Influence of boron doping on mechanical and tribological properties in multilayer CVD-diamond coating systems

Titanium alloy (Ti6Al4V) substrates were deposited with smooth multilayer coatings, by hot filament chemical vapour deposition technique. The effect of boron doping on lattice parameter, residual stresses, hardness and coefficient of friction in multilayer-diamond coating system was studied. The frictional behaviour of the coatings was studied using a ball-on-disc micro-tribometer by sliding the coated samples of titanium alloy (Ti6Al4V) substrates against alumina (Al₂O₃) balls, and increasing normal load from 1 to 10 N. The average friction coefficient decreased from 0.36 to 0.29 for undoped multilayer-diamond coating system and from 0.33 to 0.18 for boron- doped (BD) multilayer-diamond coating system. The average indentation depths for undoped and BD multilayer- diamond coating systems were found to be equal to ～>58 and ～65 nm, respectively, and their hardness values were 60 and 55 GPa, respectively.     

Structure,hardness and tribological properties of nanolayered TiN/TaN multilayer coatings

TiN/TaN coatings, consisting of alternating nanoscaled TiN and TaN layers, were deposited using magnetron sputtering technology. The structure, hardness, tribological properties and wear mechanism were assessed using X-ray diffraction, microhardness, ball-on-disc testing and a 3-D surface profiler, respectively. The results showed that the TiN/TaN coatings exhibited a good modulation period and a sharp interface between TiN and TaN layers. In mutilayered TiN/TaN coatings, the TiN layers had a cubic structure, but a hexagonal structure emerged among the TaN layers besides the cubic structure as the modulation period went beyond 8.5 nm. The microhardness was affected by the modulation period and a maximum hardness value of 31.5 GPa appeared at a modulation period of 8.5 nm. The coefficient of friction was high and the wear resistance was improved for TiN/TaN coatings compared with a homogenous TiN coating, the wear mechanism exhibited predominantly ploughing, material transfer and local spallation.     

Microstructure and mechanical properties of nanostructure multilayer CrN/Cr coatings on titanium alloy

Five different nanostructured, multilayer coatings (CrN/Cr)x8 with different thickness ratio of Cr and CrN layers were deposited by PAPVD (Plasma Assisted Physical Vapour Deposition) vacuum arc method on Ti6Al4V titanium alloy. The microstructure, chemical and phase composition of the CrN and Cr sub-layers were characterized by SEM with EDX and Cs-corrected dedicated STEM on cross-sections prepared by focus ion beam. Besides, hardness and Young's modulus of the (Cr/CrN)x8 coatings has been measured. The adhesion has been tested by scratch test method. The obtained (CrN/Cr) multilayer coatings, 5-6 μm in thickness, have homogeneous and nanocrystalline structure, free of pores and cracks. The microstructures of Cr and CrN layers consist of columnar grains below 100 nm in diameter. The hardness and Young's modulus of these coatings depend linearly on thickness ratio of Cr and CrN layers. The decrease of the thickness ratio Cr/CrN 0.81 to 0.15 results in the increase of hardness from 1275 HV to 1710 HV and Young's modulus from 260 GPa to 271 GPa.     

AlN/TiSiN纳米多层膜的微观组织和力学性能研究

采用TiSi复合靶和Al靶,用射频磁控溅射工艺沉积不同TiSiN层厚度的AlN/TiSiN纳米多层膜。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)和纳米压痕仪研究了不同TiSiN层厚度对AlN/TiSiN纳米多层膜的微观组织和力学性能的影响。结果表明,随着TiSiN层厚度的增加,AlN相的结晶程度先增加后降低,涂层的硬度先提高后降低,当TiSiN层厚度为0.5nm时具有最高的硬度和弹性模量。HRTEM观测可知,在TiSiN层厚度为0.5nm时,TiSiN层在AlN层的模板作用下呈密排六方结构,并与AlN层呈共格外延生长,薄膜的强化主要与共格外延生长结构有关。     

Influence of TiN-nanolayered insertions on microstructure and mechanical properties of TiSiN nanocomposite film

