Closed Field Unbalanced Magnetron Sputtering Research Articles

PVD Coatings for Lightweight Bipolar Plates

Bipolar plates are one of the main components of proton exchange membrane fuel cells (PEMFCs). Their functions include distributing reactants, supporting the cell, and conducting heat and electricity. They account for a significant proportion of the fuel cell stack’s weight and volume. The main materials currently used for bipolar plates are graphite and stainless steel. Aluminium has a much lower density than steel and is easier to form than both steel and graphite. Its use, therefore, would allow fuel cells with higher power densities but is hindered due to it being prone to corrosion. This work focused on the development of corrosion-resistant and conductive coatings to address this issue. Carbon coatings with Ti and Cr adhesion layers were deposited on aluminium substrates using closed-field unbalanced magnetron sputtering. These coatings were tested for corrosion properties and performance on the cathode side of a single-cell fuel cell. Coated aluminium samples were also tested for their ability to maintain their corrosion protection after being formed. Coating with a Cr adhesion layer outperformed that with a Ti adhesion layer in both forming and fuel cell tests, demonstrating much lower performance degradation after accelerated stress testing.

Effect of diffusion barriers on steam oxidation properties and interface evolutions of Cr coating for zirconium alloy at 1200 °C

Currently, Cr-based coatings are considered the most promising protective coatings for zirconium alloy claddings under the ATF design concept. However, the primary factor affecting the oxidation resistance of Cr coatings is the interdiffusion of Cr and Zr. In this study, Cr coatings with three refractory metal interlayers of Nb, Mo, and Ta were deposited on zirconium alloy surfaces using closed-field unbalanced magnetron sputtering. The study investigated the effects of different interlayers on the microstructure, oxidation properties, and interface evolution process of Cr coatings under steam conditions at 1200 ℃, and compared them with Cr coatings without intermediate layers. The results indicate that the refractory metal interlayer influences the orientation and growth rate of Cr coating grains. The formation of a Laves phase mixed layer in the interlayer during oxidation effectively hinders the diffusion of O and Cr to the zirconium alloy matrix, enhancing its oxidation resistance. Furthermore, the diffusion rate and vacancy concentration of Mo and Ta elements to the Zr layer exceed that of diffusion to the Cr layer. During the cooling process, a precipitate phase forms in the Zr-4 matrix, while the Nb coating forms an infinite solid solution in the β-Zr.

Nb-doped hydrogenated diamond-like carbon coated biodiesel injectors material: Synthesis, structure and properties

Despite the economic and environmental benefits of biodiesel, it poses significant challenges, including coking on metal surface and increased wear on diesel engine injector nozzles. Therefore, this study investigates the synthesis of niobium-doped diamond-like carbon (Nb-DLC) coatings on two types of injector nozzle materials (viz. H13 steel, AISI 420 stainless steel) using the Closed-Field Unbalanced Magnetron Sputtering (CFUBMS) technique. Comprehensive characterizations, including microstructural analysis, crystal structure evaluation, hardness assessment, and tribological property assessment, were conducted. The Nb-DLC coatings demonstrated a stable friction coefficient, with values four times lower than that of the substrate materials. The present findings demonstrate significant enhancements in terms of structural composition, crystalline phase, hardness, friction coefficients, and adhesion properties due to the Nb-DLC coatings. Therefore, Nb-DLC coated materials could be the promising candidate material for biodiesel engine injector nozzle applications. This emphasizes their potential to contribute significantly to the sustainable consolidation of biodiesel within automotive engine.

