Scratch adhesion and wear failure characteristics of PVD multilayer CrTi/CrTiN thin film ceramic coating deposited on AA7075-T6 aerospace alloy

This study highlights the scratch adhesion failure characterization and tribo-mechanical properties of physical vapor deposited (Cr, Ti) N coating on AA7075-T6 by using magnetron-sputtering technique. The surface morphology, microstructure and chemical composition of CrTi/CrTiN film were inspected by an optical microscope, scanning electron microscope (SEM) incorporated with energy dispersive X-ray spectroscopy (EDX) in addition to focused ion beam milling. The coating to substrate critical load of about 1261 mN was obtained, by employing coating deposition parameters of; DC power (300 W, RF power (200 W)), temperature (300 °C) and nitrogen flow rate (6%). Failure adhesion characteristics exhibited initial arc-tensile cracking followed by chipping and spallation that led to complete coating failure at L_c3. The tribo-mechanical aspects were evaluated by a pin-on-plate reciprocating testing unit, which showed a lower friction coefficient of 0.36 for CrTiN as compared with 0.43 for AA7075-T6. Subsequently, the wear depth was also reduced from 9.5 to 5.9 μm. It was revealed that the wear mechanism for AA7075-T6 was extensive deformation, abrasion and delamination, while the CrTiN exhibited slightly oxidative abrasive wear mode.     

The influence of multilayer structure on mechanical behavior of TiN/TiAlSiN multilayer coating

Nitride coatings have been generally applied on light alloys like titanium and aluminium to promote their multiple performances, including hardness, thermal stability and wear resistance. In this work, TiAlSiN/TiN multilayered (ML) coating and TiAlSiN single-layer (SL) coating were deposited on TC18 (Ti5Al5Mo5V1CrFe) alloy by Multi-arc ion plating technique. The microstructure and chemical composition of the coatings were evaluated by SEM, XRD and XPS. Additionally, hardness, adhesion and wear resistance were measured through nanoindentation, scratch spectrometer and ball-on-disk tribometer. The results present that both ML and SL coating contain three main phases of TiN, Al₂O₃ and Si₃N₄. Nevertheless, the adhesion of ML coating is 62.4 N, compared to that of the SL coating is 51.8 N. The parameter H³/E² as an indication of plastic deformation to evaluate wear resistance shows that the ML coating has high hardness and high toughness concurrently. The tribological study indicated that the wear rate of the ML coated specimen was 1/7 of the SL coated counterpart.     

The effect of nitrogen flow rate on TiBN coatings deposited on cold work tool steel

TiBN coatings have high hardness and high adhesion. Due to these excellent properties there has been increasing interest in TiBN coatings. In this study, TiBN coatings were deposited on AISI D2 cold work tool steel and silicon wafers by closed field unbalanced magnetron sputtering (CFUBMS). The structural, mechanical and adhesion properties of these coatings were analysed by X-ray diffraction, scanning electron microscopy, microhardness test, indentation test and scratch tests. TiBN coatings produced by magnetron sputtering exhibited a dense and columnar structure. These results indicate that TiB₂, TiN and h-BN exist in crystalline forms at all coatings. The highest hardness was obtained at the lowest nitrogen flow rate. Very few cracks were observed at the edge of the indentation marks at the highest nitrogen flow rate. The highest critical load obtained with scratch test was identified as 102?N.     

On the evaluation of adhesion of coatings by automatic scratch testing

Automatic scratch testing is an expedient technique for comparatively evaluating the cohesive failure load and adhesion failure load of thin coatings on various substrates. In combination with SEM examination of the scratch track, this technique has been used herein to detect and evaluate various effects on coating strength and adhesion. For soft Triballoy T-800 and Stellite SF-6 cobalt-base coatings on 4340 low alloy steel, adhesion was found to be strong and failure was found to be cohesive in the coating. In the presence of a plated chromium interlayer, pre-existing cracks lowered substantially the cohesive failure load, which was also lowered by an increase in the coating deposition pressure. The spacing of transverse cracks within the coating was found in all cases to decrease with increasing applied normal load. In soft aluminum coatings on depleted uranium (DU)-0.75% Ti alloy specimens, alloying aluminum with magnesium or zinc enhanced the coating strength and adhesion. In (Al-Mg) coatings on this substrate, a smoother surface led to a lower friction coefficient and a higher adhesion failure load. In hard, thin TiN coatings on 17-4 PH steel, a lower bias voltage applied to the substrate yielded higher cohesive and adhesion failure loads. In hydrogenated amorphous SiC thin coatings on 4340 steel, loss of hydrogen by annealing converted the residual compressive stresses into tensile stresses and lowered both the cohesive and the adhesion failure loads. Finally, automatic scratch testing proved helpful in determining delamination loads in multilayer TiN/Ti/TiN coatings on DU-0.75% Ti alloy.     

