Effects of nitrogen ion implantation and implantation energy on surface properties and adhesion strength of TiN films deposited on aluminum by magnetron sputtering

The performance of tribological coatings depends greatly on the adhesion strength between the coatings and substrates. In this work, we investigated the influence of the ion implantation energy of nitrogen on the adhesion and surface properties of TiN deposited on aluminum substrate. Aluminum samples were implanted with 15 keV, 30 keV and 40 keV nitrogen ions before TiN films were deposited using magnetron sputtering in a custom-designed multi-functional ion implanter. The adhesion properties of the implanted TiN films were assessed using nano-scratch tests and were observed to vary with the nitrogen ion implantation energy. Our frictional test results show that an appropriate ion implantation energy and dose can improve the frictional behavior of TiN films deposited on aluminum.     

Deposition,structure and hardness of Ti–Cu–N hard films prepared by pulse biased arc ion plating

In this work, Ti–Cu–N hard nanocomposite films were deposited on 304 stainless steel (SS) substrate by using pulse biased arc ion plating system with Ti–Cu alloy target. The effects of negative substrate pulse bias voltages on chemical composition, structure, morphology and mechanical properties were investigated. The composition and structure of these films was found to be dependent on the pulse bias, whereas the pulse biases put little influence on hardness of these films. The XPS spectra of Cu 2p showed that obtained peak values correspond to pure metallic Cu. Cu content in Ti–Cu–N nanocomposite films changed with pulse bias voltage. In addition, X-ray diffraction analysis showed that a pronounced TiN (111) texture is observed under low pulse bias voltage while it changed to TiN (220) orientation under high pulse bias voltage. Surface roughness of the Ti–Cu–N nanocomposite films achieved to the minimum value of 0.11 μm with the negative pulse bias voltage of −600 V. The average grain size of TiN was less than 17 nm. The mechanical properties of Ti–Cu–N hard films investigated by nanoindentation revealed that the hardness was about 22–24 GPa and the hardness enhancement was not obtained.     

Deposition,structure and hardness of Ti–Cu–N hard films prepared by pulse biased arc ion plating

In this work, Ti–Cu–N hard nanocomposite films were deposited on 304 stainless steel (SS) substrate by using pulse biased arc ion plating system with Ti–Cu alloy target. The effects of negative substrate pulse bias voltages on chemical composition, structure, morphology and mechanical properties were investigated. The composition and structure of these films was found to be dependent on the pulse bias, whereas the pulse biases put little influence on hardness of these films. The XPS spectra of Cu 2p showed that obtained peak values correspond to pure metallic Cu. Cu content in Ti–Cu–N nanocomposite films changed with pulse bias voltage. In addition, X-ray diffraction analysis showed that a pronounced TiN (111) texture is observed under low pulse bias voltage while it changed to TiN (220) orientation under high pulse bias voltage. Surface roughness of the Ti–Cu–N nanocomposite films achieved to the minimum value of 0.11 μm with the negative pulse bias voltage of ?600 V. The average grain size of TiN was less than 17 nm. The mechanical properties of Ti–Cu–N hard films investigated by nanoindentation revealed that the hardness was about 22–24 GPa and the hardness enhancement was not obtained.     

Influence of negative voltage on the structure and properties of DLC films deposited on NiTi alloys by PBII

Diamond-like carbon (DLC) films have been successfully deposited on Ti-50.8 at.%Ni using plasma based ion implantation (PBII) technique. The influences of the pulsed negative bias voltage applied to the substrate from 12 kV to 40 kV on the structure, nano-indentation hardness and Young’s modulus are investigated by the X-ray photoelectron spectroscopy (XPS) and nano-indentation technique. The results show that C 1s peak depends heavily on the bias voltage. With the increase of bias voltage, the ratio of sp²/sp³ first decreases, reaching a minimum value at 20 kV, and then increases. The DLC coating deposited at 20 kV shows the highest hardness and elastic modulus values as a result of lower sp²/sp³ ratio. The corrosion resistance of specimen deposited under 20 kV is superior to uncoated NiTi alloy and slightly better than those of the other samples deposited at 12 kV, 30 kV and 40 kV.     