High-rate Deposition of Crystalline TiHfN Ultra-thin Films by Closed-field Dual-cathode DC Unbalanced Reactive Magnetron Sputtering without External Substrate Heating

High deposition rate titanium hafnium nitride (TiHfN) ultra-thin film deposition was successfully prepared by closed-field dual-cathode DC unbalanced reactive magnetron sputtering. All prepared films were polycrystalline. The morphology and atomic composition of the TiHfN ultra-thin film were characterized by field-emission scanning electron microscopy (FE-SEM) and energy dispersive spectroscopy (EDS). The columnar structure could be promoted by increasing the deposition time. Lastly, the surface-enhanced Raman scattering (SERS) activity was investigated by Rhodamine 6G (R6G) drop-dried TiHfN ultra-thin film surface. The TiHfN ultra-thin films deposited at 20 s were found to have a high SERS activity, whose detection of R6G molecule at 10-5 M. The result could open preliminary studies on ternary transition metal nitride (TTMN) thin films for the alternative plasmonic sensors as SERS chips.

Effect of deposition parameters on structural and mechanical properties of Novel h-BN doped TiCrNbN coatings

In this paper, the novel h-BN doped TiCrNbN thin films was deposited on the DIN 1.2714 steel using closed field unbalanced magnetron sputtering (CFUBMS) technique with variable working pressure, bias voltage, and LaB6 target voltage. The main goal is to determine the contribution of degrees of these parameters on structural and mechanical properties using Analysis of Variance (ANOVA). The deposition parameters were leveled based on L9 (33) orthogonal Taguchi design method. Microstructural and thickness of coatings were investigated using SEM. The coatings had granular and flawless surface properties. The thickness of the coatings was determined in the range of 874 nm and 1.69 μm. The deposition parameter that has the highest contribution to coating thickness is working pressure. Hardness and adhesion strength of coatings were determined employing nanohardness and scratch tester, respectively. The highest hardness among the coatings was 24.67 GPa, obtained with the 3x10-3 Torr working pressure, 100 V bias voltage and 600 V LaB6 target voltage parameters. The deposition parameter that has the highest contribution to hardness is working pressure. The coating conditions with the highest hardness exhibited the highest adhesion strength. The superiority of the contribution of working pressure on the adhesion strength was prominent compared to other parameters.

Combined magnetron sputtering and laser annealing process for the fabrication of proton conducting thin films

Acceptor doped barium zirconates are known for their exceptional protonic conductivity and the challenges in their fabrication. Within this work, BaZr0.8Y0.2O3-δ (BZY20) films were successfully deposited on a BaZr0.7Ce0.2Y0.1O3-δ/Ni (BZCY72/Ni) substrate using a combination of closed-field unbalanced magnetron sputtering and various annealing techniques such as conventional furnace annealing and laser annealing. Thin films could be tempered at only 800 °C with an additional laser annealing step and exhibit a heigh density as well as a sufficient protonic conductance. The highest measured ionic conductivity was 1.11*10−3 S/cm. The provided synthesis could pave the way for employing metallic supports in protonic ceramic fuel cells by using lower sintering temperatures than normally required.

Developing advanced CrSi coatings for combatting surface degradation of N-type (Zr,Ti)Ni(Sn,Sb) and P-type (Zr,Ti)Co(Sn,Sb) half Heusler thermoelectric materials

In this study, advanced oxidation-protective CrSi coatings were developed and deposited on N-type (Zr,Ti)Ni(Sn,Sb) and P-type (Zr,Ti)Co(Sn,Sb) thermoelectric (TE) materials using an environmentally friendly closed field unbalanced magnetron sputtering PVD system. The oxidation behaviour of the CrSi-coated and uncoated samples was evaluated through static oxidation tests at 500 °C and 600 °C for 10h and 50 h, respectively. In addition, the samples were exposed to cyclic oxidation tests between 25 °C and 500 °C for 10, 30 and 50 cycles, with each cycle consisting of 1h of oxidation at 500 °C, to examine the coating ability to withstand thermal shock, which is involved in the service of TE devices. The surface morphology, cross-section layer structure, elemental distribution and phase constitution were analysed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX) and X-ray diffraction (XRD). The mass gain after the oxidation tests was measured and calculated for each sample to study the oxidation kinetics. The uncoated samples exhibited a considerable amount of oxidation, leading to change in the surface morphologies, and the formation of alternated layers including oxide products (Zr(Ti)O2, SnO2) and Ni3Sn4 compound for the N-type and (Zr(Ti)O2, SnO2, Sb2O4) and CoSb compound for the P-type material, after static and cyclic oxidation tests. The experimental work in this study has, for the first time, demonstrated that the CrSi coatings developed with very high thermal stability and oxidation resistance can effectively protect both the N-type and P-type materials from oxidation and sublimation even during cyclic oxidation tests. The strong affinity of Cr and Si to oxygen can trap oxygen, retard its inward diffusion and thus protect the TE material substrate from oxidation. This finding could pave the way towards the further development of long-life high-performance TE generators and devices, thus contributing to the net zero target.