Preparation of a hydrophobic cerium oxide nanoparticle coating with polymer binder via a facile solution route

In this work, cerium oxide (CeO₂) nanoparticles (NPs) were synthesized using a facile, low temperature solution process and coated using spin coating and spray coating approaches, for the fabrication of a hydrophobic surface coating. Silicon wafer (Si) substrates coated with CeO₂ NPs exhibited excellent hydrophobic behavior, but poor adhesion of the NPs to the substrate was observed - likely due to the low surface polarity of CeO₂ NPs. Polyacrylic acid (PAA) was introduced as an adhesion promoter to improve NP surface characteristics and obtain an adherent and cohesive coating. Slight polarity tuning and binder inclusion significantly enhanced the binding capability of the NPs as determined by peel-off measurements. The superior mechanical properties of NP coatings were attributed to the incorporation of PAA in the polymeric network. It improves inter-particle and particle-substrate secondary interactions, ultimately aiding NP cohesion and adhesion when deposited onto the Si substrate. The adhesive and hydrophobic properties of CeO₂ NP coatings were maintained upon exposure to high temperatures, and the coatings are transparent as well, making them suitable for various applications, such as cookware, glass coating and technology components.     

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.     

Correlation between microstructure,chemical components and tribological properties of plasma-sprayed Cr2O3-based coatings

The wear resistance of chromium oxide (Cr₂O₃) coatings could be improved by doping modification and changing the structural scale, etc. In this study, micrometric Cr₂O₃ coatings were doped with different additives, CeO₂ and Nb₂O₅. Moreover, Cr₂O₃ coatings were deposited from nanostructured feedstock by the combination process of plasma spraying and dry-ice blasting. The correlation between the microstructure, chemical components and tribological properties of plasma-sprayed Cr₂O₃-based coatings was discussed based on the investigation of their porosity, hardness and friction behaviors. The results showed that the composite coatings doped with additives exhibited a higher microhardness, corresponding to a lower porosity than pure Cr₂O₃ coating under the identical plasma-spray condition. CeO₂ constituent was found to improve the wear resistance of Cr₂O₃ coating while Nb₂O₅ incorporation corresponds to a steep rise in the friction coefficient. The mismatch of coefficient of thermal expansion (CTE) between Cr₂O₃ and Nb₂O₅ lamellae facilitated the origin of fatigue cracks and the formation of microfracture pits. Although the combination process promotes a porosity reduction, the nanostructured Cr₂O₃ (n-Cr₂O₃) coatings present a lower microhardness than micrometric coatings, due to their loosen microstructure from insufficient plasma power compared to microscaled coatings. The wear mechanisms of both the micro- and nanometric Cr₂O₃ coatings are fatigue cracks and material transfer.     

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.     

Mechanical and tribological assessment of composite AlCrN or a-C:Ag-based thin films for implant application

The present study focuses on the comparison of cathodic arc deposited AlCrN (ternary coating) and Ag alloyed a-C (amorphous carbon base coating) on chrome nitride (CrN) medical grade 316 LVM stainless steel. The work comprises of morphological, structural, nanomechanical and tribological evaluation in physiological simulated body fluid (SBF) lubrication following conditions pertaining to simulated hip joint. According to the findings, H/E, H³/E² and E_coating/E_substrate significantly effect the nanomechanical and tribological properties of the coatings. While a-C:Ag/CrN exhibited better L_y value compared to AlCrN/CrN due to better surface quality, the later has shown higher L_c2 value during nanoscratch test attributed to lower H³/E² and higher plastic work done. Inspite of lower friction coefficient, a-C:Ag/CrN observed higher wear rate during simulated tribotest attributed to low hardness, separate graphitic structure due to Ag doping and sudden increase of friction coefficient ascribed to severe abrasive delamination of a-C:Ag top layer. The wear mechanism observed under SEM microscopy indicate severe adhesion of Ti6Al4V counterbody on AlCrN/CrN coated surface. The size of wear debris obtained with AlCrN/CrN-Ti6Al4V tribopair was larger in size compared to a-C:Ag/CrN-Ti6Al4V tribopair. Nevertheless, despite inferior surface quality and lower L_y value and larger wear debris size, AlCrN/CrN coating performed better in nanoscratch (at L_c2 value) and demonstrated lower wear in simulated tribotest in physiological SBF condition.     