TiN nanolayers with different thicknesses were inserted in TiSiN nanocomposite film by magnetron-sputtering technique. The influences of TiN insertion nanolayers with different thicknesses on microstructure and mechanical properties of TiSiN film were investigated X-ray diffraction, high-resolution transmission electron microscopy, scanning electron microscopy, and nanoindentation techniques. When the TiN insertion layer thickness is <0.5 nm, TiN nanolayers can coordinate the misorientations between TiN nanocrystallites in adjacent TiSiN layers, leading to the transformation from the nanocomposite structure with TiN nanocrystallites encapsulated by SiN _x interfacial phase into columnar crystal structure, and disappearance of the strengthening effect from the nanocomposite structure. When the TiN insertion layer thickness increases to 1.0 nm, the film is strengthened with the epitaxial growth structures between TiSiN and TiN layers. As the TiN insertion layers further thicken, the hardness and elastic modulus evidently decrease, which can be attributed to the breakage of epitaxial growth structures between TiSiN and TiN layers.     

Effect of heat treatment on mechanical properties and microstructure of CrN/AlN multilayer coatings

Polycrystalline CrN/AlN multilayer coatings were deposited by RF magnetron sputtering on silicon (001) substrates. The bilayer periods of CrN/AlN were controlled from 4 nm to 20 nm by the use of shutters, which were adjusted by a programmable logic control (PLC). To evaluate the thermal stability, the films were annealed at 500 °C, 600 °C, 700 °C, 800 °C, and 850 °C, for 1 h in both vacuum and air environments. The phase transformation during thermal evolution was studied by X-ray diffraction (XRD). The microstructure of CrN/AlN multilayer coatings as-deposited and after annealing was observed by transmission electron microscopy (TEM). The hardness of as-deposited CrN/AlN coating with a period of 4 nm was 28.2 GPa, which was 60% higher than that predicted by the rule of mixtures. The hardness of CrN/AlN multilayer coatings annealed at 850 °C in vacuum remained similar to the as-deposited state, and the nano-layered structure still persisted. The thermal stability of CrN/AlN coatings was better than that of CrN coating. The hardness degradation ratio of CrN/AlN coating with modulation period of 4 nm was only 8.1% at 700 °C, which was superior to that of a simple CrN coating.     

Influence of the microstructure on the mechanical and tribological behavior of TiC/a-C nanocomposite coatings

The performance of protective thin films is clearly influenced by their microstructure. The objective of this work is to study the influence of the structure of TiC/a-C nanocomposite coatings with a-C contents ranging from ~ 0% to 100% on their mechanical and tribological properties measured by ultramicroindentation and pin-on-disks tests at ambient air, respectively. The microstructure evolves from a polycrystalline columnar structure consisting of TiC crystals to an amorphous and dense TiC/a-C nanocomposite structure when the amount of a-C is increased. The former samples show high hardness, moderate friction and high wear rates, while the latter ones show a decrease in hardness but an improvement in tribological performance. No apparent direct correlation is found between hardness and wear rate, which is controlled by the friction coefficient. These results are compared to the literature and explained according to the different film microstructures and chemical bonding nature. The film stress has also been measured at the macro and micro levels by the curvature and Williamson-Hall methods respectively. Other mechanical properties of the coating such as resilience and toughness were evaluated by estimating the H³/E?² and H/E? ratios and the percentage of elastic work (W_e). None of these parameters showed a tendency that could explain the observed tribological results, indicating that for self-lubricant nanocomposite systems this correlation is not so simple and that the assembly of different factors must be taken into account.     

Measurement of mechanical properties of multilayer coatings by nanoindentation

Abstract

Multilayer protective coatings of alternate aluminium and titanium diboride TiB₂ layers have been tested by nanoindentation to measure both hardness and Young's modulus values. The initial results show that the values obtained depend upon the depth of indentation. An alternative view is presented to show that by considering the percentage of each coating in contact with the indenter a single relationship between either hardness or Young's modulus and the amount of aluminium layer penetrated can be produced. This technique allows the influence of the percentage ceramic on the results obtained to be identified. Comparison of the nanoindentation results with three point bending tests show how the coating structure influences the results obtained.     

