Mechanical and tribological properties of multilayered TiSiN/CrN coatings synthesized by a cathodic arc deposition process

The monolayered TiSiN and multilayered TiSiN/CrN were synthesized by cathodic arc evaporation. The Ti/Si (80/20 at.%) and chromium targets were used as the cathodic materials. With the different I_[TiSi]/I_[Cr] cathode current ratios of 1.8, 1.0, and 0.55, the multilayered TiSiN/CrN coatings possessed different multilayer periods (Λ) of 8.3 nm, 6.2 nm, and 4.2 nm. From XRD and TEM analyses, both the monolayered TiSiN and multilayered TiSiN/CrN revealed a typical columnar structure and B1-NaCl crystalline, no peaks of crystalline Si₃N₄ were detected. Among the multilayered TiSiN/CrN coatings, the multilayered coating with Λ = 8.3 nm possessed higher hardness of 37 ± 2 GPa, higher elastic modulus of 396 ± 20 GPa and the lower residual stress of − 1.60 GPa than the monolayered (Ti_0.39Si_0.07)N_0.54 coating(− 7.25 GPa). Due to the higher Cr/(Ti +Cr + Si) atomic ratio, the multilayered TiSiN/CrN with Λ = 5.5 nm possessed the lowest friction coefficient. But the lowest of wear rate was obtained by the multilayered TiSiN/CrN with Λ = 8.3 nm, because of higher H³/E^?2 ratio of 0.323 GPa. The monolayered TiSiN possessed the highest wear rate of 2.87 μm²/min. Therefore, the mechanical and tribological property can be improved by the design of multilayered coating.     

过滤电弧沉积的TiN/TiCrN/CrN/CrTiN多层膜

用过滤电弧技术在高速钢表面沉积了TiN／TiCrN／CrN／CrTiN多层膜，用扫描电镜(SEM)观察了截面和断口形貌及划痕后的形貌。使用俄歇电子谱仪进行剥层成分分析，用纳米压痕仪测试了多层膜和单层膜的显微硬度和弹性模量。结果表明，在调制周期大于l00nm时，多层膜的显微硬度符合Ha11—Petch关系，在80nm时，则脱离线性关系。划痕法测试多层膜的结合力达到80N。     

Effect of bilayer period on properties of Cr/CrN multilayer coatings produced by laser ablation

Multilayers of alternate Cr/CrN coatings deposited on AISI 301 steel by a pulsed Nd:YAG laser have been tested by microindentation to measure both hardness and Young's modulus. Critical load L_C has been determined by scratch test. The total thickness of multilayers was 1 µm, and the bilayer period Λ varied from between 60 nm and 1000 nm. TEM and EDS techniques were used for investigating and analyzing the microstructure of the multilayers. The results of these measurements show that the mechanical properties of Cr/CrN multilayers depend on the bilayer period. The maximum improvement in performance over a single layer of CrN has been found to be Λ at 250 nm, particularly in terms of critical load and Young's modulus.     

Synthesis and characterization of multilayer CrN/ZrN coatings

In this study, multilayer CrN/ZrN coatings with various bi-layer periods (δ) were deposited by closed-field unbalanced magnetron sputtering and their compositions, crystalline structures and morphologies were characterized by auger electron spectroscopy (AES), X-ray diffraction (XRD) and transmission electron microscopy (TEM). Additionally, the mechanical properties of the coatings were characterized by nano-indentation and wear tests. The XRD results showed that the diffraction peak of multilayer CrN/ZrN coatings is observable between the CrN (111) and the ZrN (111). This peak has a strong tendency to increase the intensity and sharpen the width as the substrate rotation speed increases, indicating that the grain size of the multilayer CrN/ZrN coatings gradually increases. The hardness of films was dependent on the bi-layer period (δ), and the maximum hardness and elastic modulus were approximately 31.8 GPa and 321.5GPa, respectively. Moreover, the results of the wear tests showed that the multilayer CrN/ZrN coatings exhibited greatly improved wear resistance compared to the monolithic CrN coatings.     

Multilayered gradient CrN/ZrN coatings synthesized by magnetron sputtering

The multilayer gradient CrN/ZrN coatings were synthesized by a dual cathode DC magnetron sputtering.The influence of different species of reaction gases and partial pressures on structure and mechanical properties was investigated using XRD, AES, XPS, and nanoindentation. The results show that N2-NH3 mixture process gas is of benefit to the synthesis of superhard multilayered gradient CrN/ZrN coatings. The presence of the preferred orientations of CrN(111), (200) and ZrN (111), (220) in the structure is a main reason for superhardness of multilayered gradient coatings.     