Thin Film Based Membrane Electrode Assemblies for Solid-State Ammonia Synthesis

Ammonia is the of the most crucial chemicals and currently primarily produced through the Haber-Bosch process causing the industrial ammonia production to emit more CO2 than any other chemical-making reaction. While the current primary function of ammonia lies within the fertilizer production, it can also be directly used as a fuel for power generation or in the maritime industry. Compared to hydrogen, ammonia has superior storage and transportation capabilities due to its greater volumetric energy density and mild conditions for liquefication. Given the need of reducing global carbon emissions, ammonia could be synthesized electrochemically using air, water and electricity by the Solid-State Ammonia Synthesis (SSAS). Protonic ceramic cells operate within an intermediate temperature regime of around 450 - 550 °C which is well suited for this process. Within our work, we present a tubular membrane electrode unit entirely made of ceramic components based on a barium zirconate thin film electrolyte. An ammonia production rate of 9.06 × 10-10 mol s-1 cm-2 and a Faradaicefficiency of 6.58% were achieved using a NiO-BaZr0.7Ce0.2Y0.1O3- δ | BaZr0.8Y0.2O3- δ | Ru@Ba0.5Sr0.5TiO3-δ cell.A key innovation lies in the production of dense BaZr0.8Y0.2O3-δ electrolyte layers, ranging from 1 to 5 µm in thickness, utilizing a Closed-Field Unbalanced Magnetron Sputtering (CFUMS) process. This technique allows precise adjustments of stoichiometric ratios within the perovskite structure, offering improved sputtering yields compared to conventional methods. Furthermore, the crystallinity, phase purity, and microstructure of sputter-deposited thin films are enhanced through selective laser annealing (SLA), resulting in high-density films composed of single-phase BaZr0.8Y0.2O3-δ with average crystallite sizes of 200 nm while avoiding substrate damage from thermal stress. Electrochemical performance was evaluated through impedance spectroscopy, half-cell tests and full cell tests providing insights into the efficacy of the developed tubular membrane reactor for the electrochemical synthesis of ammonia. The results demonstrate the feasibility of utilizing ceramic proton conductors in SSAS, particularly highlighting the potential of high-pressure operation up to 80 bars in tubular cells at relatively low temperatures around 450 °C, thereby achieving attractive NH3 production rates.This research contributes to the evolving landscape of sustainable ammonia synthesis by presenting a novel approach that integrates advanced materials and manufacturing techniques. Electrification and decentralization of the ammonia supply chain will expand the market by supporting its current use as fertilizer source and enable a new route as green energy carrier paving the way for an ammonia-based economy. Figure 1

Duplex surface engineering of cold spray Ti coatings and physical vapor-deposited TiN and AlTiN thin films