Conversion of HA on NT-C/C Composites from Ultrasonic Induction Heating Deposited Monetite to FHA Coating by an Alkaline Followed by NaF Solution Hydrothermal Treatment Methods

An ultrasonic induction heating (UIH) deposited monetite coating on (NH₄)₂S₂O₈ treated (NT) C/C composites was subjected to a hydrothermal treatment to form a hydroxyapatite (HA) coating. This HA coating was then placed in a NaF solution and hydrothermally treated a second time to produce a fluorinated hydroxyapatite (FHA) coating. The structure, morphology and chemical composition of the HA and FHA coatings were characterized by XRD, FTIR, XPS SEM and EDS, and the adhesiveness of the two coatings to the NT-C/C substrates was evaluated by a scratch test. The results showed that after the NaF treatment, the FHA coating was a mixture of FHA and HA with some calcium oxides, and the FHA showed a higher degree of crystallization than the HA coating though the morphologies were similar. In addition, the EDS-determined Ca/P atomic ratio for the FHA coating was about 1.78 which was larger than 1.69 ratio of the HA coating. The bonding strength of the HA coating on C/C could reach a critical load of 60.3 N, while that of the as-prepared F-containing HA coating only had a critical load of 42.4 N. The reason of the lower adhesion for the FHA coating than that for the HA coating is suggested to be correlated with the constituent and structure of the two coatings.     

Study of the structure,properties, scratch resistance and deformation behaviour of graded Cr-CrN-Cr(1-x)AlxN coatings

An in-depth investigation of the structure, properties, scratch adhesion characteristics of graded Cr-CrN-Cr_(1-x)Al_xN coatings synthesized onto M42 steel substrates using closed – field unbalanced magnetron sputtering (CFUBMS) was carried out. Advanced microscopy (scanning and transmission electron microscopy), focused ion beam (FIB) imaging, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and micro–scratch tests was used to investigate the microstructure, mechanical properties and scratch performance as a function of Al content. FIB and TEM investigations revealed that the coatings exhibited a distinct structure; i.e., an adhesive Cr layer, a CrN transition layer and a graded CrAlN top layer with a face centered cubic (FCC) B1 structure. A columnar morphology was exhibited by the coatings and the dimensions of the columnar grains decreased with increasing Al content. Residual stress measurements, obtained from the XRD – sin²ψ method, revealed increasing compressive stresses with increasing Al content. Furthermore, nanoindentation tests showed an increase in mechanical properties, fracture toughness index (H/E) and plastic deformation resistance (H³/E²) as the Al content increased, accompanied by a decrease in the critical load, L_C, during scratch testing implying a decrease in scratch toughness.     

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.     

Intentional Polymer Particle Contamination and the Simulation of Adhesion Failure due to Transit Scratches in Ultra-thin Solar Control Coatings on Glass

The major in-service failure mechanism of modern solar control coatings for the architectural glass can be mechanical (e.g., scratch damage). Many of these coatings are multilayer structures of less than 100 nm thickness and different coating architectures are possible (i.e., different layer materials, thickness and stacking order). For high-performance solar control coatings deposited by physical vapour deposition processes the active layer is a thin silver coating (approx. 8 nm thick) surrounded by antireflection coatings (e.g., ZnO, SnO₂) and barrier layers (e.g., TiO _x N _y ). Scratches are often found during delivery of the coated glass (called transit scratches) and it has been determined that the cause of the scratches was the polymer balls sprayed onto the glass to separate sheets while in transportation. This study has developed a simulation test for the transit scratches and has determined that the adhesion of layers within the multilayer stack is critical in determining performance. To test the adhesion of the coatings, coated samples have been subjected to scratch tests using a range of indenters and the most visible damage has been characterised. Through-thickness cracks were observed and it was seen that the coating was stripped by the balls at the weakest point in the coating stack. Microanalysis reveals this weakest point to be the silver/zinc oxide interface in the materials analysed in this study.     

Optimization of microstructure and properties of composite coatings by laser cladding on titanium alloy

Recently, the current technological progress in developing laser cladding technology has brought new approaches in surface modification of titanium alloys. Herein, composite coatings were fabricated by the laser cladding process on Ti811 alloys using a coaxial powder feeding method. A comprehensive study was performed on the laser energy density (L_ed) and CeO₂ content on the structure distribution, microhardness and tribological properties of the coatings. In addition, the growth mechanism of the TiC–TiB₂ structure was studied based on the Bramfitt two-dimensional lattice mismatch theory. The results indicated that the phase composition of the coating mainly contained TiC, TiB₂, Ti₂Ni, and α-Ti. The optimized coating contributed to uniform microstructure distribution and fine grain size when L_ed was 45 J/mm² and the CeO₂ content was 2 wt%, playing an important role in the best forming quality and properties. Besides, the high matching degree of an interface between TiC (111) and TiB₂ (0001) contributed to the TiC–TiB₂ composite structure, which positively influenced the grain size and distribution of TiC. The microhardness and wear resistance of the 2Ce coating was dramatically enhanced due to the fine grain strengthening and dispersion strengthening effects of CeO₂, contributing directly to generate a high average hardness of 811.67 HV_0.5 with a lower friction coefficient.     