High temperature tribological characterisation of TiAlSiN coatings produced by cathodic arc evaporation

This study reports on the wear properties at medium-high temperatures of TiAlSiN films deposited by cathodic arc evaporation on hot work steel substrates. The chemical composition and microstructure of the coatings were characterised by glow discharge optical emission spectroscopy, scanning electron microscopy and X-ray diffraction. The mechanical properties, i.e. hardness and elastic modulus were evaluated by nanoindentation, and the adhesion of the coatings was tested by scratch tests. Coatings with stoichiometries of Ti_0.31Al_0.1Si_0.06N_0.53 and Ti_0.23Al_0.12Si_0.09N_0.55 exhibit microstructures consisting of solid solutions of (Ti,Al,Si)N, where Al and Si replace Ti atoms. These films show high hardness and good adhesion strength to the hot work steels. Conversely, coatings with a stoichiometry of Ti_0.09Al_0.34Si_0.02N_0.55 show a wurtzite-like microstructure, low hardness and poor adhesion strength.The wear rates of the coatings were investigated by ball-on-disc experiments at room temperature, 200 °C, 400 °C and 600 °C, using alumina balls as counter surfaces. At room temperature, the films show wear rates of the same order of magnitude of TiN and TiAlN coatings. On the other hand, the wear rates of solid solution (Ti,Al,Si)N coatings measured at 200, and 400 °C are one order of magnitude smaller than those measured at room temperature due to the formation of oxide-containing tribofilms on the wear tracks. At 600 °C the wear rates increase but still keep smaller than those measured at room temperature, although this effect can be influenced by the softening of the steel substrates by over-tempering. EDS analyses revealed that, between 200 °C and 400 °C, the oxidation of the coating occurs only at the contact zone between the film and the counterpart body due to the sliding process.     

深振荡磁控溅射复合沉积CrN/TiN超晶格涂层的摩擦学性能

研究了IN718高温合金、WC-6%Co硬质合金和Si(100)基体上深振荡磁控溅射复合沉积CrN/TiN超晶格涂层的摩擦学性能。研究表明,涂层的生长对基体的类型没有选择性。随着基体硬度的升高,划痕结合力失效临界载荷增大,涂层结合力失效机制由翘曲失效转变为基体/涂层协同变形,未发现涂层的剥落失效。载荷为2N时,磨损机制由磨粒磨损和氧化磨损转变为轻微磨粒磨损。载荷为4 N时,IN 718基体上涂层的磨损机制为严重的氧化磨损,WC-6%Co基体上的涂层的磨损机制为磨粒磨损和氧化磨损,氧化物的产生、堆积和转移导致摩擦系数的波动。     

Structure and properties of cathodic vacuum arc deposited NbN and NbN-based multi-component and multi-layer coatings

Binary Nb-N coatings, ternary Ti-Nb-N and Zr-Nb-N, and multi-layer TiN/NbN coatings consisting of up to 100 alternating TiN and NbN layers, were deposited onto WC-Co substrates, using two different vacuum arc deposition (VAD) systems: with and without magnetic guiding of the metal plasma flow. Binary Nb-N coatings were fabricated by deposition of metal plasma produced by a Nb cathode in a background of reactive nitrogen gas at different pressures, P. Ternary coatings were fabricated at co-deposition of plasmas originating from two different cathode materials. Multilayer coatings were fabricated by alternatively depositing plasmas of Ti and Nb in reactive nitrogen gas. The crystalline coating structure, phase composition, hardness and critical load for coating failure were studied.For binary Nb-N coatings fabricated using both deposition systems, the phase composition, the Vickers hardness, HV, and the critical load strongly depended on the deposition pressure. Using VAD with magnetic plasma guiding, the highest HV of ∼ 42 GPa was measured for coatings deposited at low nitrogen pressure. These coatings contained a hexagonal β-Nb₂N phase and had a relatively low critical load. The highest critical load and HV ∼ 38 GPa were obtained for coatings consisted of a single phase NaCl-type cubic δ-NbN structure, deposited at a higher nitrogen pressure. The structure and properties of Nb-N coatings deposited using VAD without magnetic plasma guiding had a similar correlation with the deposition pressure, however, their hardness values were lower.Ternary Ti-Nb-N and Zr-Nb-N coatings fabricated by both deposition processes had a single phase cubic NaCl-type structure and the hardness higher than that of the binary nitrides TiN, ZrN and NbN. The hardest coatings, HV ∼ 51.5 Pa, deposited with magnetic plasma guiding had a single-phase cubic δ-(Ti,Nb)N structure and a Ti:Nb ratio of ∼ 50:50 (at.%).Multilayer coatings TiN/NbN consisting of 20-40 alternating TiN and NbN layers with total thickness of 4-5 μm increased the life time of cemented carbide cutting inserts at turning tough Ni-base alloys by 2-7 times relative to uncoated cutting tools, while conventional vacuum arc deposited TiN coatings were not effective in machining of these alloys.     