The feasibility of a duplex coating based on cold spray technology and magnetron sputtering was evaluated for repair applications requiring a ‘thin-on-thick’ layered structure. Commercially pure angular-shaped Ti grade 4 particles are fed to a cold spray gun and accelerated toward a Ti alloy substrate to deposit thick coatings (∼4.5 mm). TiN and AlTiN thin films are deposited on polished cold spray coatings using a four-source closed-field unbalanced magnetron sputtering (CFUBMS) system. Microstructure was characterized using focused ion beam (FIB) lift-out, scanning electron microscopy (SEM), and electron channeling contrast imaging (ECCI). The nanoindentation technique was used to evaluate the mechanical properties of coatings. The H/E ratios and H3/E2 ratios for TiN films were found to be 0.098 and 0.26 GPa, respectively, while those for AlTiN films were measured at 0.066 and 0.052 GPa, respectively, suggesting higher capacity of TiN films to withstand both elastic and plastic deformation. Using scratch testing, the adhesion of TiN and AlTiN thin films to cold spray Ti was investigated, with TiN-Ti duplex coatings exhibiting better performance compared to AlTiN-Ti coatings. Tribological testing was performed on duplex coatings using a reciprocating tribometer equipped with an alumina ball counterface. The wear rate for AlTiN-Ti coatings after 2000 sliding cycles was found to be (1.0 × 10−3 ± 0.1 × 10−3 mm3/Nm), three orders of magnitudes higher than that for TiN-Ti (8 × 10−6 ± 2 × 10−6 mm3/Nm. SEM was used to reveal worn surface morphologies and cross-sectional analysis of the wear track. Subsurface microstructural changes due to wear were examined using focused ion beam cross-sectioning, revealing bending cracks and tribofilm formation.

Fatigue and tensile behaviour of Ti+TiN+Ti+TiVN multilayer nitride films coated on AZ91 magnesium alloy by closed field unbalanced magnetron sputtering

Despite their extensive use in the automotive and aerospace industries, Mg and Mg alloys, which are light metals, exhibit low fatigue and tensile strength. In this study, transition metal-nitride (TMN) multilayer coatings (Ti+TiN+Ti+TiVN) were coated twice on AZ91 Mg alloy using a Confined Field Unbalanced Magnetron Sputtering (CFUBMS) system to increase fatigue and tensile strength. The structural properties of the films were analyzed by using X-ray diffraction (XRD), scanning electron microscope (SEM), and energy dispersive spectrometry (EDS) methods, and the mechanical properties were analyzed by rotating bending fatigue and tensile testing machines. Ti+TiN+Ti+TiVN multilayer nitride surface coatings on AZ91 Mg alloys showed a dense and columnar microstructure and according to XRD results (111) was the preferred orientation with the dominant peak. The fatigue limit value of the AZ91 base material was fixed at 60.46 MPa, while it increased to 68.48 MPa after being coated with multilayer nitride. Along with the multilayer nitride coating, the tensile strength increased from 169.98 MPa to 175.43 MPa. As a result, the multilayer hard nitride coating with low surface roughness, which fills the defects, notches, and voids on the surface of the AZ91 base material, increased the fatigue and tensile strength in parallel. Based on the outcomes of the research, the literature has been enriched with an innovative approach through the enhancement of fatigue and tensile strengths by applying a CFUBMS coating to lightweight metals and alloys, such as AZ91, especially in the transportation industry where lightness and dynamic load resistance are essential.

Investigation of Cu-doped amorphous carbon film in improving corrosion resistance and interfacial conductivity of proton exchange membrane fuel cell

This study investigated Cu-doped a-C films prepared under a substrate bias gradually reducing from 120 to 60 V and different Cu target currents of 0, 0.15, 0.2, 0.3, 0.5 A, respectively, using closed field unbalanced magnetron sputtering physical vapour deposition technique. While the Cu-doped a-C film at the lowest Cu target current of 0.15 A (A0.15) remained an amorphous microstructure, Cu nanoprecipitates occurred at Cu target currents of 0.2–0.5 A. All the Cu-doped a-C films prepared exhibited good combination of corrosion resistance to a corrosive chemical mixture of 0.5 M H2SO4 + 5 ppm HF (as suggested by the corrosion current densities) and interfacial electric conductivity (as demonstrated by the interfacial contact resistance, ICR). Among all coatings, A0.15 showed the best corrosion resistance and interfacial electric conductivity, which is attributable to the precipitate-free Cu-doped amorphous microstructure. The measured current density of A0.15 was 1.95 × 10−7 A/cm2 at 0.6 V (vs. SCE) during potentiodynamic polarization, which was lower than that of the Cu-free a-C film at 7.34 × 10−7 A/cm2. The ICR value of A0.15 was 4.40 mΩcm2 at an assembly pressure of 1.4 MPa, which is about one third of the Cu-free a-C film. This study demonstrates a new deposition strategy combining Cu-doping and the control of substrate bias to improve the corrosion resistance and interfacial electric conductivity of a-C films for PEMFC.