Influence of Substrate Negative Bias on Structure and Properties of TiN Coatings Prepared by Hybrid HIPIMS Method

TiN coatings were deposited using a hybrid home-made high power impulse magnetron sputtering(HIPIMS)technique at room temperature.The effects of substrate negative bias voltage on the deposition rate,composition,crystal structure,surface morphology,microstructure and mechanical properties were investigated.The results revealed that with the increase in bias voltage from-50 to-400 V,TiN coatings exhibited a trend of densification and the crystal structure gradually evolved from(111) orientation to(200)orientation.The growth rate decreased from about 12.2 nm to 7.8 nm per minute with the coating densification.When the bias voltage was-300 V,the minimum surface roughness value of 10.1 nm was obtained,and the hardness and Young's modulus of TiN coatings reached the maximum value of 17.4 GPa and 263.8 GPa,respectively.Meanwhile,the highest adhesion of 59 N was obtained between coating and substrate.     

Influence of bias voltages on the structure and wear properties of TiSiN coating synthesized by cathodic arc plasma evaporation

Nanocomposite TiSiN films have been deposited on M2 tool steel substrates using TiSi alloy as target by a dual cathodic arc plasma deposition (CAPD) system. The influences of bias voltages on the microstructure, mechanical and tribological properties of the films were investigated. Scanning electron microscopy, transmission electron microscopy, X-ray diffraction techniques were employed to analyse the microstructure, grain size and residual stress. Nano-indentation and tribometer testers were used to measure the mechanical and tribological properties of nanocomposite TiSiN thin films. The results showed that the hardness of the films ranged from 25 to 37 GPa, which were higher than that of TiN (21 GPa). The coefficient of friction of the TiSiN thin films was more stable but was higher than that of TiN when wear against both Cr steel and WC-Co ball, respectively. When encountered with both Cr steel and WC-Co ball of the counter ball, the tribological mechanisms of TiSiN thin films are adhesive and abrasion wears, respectively. It has been found that the microstructure, mechanical and wear properties of the films were correlated to bias voltage, grain size, and amorphous Si₃N₄ nanocomposite formed in film structure, resulting in a superhard TiSiN coating.     

多元氮化物薄膜及其沉积工艺对NiTi记忆合金性能和组织的影响

采用真空阴极电弧沉积技术,在NiTi记忆合金表面沉积了TiAlBN和TiAlCrFeSiBN多元膜和TiN薄膜,研究了薄膜成份及沉积工艺对NiTi合金性能和组织的影响.结果表明,在NiTi合金表面沉积TiAlBN和TiAlCrFeSiBN多元膜和TiN薄膜均可降低合金在Hank溶液中的Ni溶出速率,其中多元膜的Ni溶出速率最小;提高偏压对沉积了TiAlBN多元膜的NiTi合金的Ni溶出速率无明显影响,但使沉积了TiAlCrFeSiBN膜的NiTi合金的Ni溶出速率降低.在TiAlBN和TiAlCrFeSiBN多元膜表面存在较多细小的钛滴和孔隙,钛滴与薄膜基体之间的融合良好;在TiN薄膜表面存在一些大钛滴和孔隙,钛滴与薄膜基体之间的融合不好.镀膜后,NiTi基体的加热相变点移向低温区,其幅度与薄膜成份及沉积工艺有关,提高偏压使沉积了两种多元膜的NiTi基体的相变点移动幅度增大,但却使沉积了TiN膜的NiTi基体的相变点的移动幅度减小.镀膜过程均使NiTi中的M体尺寸增大.     

Microstructure and mechanical properties of CrAlN coatings deposited by modified ion beam enhanced magnetron sputtering on AISI H13 steel

CrAlN coatings were deposited on silicon and AISI H13 steel substrates using a modified ion beam enhanced magnetron sputtering system. At the modified ion beam bombardment, the effects of bias voltage and Al/(Cr + Al) ratio on microstructure and mechanical properties of the coatings were studied. The X-ray diffraction data showed that all CrAlN coatings were crystallized in the cubic NaCl B1 structure, showing the (111), (200), and (220) preferential orientation. It is noted that the (111) diffraction peak intensity decreased and the peaks broadened as the bias voltage increased at the same ratio of Al/Cr targets power, which is attributed to the variation in the grain size and microstrain. The microstructure observation of the coatings by field emission scanning electron microscopy cross-section morphology shows that the columnar grain became more compact and dense with increasing substrate bias voltage and Al concentration. At a substrate bias voltage of −120 V and a Al/(Cr + Al) ratio of 40%, the coating had the highest hardness (33.8 GPa) and excellent adhesion to the substrate.     