Influence of bilayer period and thickness ratio on the mechanical and tribological properties of CrSiN/TiAlN multilayer coatings

Nanostructured CrSiN/TiAlN multilayer coatings were deposited by a bipolar asymmetric reactive pulsed DC magnetron sputtering system. The thickness ratio of CrSiN to TiAlN layers was fixed at 1:1. The bilayer periods of the coatings were controlled to be from 6 to 40 nm. Furthermore, two CrSiN/TiAlN multilayer coatings with the same bilayer period (20 nm) but different CrSiN/TiAlN thickness ratios (2:8 and 8:2) were also deposited to explore the influence of thickness ratio on the mechanical properties of the multilayer coatings. The crystalline structures of the coatings were determined by a glancing angle X-ray diffractometer. The microstructures of thin films were examined by a scanning electron microscopy and a transmission electron microscopy, respectively. A nanoindenter, a micro Vickers hardness tester, and a pin-on-disk wear tester were used to evaluate the hardness, the toughness and the tribological properties of the thin films, respectively. The maximum hardness of the multilayers was obtained when the bilayer period was at 10 nm for the coating with the same thickness ratio of CrSiN to TiAlN layers (1:1). Meanwhile, the thickness ratio of CrSiN to TiAlN layer had great influence on the hardness and the toughness properties of the multilayer coatings. The hardness and the toughness of the CrSiN/TiAlN multilayer coatings increased as the individual TiAlN layer thickness increased.     

Microstructure, mechanical and tribological properties of CrN/W2N multilayer films deposited by DC magnetron sputtering

CrN/W₂N multilayer films with various bilayer periods of 15-85 nm were deposited on high speed steel (W18Cr4V) substrates by means of DC closed field unbalanced magnetron sputtering. The morphology and microstructure of the multilayer films were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM). The mechanical and tribological properties were evaluated using a nanoindentor, Rockwell and scratch tests and a conventional ball-on-disk tribometer, respectively. There were some transverse grains at the layer interface and the interface between the CrN and W₂N layers was not so sharp owing to atom diffusion through the interface. In the bilayer period range, the microhardness, elastic modulus and adhesive strength of the CrN/W₂N multilayer films increased with the decrease of bilayer period. The CrN/W₂N multilayer film with a bilayer period of 15 nm showed the highest hardness (29.2 GPa), elastic modulus (376 GPa) and best adhesion strength, it also had the highest wear resistance and lowest friction coefficient.     

Microstructure and tribological properties of CrN and CrSiCN coatings

Three CrN based coatings were deposited on 17-4PH precipitation hardening stainless steel substrate using plasma enhanced magnetron sputtering (PEMS) technique. The three coatings evaluated in this study assumed the nominal compositions of Cr_0.68N_0.32 (sample CrN), Cr_0.55Si_0.013C_0.14N_0.3 (sample CrSiCN-1), and Cr_0.43Si_0.034C_0.25N_0.29 (Sample CrSiCN-2)_. The microstructure, mechanical properties and wear and erosion resistance of the coatings were evaluated to examine the effect of Si and C additions to CrN. The results indicated that with the incorporation of Si and C, the microstructure transformed from hexagonal Cr₂N (for CrN coating) to B1 structure containing crystalline Si₃N₄ (for CrSiCN-2). The initial addition of Si (1.3 at.%) and C resulted in increase of hardness (H), Young's modulus (E) and the ratio of H³/E². With further increase in Si (3.4 at.%) and C, the hardness and Young's modulus decreased. The coefficient of friction was observed to decrease with the addition of Si and C, irrespective of microstructure changes. The combination of reduced coefficient of friction and microstructure modifications has resulted in improved wear resistance for sample CrSiCN-2 (with a wear rate ∼ 60% lower than CrN). The erosion resistance test results showed brittle erosion characteristics for samples CrN and CrSiCN-1 where erosion rate increased with erodent impingement angle and reached the highest rate at 75° and 90°, respectively. CrSiCN-2 coating, while exhibiting higher erosion rate at low impingement angle, demonstrated reduced erosion rate at higher angle due to the ductile nature of the coating under erosion test condition.     