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.     

Strongly adherent Al2O3 coating on SS 316L: Optimization of plasma spray parameters and investigation of unique wear resistance behaviour under air and nitrogen environment

Plasma spray deposition of Al₂O₃ is a well-established technique for thick ceramic coatings on various substrates to shield them from corrosion and wear. Owing to its high hardness, aluminum oxide is known to protect stainless steel substrates from wear. However, the plasma process requires optimization for desired coating thickness and adhesion strength. It is also necessary to understand the sensitivity of friction and wear resistance of the deposited coating on exposed environment for evaluation of service life. The study offers comprehensive investigation on plasma process parameters for the development of strongly adherent aluminium oxide coatings on SS 316L substrate. Impact of environment like dry air and dry nitrogen on tribological properties of the coatings was also investigated. Dense adherent coatings of alumina could be deposited on SS 316L at a plasma power of 20 kW with an intermediate bond coat of NiCrAlY to enhance the adhesion properties. The effects of stand-off distance and bond coat thickness on adhesion strength were additionally examined. Further, the coatings were characterised for phase composition, microstructure, microhardness and wear resistance potential. Reciprocating wear tests of the coatings were carried out using ball on disc reciprocating tribometer at different loading conditions (5, 10 and 15 N) at constant (5 Hz) sliding frequency. Unlike the coefficient of friction (COF), wear volume was found to increase with an increase in normal load. These adherent coatings revealed promising properties for the applications where the tribological failure of SS 316L in dry air or dry nitrogen environment is to be controlled.     

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.     

Effect of MoS2/PTFE coatings on performance of Si3N4/TiC ceramics in dry sliding against WC/Co

To enhance the tribological performance of Si₃N₄/TiC ceramics, MoS₂/PTFE composite coatings were deposited on the ceramic substrate through spraying method. The micrographs and basic properties of the MoS₂/PTFE coated samples were investigated. Dry sliding friction experiments against WC/Co ball were performed with the coated ceramics and traditional ones. These results showed that the composite coatings could significantly reduce the friction coefficient of ceramics, and protect the substrate from adhesion wear. The primary tribological mechanisms of the coated ceramics were abrasive wear, coating spalling and delamination, and the tribological property was transited from slight wear to serious wear with the increase of load because of the lower surface hardness and shear strength. The possible mechanisms for the effects of MoS₂/PTFE composite coatings on the friction performance of ceramics were discussed.     

Microstructure and properties of TiAlCrN ceramic coatings deposited by hybrid HiPIMS/DC magnetron co-sputtering

TiAlCrN ceramic coatings were prepared utilizing a hybrid deposition technique consisting of High Power Impulse Magnetron Sputtering (HiPIMS) and Direct Current Magnetron Sputtering (DCMS). The chemical composition, phase structure, morphologies, mechanical and tribological properties of such coatings were systematically investigated. Results indicated that the content of Ti element increased monotonically from 0 at.% to 22 at.% with increasing of Ti target power. The TiAlCrN ceramic coatings presented a competitive growth tendency between (111) and (200) crystal plane through the energetic ion bombardment. Higher Ti target power resulted in stronger compressive intrinsic stress, which significantly suppressed the precipitation of hcp-AlN phase. With enhancing ion bombardment, diffusion energy and nucleation rate of adatoms on the growing surface increased, which caused a denser structure and ultra-smooth surface. The hardness and toughness also varied as a function of Ti target power, with the maximum hardness of 28.3 GPa under a Ti target power of 5 kW. Positive correlation between the adhesion strength (i.e., the critical load of the scratch test) and H³/E² ratio was discovered indicating a strong dependence of adhesion properties on toughness for the TiAlCrN ceramic coatings in this study, which agreed well with the literatures. As for the tribological behavior, the lowest wear rate of 8.9 × 10^-17 m³N^-1m^-1 was obtained for the TiAlCrN ceramic coating deposited at a Ti target power of 5 kW.     

Influence of substrate treatment on the tribological properties of DLC coatings

Due to the very thin nature of DLC coatings, the substrate must carry the main part of the applied load. If the substrate has insufficient strength to carry the contact load and thus support the coating, plastic deformation will occur, leading to premature failure of the coating. The challenge to improve the properties of hard DLC coatings by thermo-chemical pre-treatment of the substrate has gained much attention in recent years, leading to a new method called duplex treatment. In the present study, a hydrogen-free hard carbon coating deposited on plasma nitrided AISI 4140 steel was investigated with respect to microhardness, residual stress, scratch adhesion and dry sliding wear resistance. The pin-on-disc results showed that nitriding of the substrate improves the wear resistance of the hydrogen-free hard carbon coating as compared to the hardened substrate. The improvement can be related to the increased load carrying capacity of the steel substrate and to improved coating to substrate adhesion.