Structure, mechanical and tribological properties of diamond-like carbon films on aluminum alloy by arc ion plating

The low hardness and poor tribological performance of aluminum alloys restrict their engineering applications. However, protective hard films deposited on aluminum alloys are believed to be effective for overcoming their poor wear properties. In this paper, diamond-like carbon (DLC) films as hard protective film were deposited on 2024 aluminum alloy by arc ion plating. The dependence of the chemical state and microstructure of the films on substrate bias voltage was analyzed by X-ray photoelectron spectroscopy and Raman spectroscopy. The mechanical and tribological properties of the DLC films deposited on aluminum alloy were investigated by nanoindentation and ball-on-disk tribotester, respectively. The results show that the deposited DLC films were very well-adhered to the aluminum alloy substrate, with no cracks or delamination being observed. A maximum sp³ content of about 37% was obtained at −100 V substrate bias, resulting in a hardness of 30 GPa and elastic modulus of 280 GPa. Thus, the surface hardness and wear resistance of 2024 aluminum alloy can be significantly improved by applying a protective DLC film coating. The DLC-coated aluminum alloy showed a stable and relatively low friction coefficient, as well as narrower and shallower wear tracks in comparison with the uncoated aluminum alloy.     

Bias effects on the tribological behavior of cathodic arc evaporated CrTiAlN coatings on AISI 304 stainless steel

In this study, CrTiAlN coatings were deposited on AISI 304 stainless steel by cathodic arc evaporation under a systematic variation of the substrate bias voltage. The coating morphology and properties including surface roughness, adhesion, hardness/elastic modulus (H/E) ratio, and friction behavior were analyzed to evaluate the impact of the substrate bias voltage on the coating microstructure and properties. The results suggest that for an optimized value of the substrate bias voltage, i.e. − 150 V, the CrTiAlN coatings showed increased Cr content and improved properties, such as higher adhesion strength, hardness, and elastic modulus in comparison to the coatings deposited by other substrate bias voltage. Moreover, the optimum coatings achieved a remarkable reduction in the steel friction coefficient from 0.65 to 0.45.     

Deposition of nano-scaled CrTiAlN multilayer coatings with different negative bias voltage on Mg alloy by unbalanced magnetron sputtering

In a magnetron sputtering system, the negative substrate bias voltage has been used as a basic process parameter to modify the deposition structure and properties of coatings. In this paper we report the effect of bias voltage ranging from −40 V to −90 V on nano-scaled CrN/TiN/CrN/AlN (CrTiAlN) multilayer coatings synthesized on a Mg alloy by a closed-field unbalanced magnetron sputtering ion plating system in a gas mixture of Ar + N₂. The technological temperature and atomic concentration in the multilayer coatings were controlled by adjusting the current density of different metal magnetron targets and the plasma optical emission monitor. The composition, crystallographic structure, deposition model and friction coefficient of multilayer coatings were characterized by X-ray photoelectron spectrometry (XPS), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and ball-on-disc testing. The experimental results show that the deposition model and friction coefficient of nano-scaled CrTiAlN multilayer coatings were significantly affected by the negative bias voltage (V_b). The nitride species in multilayer coatings mainly involve CrN, AlN and TiN, and XRD analysis shows that the crystallographic structure was face-centered cubic. Under different bias voltage conditions, the multilayer coating composition shows a fluctuation, and the Al and Cr concentrations respond in the opposite sense to the bias voltage, attaining their greatest values at V_b = −70 V. The surface and cross-sectional morphology shows deposition model change from a columnar model into non-columnar model with the increase in negative bias voltage. The friction coefficient of the nano-scaled multilayer coatings at V_b = −55 V stabilize after 10 000 cycles.     