Influence of bi-layer period thickness on the residual stress, mechanical and tribological properties of nanolayered TiAlN/CrN multi-layer coatings

TiAlN/CrN nanoscale multi-layered coatings have been deposited using cathodic arc evaporation system. The coatings were deposited using one Ti₅₀Al₅₀ alloy target and one Cr target with a fixed target power in all the processes, while the bi-layer thickness was varied by various rotation speeds of the substrate holder in order to produce different nanoscale multi-layered period thickness. The texture structure, residual stress, and nanoscale multi-layer period thickness of the coatings were determined by X-ray diffraction using both Bragg-Brentano and glancing angle parallel beam geometries. Hardness and adhesion strength of the coatings were measured by Nano-indentation and Rockwell-C indentation methods, respectively. It has been found that the structural and mechanical properties of the films correlate with nano-scaled bi-layer thickness and crystalline texture. The maximum hardness of nano-scaled TiAlN/CrN multi-layered coatings was approximately 36 GPa with highest residual stress of −6.2 GPa, for a bi-layer thickness ranging from 6 to 12 nm.     

Effect of grain size on mechanical properties in CrAlN/SiNx multilayer coatings

Both CrAlN and SiN_x coatings were deposited sequentially by RF magnetron sputtering. During sputtering, thickness of SiN_x layer was set to be 1 nm, while that of CrAlN layer was controlled to be 4, 20, 40, 100, and 200 nm. According to XRD results, it was revealed that grain size of the CrAlN coatings increased from 3.6 nm to 24.2 nm with the increasing thickness. From HRTEM images, the variation on grain size was attributed to the amorphous SiN_x layer, which significantly retarded the continuous growth of CrAlN layer. Hardness of the CrAlN/SiN_x coatings with various bilayer thicknesses was measured by nanoindentation. The relationship between grain size and hardness could be interpreted by the Hall-Petch equation, and an improved hardness around 32 GPa was achieved.     

ZrN/TiSiN纳米多层膜的微观结构和力学性能研究

采用反应磁控溅射的方法,利用Zr靶与TiSi复合靶成功制备了不同TiSiN层厚度的ZrN/TiSiN纳米多层膜。利用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、扫描电子显微镜(SEM)和纳米压痕仪研究了不同TiSiN层厚度对ZrN/TiSiN纳米多层膜的微观结构和力学性能的影响。结果表明,ZrN/TiSiN纳米多层膜主要由面心立方的ZrN相组成,随着TiSiN层厚度的增加,纳米多层膜的结晶程度先增加后降低,其硬度和弹性模量也先升高后降低。当TiSiN层厚度为0.7nm时,纳米多层膜具有最高的硬度和弹性模量,分别为28.7和301.1GPa,远超过ZrN单层膜。ZrN/TiSiN纳米多层膜的强化效果可由交变应力场和模量差理论进行解释。     

Designing multilayer diamond like carbon coatings for improved mechanical properties

New multilayer coatings were produced by incorporating alternating soft and hard DLC layers enabled by varying the bias voltage during deposition process while maintaining a constant hard-to-soft layer thickness ratio.These coatings were deposited onto a Cr/Cr Cxgraded layer by closed field unbalanced magnetron sputtering(CFUBMS).The cross-sectional analysis of the coatings showed that the multilayer coatings possess sharp interfaces between the soft and hard layers with the hard to soft layer thickness ratio(1:1.33)constant in all the coatings.Raman analysis uncovered the increasing sp³character of the DLC coatings as a result of decreasing ID/IGratio and increasing full width at half maximum(FWHM)values of the G band peak induced supposedly by an increase in bias voltage during hard layer deposition.Nanoindentation tests showed an increase in hardness of the DLC coatings which can be correlated with the increase in the sp³content of the coatings as well as decreasing sp²-C cluster size,as calculated from the ID/IGratio.Furthermore,the coatings exhibited excellent plastic deformation resistance and adhesion strength upon microindentation and scratch testing,respectively.Although further investigations are required to assess coating durability,the multilayer design could offer the DLC coatings with a rare opportunity to combine the high hardness with damage resistance with a constant bilayer thickness and without the need to introduce complex multilayer system.     