Comparative Performance Evaluation of Magnetron Sputtered TiN, AlCrN, and TiAlCrN Coatings

This study presents a comparative performance evaluation of magnetron-sputtered TiN, AlCrN, and TiAlCrN coatings on tool steel substrates. Coatings play a pivotal role in enhancing the durability of engineering components exposed to harsh conditions. TiN is known for outstanding hardness and durability, AlCrN for superior wear resistance, and TiAlCrN for exceptional thermal stability and oxidation resistance. The substrate (EN 1.2363) underwent PVD coating using a closed-field unbalanced magnetron sputter ion plating (CFUBMSIP) process in a water-cooled stainless-steel vacuum chamber with four magnetron ports, operating for 3 hours per batch followed by 12 hours of natural convection cooling, utilizing TiN, AlCrN, and TiAlCrN films deposited for 180 minutes in an Ar and nitrogen atmosphere. X-ray diffraction (XRD) revealed distinctive crystal structures, with all coatings exhibiting a common preferred orientation of the (111) plane and TiAlCrN showing a ternary nitride phase. Scanning electron microscopy (SEM) images displayed the compact nature of TiAlCrN with finer grains, while TiN exhibited a densely compacted with no evidence of delamination and AlCrN showed denseness with smaller grains. Nano-indentation test was conducted to assess the coatings' hardness and elastic modulus. TiAlCrN exhibited the highest hardness (3091±243 HV), highest elastic modulus (369.86±54.19 GPa), and the best wear rate (0.1887 x 10-4 mm3/Nm-1) suggesting potential suitability for applications demanding superior rigidity and wear resistance. The study provides valuable insights for materials scientists and engineers in optimizing coating selection for specific applications.

Application of honeycomb pattern to Ti2AlN MAX phase films by plasma etching

The honeycomb pattern possesses a distinctive hexagonal structure capable of seamless repetition on a flat surface, leaving no gaps. Moreover, all arm thicknesses and angles are equal to one another. This remarkable configuration is deemed biomimetic, with numerous examples found in nature. Notably, it exhibits remarkably low density and exceptional mechanical strength. MAX phase films have gathered significant attention due to their exceptional capacity to amalgamate the essential properties of both metals and ceramics. Additionally, they possess the unique ability to effectively mend surface cracks that may arise as a result of friction-wear, restoring the material to a certain degree of integrity. In this study, Ti2AlN MAX phase thin films were deposited on M2 steel substrates by a closed field unbalanced magnetron sputtering system (CFUBMS). 750 °C heat treatment was applied to obtain the produced films in crystalline form. In addition, plasma etching parameters suitable for the phase structure of the deposited film were determined. With the inductive coupling plasma etching (ICP) process, the honeycomb pattern was given to the Ti2AlN MAX phase films with a continuous and smooth geometry at a depth of 2 μm. This study gives ideas for the development of multi-coating systems in which patterns of different geometries are included in a single layer.

