scratch testing of bilayer NiCrN coating shows better interlayer adhesion and adhesion with mild steel substrate. The combination of electrodeposition and magnetron sputtering can produce inexpensive NiCrN coating containing hard CrN phase with better mechanical properties for automotive applications.     

Effects of tailored nitriding layers on comprehensive properties of duplex plasma-treated AlTiN coatings

Duplex-treated AlTiN coatings were deposited by advanced plasma assisted arc (APA-Arc) technology on pre-plasma nitrided AISI-H13 steel substrates using different N₂/H₂ flow ratios. The microstructures and properties of the AlTiN coatings were comprehensively characterized and analyzed. The results show that the N₂/H₂ flow ratios can tailor the thickness of compound layer during plasma nitriding process and the bright nitriding layer without compound layer is achieved. The properties of duplex-treated AlTiN coatings are well improved compared with monolayer AlTiN coating. The adhesion of the AlTiN coating is well enhanced by duplex treatment process, and adhesion grade increases from HF3-4 for monolayer AlTiN coating to HF1 for composite coatings. Moreover, the composite coatings with various thickness compound layers show different load-bearing capacities, and the interfacial adhesion force of the composite coating without compound layer reaches 61 N. The hardness of AlTiN coating is also enhanced by duplex treatment with the highest hardness of 2935 HV_0.05. Meanwhile, tribological properties of AlTiN coatings are also slightly improved by duplex treatments.     

A macroscopically nondestructive method for characterizing surface mechanical properties of polymeric coatings under accelerated weathering

The surface of coatings and plastics is the first target in any degradation process initiated by ultraviolet (UV) radiation or mechanical stress (via scratch and abrasion). Surface damage can lead to changes in optical, morphological, and mechanical properties and can result in pathways for ingress of moisture and corrosive agents. Current test methods for monitoring performance of protective coatings focus on chemical properties and optical properties, such as color and gloss measurements, or invasive tests such as abrasion and cross-cut adhesion. In this study, a macroscopically nondestructive performance protocol using nanoindentation metrology via a well-controlled scratch test was applied to evaluate the scratch resistance and monitor the surface mechanical property changes in a protective coating under accelerated weathering. Polyurethane (PU) coatings with different polyol compositions were chosen for this study. Coating specimens were exposed to high-intensity UV radiation at 55°C and 75% RH conditions. Exposed specimens were removed at specified UV exposure times for surface modulus/hardness and scratch resistance characterization via nanoindentation and scratch test. The effect of polyol type and UV radiation dose on the scratch damage (scratch morphology) was investigated and correlated with the surface hardness and modulus of the materials.     

Influence of power frequency on the performance of SiC thin films deposited by pulsed DC magnetron sputtering

Because of its high stability, good wear resistance, and high mechanical hardness, SiC is widely used in various mechanical parts as a protective film. However, there have been few reports published on the preparation of SiC films by pulsed DC magnetron sputtering. In this work, SiC films were deposited onto glass and ceramic substrates from a sintered SiC target through pulsed DC magnetron sputtering. The influence of the variation of the power pulse frequency (0?kHz, 50?kHz, 150?kHz, 250?kHz, and 300?kHz) on the film’s performance was studied. The surface morphology, structural characteristics, hardness, and adhesion strength of the deposited SiC films were investigated here. The results show that all the deposited films adhered well to the substrate. They were smooth, compact, and presented an amorphous structure. The film hardness was found to increase as the pulse frequency was increased. When the pulse frequency was 250?kHz, the resulting SiC film possessed optimal mechanical properties with a hardness of 25.74?GPa (measured using a nanometer indentation instrument) and an adhesion strength of about 36?N (measured by scratch tester).     

Microstructure,adhesion, mechanical and corrosion properties of TiN coatings deposited by high energy pulse-enhanced vacuum arc evaporation

Abstract

Pulse-enhanced vacuum arc evaporation (PEVAE) which combines pulsed and direct current operation of the arc source is a new method in cathodic arc evaporation technology. One advantage is to emit large amount of electrons which leading to more ionization of gas and metal. In this work, microstructure, adhesion and properties of TiN coatings related to substrate ion current and deposition energy E_bi at different nitrogen pressure were investigated. The experimental results revealed that compared to DC mode the substrate current and energy E_bi during PEVAE process were increased by 111 and 40.0% at most inducing denser morphology, a little bigger crystal size and much higher compressive stress which was related to the enhancement effect of the high pulse current on electron emission. Hardness values of TiN coatings were increased up to about 36–38?GPa. Adhesion of the coating was substantially improved with critical load 100?N and adhesion class HF 1 in scratch test and indentation test, respectively. This is due to denser morphology, higher H/E and H³/E² ratios and less defects caused by higher substrate ion current and E_bi. The resistance to electrochemical corrosion and high-temperature oxidation and wear performance were also substantially improved because of the denser structure and higher H³/E² ratio. In spite of changes in the nitrogen pressure, less changes had taken place in the microstructure and properties of the TiN thin coatings deposited by PEVAE than those prepared with the DC mode.     

DLC–ceramic multilayers for automotive applications

The present work explores the deposition of hard, wear resistant multilayer coatings, by magnetron sputtering onto Aluminium (Al) alloy substrates that are used in the automotive industry. Multilayer coatings have been manufactured to increase surface hardness and wear resistance for a commercial powder metallurgy Al alloys (Al 2618). The multilayer coating consisted of 25 bi-layers of Titanium Diboride (TiB₂) and diamond-like carbon (DLC). These DLC/TiB₂ coatings were fabricated, maintaining a constant composition wavelength (sum of two layers [λ] = 200 nm) for an array of ceramic fractions ranging from 75% to 95% by volume. The effect of the DLC content on the structure and performance (hardness and adhesion) of the films was investigated. The bi-layer thickness influences the failure patterns resulting from the scratch testing. This study has found hardness values of 27.8 GPa, with a critical load of 20 N and a friction coefficient of 0.47. As a result of these findings the multilayer with 10% of DLC was found to be a better compromise between high hardness (23.8 GPa) and high adhesion (critical load higher than 20 N) and with no signs of cracking during friction testing, proving to be a solution to be employed in components located in the upper valve train area of high performance vehicles.