Influence of modulation ratio on the structure and mechanical properties of TiB2/TiAlN multilayered coatings

TiB₂/TiAlN multilayered coatings with various modulation ratios (t_TiB2:t_TiAlN) were grown using radio-frequency magnetron sputtering at room temperature. Nanoindentation, tester for material surface properties, and XRD were used to investigate the influence of modulation ratio on microstructure and properties of the multilayers. All multilayers showed improved mechanical properties, compared with the average value of the monolithic TiB₂ and TiAlN coatings. The multilayer with modulation ratio of 5:2 displayed the highest hardness (36 GPa) and longest time to crack during wear. A marked layer structure with the strong mixture of TiAlN (111), AlN (111), and TiB₂ (001) textures with smaller grain sizes was responsible for the enhanced hardness.     

The effect of nanolayer thickness on the structure and properties of multilayer TiN/MoN coatings

The effect of nanolayer thickness on the structure and properties of nanocomposite multilayer TiN/MoN coatings is revealed. The multilayer (alternating) TiN/MoN coatings are prepared by the Arc-PVD method. The selected thickness of the nanolayers is 2, 10, 20, and 40 nm. The formation of two phases—TiN (fcc) and γ-Mo₂N—is found. The ratio of Ti and Mo concentrations varies with varying layer thickness. The maximum hardness value obtained for different thicknesses of the layers does not exceed 28–31 GPa. The stability of TiN/MoN during cutting and tribological tests is significantly higher than that of products with TiN coatings. The nanostructured multilayer coatings with layer thicknesses of 10 and 20 nm exhibit the lowest friction coefficient of 0.09–0.12.     

Influence of Ag thickness on electrical, optical and structural properties of nanocrystalline MoO3/Ag/ITO multilayer for optoelectronic applications

In this study, MoO₃/Ag/ITO/glass (MAI) nano-multilayer films were deposited by the thermal evaporation technique and then were annealed in air atmosphere at 200 °C for 1 h. The effects of Ag layer thickness on electrical, optical and structural properties of the MoO₃(45 nm)/Ag(5-20 nm)/ITO(45 nm)/glass nano-multilayer films were investigated. The sheet resistance decreased rapidly with increasing Ag thickness. Above a thickness of 10 nm, the sheet resistances became somewhat saturated to a value of 3(Ω/□). The highest transparency over the visible wavelength region of spectrum (85%) was obtained for 10 nm Ag layer thickness. Carrier mobility, carrier concentrations, transmittance and reflectance of the layers were measured. The allowed direct band-gap for an Ag thickness range 5-20 nm was estimated to be in the range 3.58-3.71 eV. The XRD pattern showed that the films were polycrystalline. X-ray diffraction has shown that Ag layer has a (111) predominant orientation when deposited. The figure of merit was calculated for MAI multilayer films. It has been found that the Ag layer thickness is a very important factor in controlling the electrical and optical properties of MAI multilayer films. The optimum thickness of the Ag layer for these films was determined. The results exhibit that the MAI transparent electrode is a good structure for use as the anode of optoelectronic devices.     

Mechanical and tribological properties of gradient a-C:H/Ti coatings

The unusual combination of high hardness and very low friction coefficient are the most attractive tribological parameters of DLC (diamond-like carbon) layers. However, their usability is strongly restricted by the limited thickness due to high residual stress. The main goal of the presented work was to obtain thick, wear resistant and well adherent DLC layers while keeping their perfect friction parameters. As a proposed solution a Ti-Ti _x C _y gradient layer was manufactured as the adhesion improving interlayer followed by a thick diamond-like carbon film. This kind of combination seems to be very promising for many applications, where dry friction conditions for highly loaded elements can be observed. Both layers were obtained in one process using a hybrid deposition system combining PVD and CVD techniques in one reaction chamber. The investigation was performed on nitrided samples made from X53CrMnNiN21-9 valve steel. Structural features, surface topography, tribological and mechanical properties of manufactured layers were evaluated. The results of the investigation confirmed that the presented deposition technique makes it possible to manufacture thick and well adherent carbon layers with high hardness and very good tribological parameters. Preliminary investigation results prove the possibility of application of presented technology in automotive industry.     