Corrosion behavior of metallic coatings on titanium bipolar plates of proton exchange membrane water electrolysis

The corrosion resistance, conductivity, and cost of the metallic bipolar plates are the main limitations for the Proton Exchange Membrane Water Electrolysis (PEMWE) commercialization. In the present study, Ta, Nb, and Ti non-precious metallic coatings were deposited by closed-field unbalanced magnetron sputtering to increase the corrosion resistance and conductivity of titanium bipolar plates in PEMWE, respectively. The coating samples suffer from corrosion in a simulated extreme anode operating environment of PEMWE (0.5 M H2SO4 + 5 ppm HF, 80 °C, O2). The surface of the Ti coating forms the micropores due to the high dissolution rate in initial formation stage of the passivation film, resulting in a higher current density (1.41 × 10−6 A cm−2). The hydrolysis reaction of Ta coating causes the adsorption of sulfide ions, thereby affecting the density of the passivation film. Despite the Ta coating exhibiting a favorable current density (4.82 × 10−7 A cm−2), ICR (463.11 mΩ cm2) is lamentably poor. The surface of Nb coating has been completely covered by Nb2O5 and NbO2 in the simulated PEMWE environment. The reoxidation process of NbO2 promotes the rate of passivation film formation and provides excellent conductivity. Therefore, Nb coating exhibits the lowest current density and interfacial contact resistance of 2.23 × 10−8 A cm−2 and 119.78 mΩ cm2, respectively, which is very low compared to the bare titanium bipolar plates.

Deposition of alternative plasmonic ZrHfN thin films via closed-field dual-cathode DC unbalanced magnetron sputtering for enhanced SEF substrate applications

We present the preparation of zirconium hafnium nitride thin films as an alternative plasmonic sensing material. The ZrHfN thin films were deposited by closed-field dual-cathode DC unbalanced magnetron sputtering without an external substrate heating/biasing. A comprehensive investigation into the effect of zirconium sputtering current on the physical structural, and chemical compositions was systematically characterized by grazing-incidence X-ray diffraction, transmission electron microscopy, atomic force microscopy, X-ray photoelectron spectroscopy, and X-ray absorption spectroscopy. Our results indicate that the optimal ZrHfN thin films deposited at 500 mA-IZr exhibit good crystallinity and high surface roughness, which presents excellent surface-enhanced fluorescent substrate performance for detecting rhodamine 6G at a limit of detection of 5.99 × 10−8 M, an enhancement factor of 15.62 ± 0.79-fold and displaying reusability through 25 cycles. These findings suggest promising prospects for developing ZrHfN-based SEF sensor chips for diverse applications in the future.

Scratch hardness of diamond-like carbon (DLC) coatings deposited by closed-field unbalanced magnetron sputtering

Thin coatings are subject to scratch and wear damage in tribological applications. Scratch hardness numbers are used to evaluate scratch and abrasive wear resistance. Few studies have measured the scratch hardness of thin films, and a proper scratch hardness measurement method for thin coatings is still lacking. In this study, the scratch hardness of these DLC coatings was measured at both micro-scale and nano-scale, respectively. The micro-scratch test using a 200 µm tip is an inapplicable method because the substrate effect has dominated the scratch hardness measurement. On the other hand, a nano-scratch hardness test using a sharper tip is an effective method to measure the scratch hardness of thin coatings. Although the scratch hardness introduces a lateral force compared with the indentation hardness, it well correlates with the nano-indentation hardness. The ratio of the scratch hardness to the indentation hardness is close to 1 for DLC coatings due to the amorphous structure. It proves that the tangential force induced by scratching does not influence the hardness property. In addition, a simple approach is proposed to obtain the scratch hardness of DLC coatings qualitatively without width measurement.

Pulsed-dc bias magnetron sputtered TiB2 ceramic coating

Titanium diboride, TiB2, is well known as a ceramic material with a hexagonal structure which presents various attractive properties, such as high hardness and excellent corrosion, thermal oxidation, and wear resistance. However, one drawback of TiB2 coatings is their poor adhesion to substrate materials due to high compressive residual stress after deposition. The present study aimed to assess whether a PVD-TiB2 coating with both high hardness and sufficiently good adhesion to the substrate and good wear properties can be developed by a closed-field unbalanced magnetron sputtering system using pulsed-dc biasing. The TiB2 coating deposited on AISI M2 steel substrates was characterized in terms of the structural, mechanical and tribological property. From the experimental results, it can be concluded that a closed-field unbalanced magnetron sputtering system using pulsed-dc biasing can be used to produce a TiB2 coating with sufficiently good adhesion (82 N), and high hardness (2300 HK0.01), and low friction (0.34) under given deposition conditions. The deposition conditions, particularly substrate biasing and rotation, which inhibited the formation of (001) orientation, played a role in the coating's lack of superhardness.