Preparation of TiAlN/ZrN and TiCrN/ZrN multilayers by RF magnetron sputtering

Titanium-based nitride coatings on cutting tools, press molds and dies can be used to prolong their life cycle because of their superior corrosion and oxidation resistance. TiAlN/ZrN and TiCrN/ZrN multilayer coatings were prepared by RF magnetron sputtering, and their microstructural evolution and corrosion resistance during heat treatment were investigated. The TiAlN/ZrN and TiCrN/ZrN multilayer coatings are degraded by heating up to 600 °C with the formation of oxides particles on the surface. During the heat treatment, the TiCrN/ZrN and TiAlN/ZrN multilayer coatings show the lowest corrosion current density and the highest polarization resistance at temperature range of 400–500 °C. Consequently, the TiAlN/ZrN and TiCrN/ZrN multilayer coatings show good corrosion resistance at temperature range of 400–500 °C during heating.     

Tribological behavior of CrN/WN multilayer coatings grown by ion-beam assisted deposition

CrN monolayer coating and CrN/WN multilayer coatings were deposited on the silicon (100) substrate by ion-beam assisted deposition process. The bilayer period of these coatings was controlled at 8 nm and 30 nm. The cross-sectional morphology of nanoscaled multilayer coatings was characterized by scanning electron microscopy and transmission electron microscopy. The wear resistance of CrN/WN multilayer coatings and CrN monolayer coating was investigated using a pin-on-disc tribometer. The surface roughness (Ra) of the coatings was evaluated by atomic force microscopy, and that of CrN and WN monolayer coating was 6.7 and 5.9 nm, respectively. The employment of multilayer configuration in CrN/WN coating with bilayer period of 8 nm and 30 nm effectively reduced the surface roughness down to 1.9 and 2.2 nm, respectively. The friction coefficient of CrN monolayer coating and CrN/WN multilayer film with a bilayer period of 30 nm was 0.63 and 0.31, respectively. Owing to the high hardness/elastic modulus ratio, as well as the dense structure and the smooth surface roughness, the CrN/WN multilayer coatings exhibited better wear resistance in the consideration of friction coefficient and the worn surface morphology.     

分离靶电弧离子镀制备TiN/TiAlN多层薄膜的微观结构和力学性能(英文)

采用分离靶电弧离子镀制备TiN/TiAlN多层薄膜。为了减少大颗粒的不利影响,利用直线型磁过滤方法来减少低熔点铝靶产生的大颗粒。结果表明,没有过滤的钛靶和磁过滤的铝靶等离子体到达基体的输出量在相同的数量级,同时,采用该方法制备的薄膜中的大颗粒数目是文献中报道的合金靶制备的薄膜大颗粒数目的1/10～1/3。Al元素的添加引起薄膜在(200)晶面的峰值降低,而在(111)和(220)晶面的峰值增强。TiN/TiAlN多层薄膜的最大硬度为HV2495,薄膜的硬度增强符合混合法则,结合力达75 N。     

Cathodic arc plasma deposition of nano-multilayered ZrN/AlSiN thin films

Thin films of ZrN/AlSiN were deposited on SKD 11 tool steel substrate using Zr and AlSi cathodes in an Ar/N₂ gas mixture in a cathodic arc plasma deposition system. The influence of the AlSi cathode arc current and the substrate bias voltage on the mechanical and structural properties of the films was investigated. X-ray diffraction, electron probe micro-analysis, high resolution transmission electron microscopy, nanoindentation and profilometry were used to characterize the films. The ZrN/AlSiN thin films had a multilayered structure by rotating the substrate in which nano-crystalline ZrN layers alternated with amorphous AlSiN layers. The hardness of the films increased as the AlSi cathode arc current was raised from 35 to 40 A, and then decreased with a further increase of the current. The hardness of the films increased with the increase of the bias voltage from − 50 to − 100 V. Further increase in the bias voltage decreased the hardness. The films exhibited a maximum hardness of 38 GPa. With the increase of bias voltage, the residual stress of the films correlated well with the hardness.     