Intrinsic stresses and stress relaxation in TiN/Ag multilayer coatings during thermal cycling

Morphology, structure and thermal behavior of magnetron sputtered TiN/Ag multilayer thin films deposited at 150 °C with a bilayer thickness Λ in the range of 75-600 nm are characterized. The films are thermally cycled and the relationship between bilayer thickness Λ, film structure and stress development is analyzed. The results indicate that the residual stresses in the as-deposited films and the behavior during heating are determined by the morphology and the mechanical properties of the Ag interlayers. The increasing crystallite size of Ag with increasing Λ and the initial porosity in the Ag layer are the reason for significant changes in the stress-temperature behavior. While coatings with Λ = 75 nm behave like a single-phase coating up to 380 °C, coatings with higher Λ show a different behavior when exceeding the deposition temperature, which is related to the densification of the Ag layers. During cooling, all coatings exhibit linear thermo-elastic behavior, where the slope of the stress-temperature curves also depends on Λ.     

Enhancement of mechanical and tribological properties in AISI D3 steel substrates by using a non-isostructural CrN/AlN multilayer coating

Enhancement of mechanical and tribological properties on AISI D3 steel surfaces coated with CrN/AlN multilayer systems deposited in various bilayer periods (Λ) via magnetron sputtering has been studied in this work exhaustively. The coatings were characterized in terms of structural, chemical, morphological, mechanical and tribological properties by X-ray diffraction (XRD), electron dispersive spectrograph, atomic force microscopy, scanning and transmission electron microscopy, nanoindentation, pin-on-disc and scratch tests. The failure mode mechanisms were observed via optical microscopy. Results from X-ray diffraction analysis revealed that the crystal structure of CrN/AlN multilayer coatings has a NaCl-type lattice structure and hexagonal structure (wurtzite-type) for CrN and AlN, respectively, i.e., made was non-isostructural multilayers. An enhancement of both hardness and elastic modulus up to 28 GPa and 280 GPa, respectively, was observed as the bilayer periods (Λ) in the coatings were decreased. The sample with a bilayer period (Λ) of 60 nm and bilayer number n  =  50 showed the lowest friction coefficient (∼0.18) and the highest critical load (43 N), corresponding to 2.2 and 1.6 times better than those values for the coating deposited with n = 1, respectively. The best behavior was obtained when the bilayer period (Λ) is 60 nm (n = 50), giving the highest hardness 28 GPa and elastic modulus of 280 GPa, the lowest friction coefficient (∼0.18) and the highest critical load of 43 N. These results indicate an enhancement of mechanical, tribological and adhesion properties, comparing to the CrN/AlN multilayer systems with 1 bilayer at 28%, 21%, 40%, and 30%, respectively. This enhancement in hardness and toughness for multilayer coatings could be attributed to the different mechanisms for layer formation with nanometric thickness such as the Hall–Petch effect and the number of interfaces that act as obstacles for the crack deflection and dissipation of crack energy.     

弧流对Ti—Si—C膜层结构与性能的影响

电弧离子镀沉积膜层具有放电温度高、离化率高和沉积速率快等特点,可以在较低温度下促进Si—C成键,是获得含Si—C键膜层的一种经济实惠的方法。本文使用Ti—Si合金靶,在Ar和C₂H₂气体环境下,在铝合金衬底上制备了Ti—Si—C膜层,并分析和研究了不同弧流下沉积膜层的相组成、磨损和腐蚀性能。结果显示,不同弧流下沉积的膜层是由B1型TiC相、立方结构的SiC相和金属Ti相组成的复合结构;大弧流由于放电温度高,有利于膜层中Si—C键的形成.弧流增加,靶材蒸发速率加快,沉积膜层的厚度增加,同时,由于靶材附近单位时间内气化和离化的Si和Ti数量增加,沉积膜层中Si和Ti含量和增加而C含量降低.弧流增加,膜层中碳化物总含量减少,造成膜层摩擦系数逐渐增加而耐磨性降低,但膜层的耐腐蚀性能增加.适当弧流下的沉积膜层可获得优异的磨损和腐蚀综合性能.