Investigation of properties of novel multilayer Cr/CrN/CrTiN/CrTiAlN hard coating with four bilayers

A novel multilayer Cr/CrN/CrTiN/CrTiAlN hard coating with four bilayers was developed by reactive closed field unbalanced magnetron sputtering (CFUBMS). The substrate temperature was kept in the range of 170 °C to 200 °C. The reactive gas flow was controlled by Optical Emission Monitoring. A thickness of 1.8 μm was determined using a calotester. The morphology and chemical composition were studied by electron microscopy (SEM and EDS). Nanohardness of 34.1 GPa and a modulus of elasticity of 386 GPa were determined using the nanoindentation technique. The scratch test against a diamond Rockwell indenter did not show features indicating poor adhesion. The reciprocating wear test revealed strong resistance to wear, and a coefficient of friction of 0.19 was determined. The developed multilayered hard coating showed optimal mechanical properties for industrial applications on instruments of low-temperature materials.

The effect of different annealing temperatures on the mechanical and tribological properties of the Ti2AlN MAX phase films

Ti2AlN MAX phase films produced at different N2 flow rates and different annealing temperatures were deposited on 52100 steel substrates using the closed-field unbalanced magnetron sputtering technique. N2 flow rates were changed to 2, 3.5, and 5 sccm. Due to the increasing N2 flow rate, film thickness decreased from 2 to 1.3 µm. Then the produced films were subjected to annealing at temperatures of 700, 750, and 800°C. After the film produced at a flow rate of 2 sccm was annealed at 750°C, the presence of the Ti2AlN MAX phase was determined. The binding energies of Ti 2p, Al 2p, and N 1s determined in the XPS analysis confirmed the existence of the Ti2AlN film. The friction coefficient measured for Ti2AlN MAX phase films was calculated as 0.53, the hardness value as 22.8 GPa, the elastic modulus as 291.4 GPa, and the wear rate as 2.96 × 10−4 mm3/(N·m).

Effect of Nb and V doped elements on the mechanical and tribological properties of CrYN coatings

One of the most promising approaches to enhancing the tribological properties of engineering coatings is to add transition elements to the structure. In this study, Nb-doped CrYN and V-doped CrYN thin films were deposited by pulsed DC reactive sputtering in a closed-field unbalanced magnetron sputtering (CFUBMS) system. The deposition parameters examined were target current (1, 1.5 and 2 A), deposition pressure (0.15, 0.25 and 0.35 Pa), pulse frequency (100, 200 and 350 kHz) and duty cycle (85 %, 70 % and 50 %). A Taguchi L9 orthogonal design was used to define the deposition process parameters for each doped film. The Nb and V-doped CrYN thin films were characterized in terms of their microstructure, thickness, composition, hardness and tribological properties by X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), nanohardness and pin-on-disc testing, respectively. The bond strength between the substrate and the films (adhesion) was analyzed by scratch testing. For the Nb-doped thin films, a maximum hardness value of 21.4 GPa and the lowest friction coefficient of 0.36 were obtained. On the other hand, in the V-doped thin films, the maximum hardness value was 16.1 GPa, while the lowest friction coefficient obtained was 0.11. In addition, Nb-doped and V-doped CrYN thin films exhibited extraordinary adhesion properties. The effect of the selected deposition parameters (target current, pulse frequency, and duty cycle) in relation to the film thickness, hardness, and coefficient of friction properties of the Nb and V-doped CrYN thin films were investigated using the Taguchi approach and optimum operating conditions were identified and confirmed.