Comparison of the tribological and antimicrobial properties of CrN/Ag, ZrN/Ag, TiN/Ag, and TiN/Cu nanocomposite coatings

Nanocomposite coatings including CrN/Ag, ZrN/Ag, TiN/Ag and TiN/Cu with varying silver or copper contents were produced by co-deposition in a dual pulsed magnetron sputtering system. The compositions and structures of the coatings were characterised using energy dispersive X-ray spectroscopy (EDX) and scanning electron microscopy (SEM), and the physical and tribological properties were assessed by means of nanoindentation and thrust washer wear testing. Although increasing silver or copper content provided a reduction in the coefficient of friction, this was accompanied by reductions in hardness for all the coatings and wear resistance for some of the coatings. Zones of inhibition were used to determine the extent of silver ion release from the coating surfaces, and a NBT (nitro-blue tetrazolium) redox dye was used to determine the antimicrobial effectiveness of the coatings following incubation. The microorganisms tested were Pseudomonas aeruginosa and Staphylococcus aureus. For the NBT assays, significant reductions in the number of viable cells were observed with increasing Ag or Cu content, compared to the ‘pure’ nitride surfaces. Whilst no zones of inhibition were observed for S. aureus, on any of the surfaces, the diameter of the ‘kill’ zones generally increased with increasing silver content for P. aeruginosa.     

Improvement of the tribological behaviour of PVD nanostratified TiN/CrN coatings — An explanation

A hard TiN/CrN multilayered coating, consisting of alternating nanometer scale TiN and CrN layers (bilayer period of 40 nm), was deposited by arc evaporation process on M2 tool steel. Monolayered TiN and CrN are also deposited in the same conditions, and used as references. In order to get a better understanding of the tribological behaviour of coated parts, two types of experiments were performed. The dry-sliding wear resistance was evaluated with a ball-on-disk tribometer, while surface fatigue resistance was determined by a cyclic multi-impact test. The architecture of layers is measured by XRD and observed by TEM. The residual stress field was characterised using XRD and the sin²ψ method at a synchrotron radiation facility.All coatings present a columnar microstructure. TiN demonstrated better wear resistance than CrN and this characteristic is still increased two times by using the nanostratified coating. In the same way, the results of surface oligo-cyclic fatigue test confirm the high performance of the nanostructured coating with respect to the monolayered ones. The differences in mechanical properties of coatings evaluated through nanoindentation measurements do not lead to a direct correlation with the tribological results, and therefore cannot explain such differences. Moreover, a microscopic analysis of the samples after both tribological tests reveals two opposite cracking mechanisms. Monolayered TiN and CrN are subjected to a transversal crack propagation until the peeling of the coating, whereas the multilayered coating only undergoes cohesive cracks deviated in the TiN/CrN interface zones. Both opposite behaviours are the consequence of the distribution of stresses along the thickness of the film.     

过滤阴极真空电弧制备非晶金刚石红外保护膜

采用过滤阴极真空电弧技术,通过施加不同衬底偏压制备了非晶金刚石薄膜.利用纳米压痕仪和光谱椭偏仪测试薄膜的力学性能和光学性能,利用KLA-Tencor台阶仪测试硅衬底在薄膜沉积前后的曲率半径,并根据Stoney方程计算薄膜应力,利用可见光拉曼光谱和电子能量损耗谱研究了薄膜的微结构.实验表明:当衬底负偏压为80 V时,薄膜的硬度、弹性模量、光学带隙和折射率均达到最大值,随着偏压的升高或降低,各参量分别降低;此时,薄膜的sp3杂化含量最高,斜坡系数却最小;在宽红外波段范围内,薄膜的消光系数趋近于零,即红外透明;另外,薄膜具有接近金刚石的高硬度和高模量,并且其微结构以及光学和力学性能可调,因此是一种优异的红外光学窗口增透保护薄膜材料.     

Mechanical and tribological properties of CrN/Ag and CrSiN/Ag nanoscale multilayers

This paper presents a concept of combining hard CrN (or CrSiN) and soft Ag lubricating materials in a nanoscale multilayer structure. The CrN/Ag and CrSiN/Ag multilayers are synthesized by reactive direct current (DC) magnetron sputtering techniques. The thickness of the Ag nanolayer in the multilayers is fixed to 4 nm while that of CrN and CrSiN nanolayers vary from 4 to 20 nm. The nitride layer effects on the mechanical and tribological properties of the multilayers have been investigated. Different mechanisms of the adhesion failure have been observed on the multilayer surfaces, depending on the nitride nanolayer types and their thicknesses. The CrSiN/Ag films exhibit poor adhesion whereas CrN/Ag multilayers demonstrate very good adhesion to AISI M2 steel substrates. The study of friction behaviors of the CrN/Ag multilayers against 100Cr6 steel balls reveals that the multilayers have low friction coefficients in comparison with that of a CrN single layer. The decrease of friction coefficients is related to the presence of the solid lubricant (Ag) nanolayer in the coatings.