Nanoindentation and atomic force microscopy measurements on reactively sputtered TiN coatings

Titanium nitride (TiN) coatings were deposited by d.c. reactive magnetron sputtering process. The films were deposited on silicon (111) substrates at various process conditions, e.g. substrate bias voltage (V_B) and nitrogen partial pressure. Mechanical properties of the coatings were investigated by a nanoindentation technique. Force vs displacement curves generated during loading and unloading of a Berkovich diamond indenter were used to determine the hardness (H) and Young’s modulus (Y) of the films. Detailed investigations on the role of substrate bias and nitrogen partial pressure on the mechanical properties of the coatings are presented in this paper. Considerable improvement in the hardness was observed when negative bias voltage was increased from 100–250 V. Films deposited at |V _B| = 250 V exhibited hardness as high as 3300 kg/mm². This increase in hardness has been attributed to ion bombardment during the deposition. The ion bombardment considerably affects the microstructure of the coatings. Atomic force microscopy (AFM) of the coatings revealed fine-grained morphology for the films prepared at higher substrate bias voltage. The hardness of the coatings was found to increase with a decrease in nitrogen partial pressure.     

An analysis of macroparticle-related defects on CrCN and CrN coatings in dependence of the substrate bias voltage

Chromium nitride coatings with and without a carbon content being assigned as CrCN and CrN were prepared by cathodic arc evaporation. The effect of negative substrate bias voltages (10-300 V) on the microstructure, phase composition and morphology of the coating surface was studied. X-ray diffraction data show that almost all coatings crystallized in the cubic structure with (111) and (200) diffraction lines appearing only for low negative bias voltage and a (220) diffraction line being present for the coatings deposited at higher negative bias voltages. For CrN coatings obtained at −300 V a hexagonal structure was also observed. In case of CrCN coatings the (220) diffraction line shows much higher intensity than in case of CrN coatings and was significantly broadened. On the surface of the coatings a large number of macroparticles of different size was observed. An increase of bias voltage causes a reduction of the areal density of macroparticles and a decrease of the mean surface roughness Ra.     

Improvement of microstructural and mechanical properties of plasma sprayed Mo coatings deposited on Al-Si substrates by pre-mixing of Mo with TiN powder

The present work embodies development of a new class of mechanically improved Mo-TiN coating material using plasma spray technique. The coatings are developed on Al-Si alloy at different torch input power levels ranging from 15 kW to 30 kW. Pre-mixing of TiN with molybdenum enhances adhesion strength and hardness of the coatings. Maximum adhesion strength of 22 MPa (±0.75) and hardness of 748 HV (±30) are found for the coating when molybdenum is pre-mixed with 10% TiN. FESEM micrographs of the as-sprayed coatings showed formation of plate-like structures of splats which indicates TiN sites as reinforcement in Mo matrix. X-ray diffraction study reveals the formation of both MoO2 and TiN as minor phases in the coating microstructure. The significant enhancement of mechanical properties like adhesion strength and hardness is attributed towards the presence of these phases.     

The effect of PVD coatings on the corrosion behaviour of AZ91 magnesium alloy

In this study, multilayered AlN (AlN + AlN + AlN) and AlN + TiN were coated on AZ91 magnesium alloy using physical vapour deposition (PVD) technique of DC magnetron sputtering, and the influence of the coatings on the corrosion behaviour of the AZ91 alloy was examined. A PVD system for coating processes, a potentiostat for electrochemical corrosion tests, X-ray difractometer for compositional analysis of the coatings, and scanning electron microscopy for surface examinations were used. It was determined that PVD coatings deposited on AZ91 magnesium alloy increased the corrosion resistance of the alloy, and AlN + AlN + AlN coating increased the corrosion resistance much more than AlN + TiN coating. However, it was observed that, in the coating layers, small structural defects e.g., pores, pinholes, cracks that could arise from the coating process or substrate and get the ability of protection from corrosion worsened were present.     

Improving hardness of biomedical Co-Cr by deposition of dense and uniform TiN films using negative substrate bias during reactive sputtering

This paper reports the deposition of a fully dense and uniform TiN film to improve the surface hardness of Co-Cr, particularly, by applying a negative substrate bias during reactive direct current (DC) sputtering. As the TiN film was deposited with a negative substrate bias voltage of 150 V, the microstructure of the films was shifted from a columnar to non-columnar one that was observed to have a dense, uniform and smooth surface. In addition, the preferred orientation was the (111) plane when the films were deposited with a negative substrate bias; however, the (200) plane when they were deposited without a substrate bias. The deposition of the dense and uniform TiN film resulted in a significant increase of the hardness of the Co-Cr. The TiN-deposited Co-Cr with a negative substrate bias showed a very high hardness of 44.7 ± 1.7 GPa, which was much higher than those of the bare Co-Cr (4.2 ± 0.3 GPa) and TiN-deposited Co-Cr without a negative substrate bias (23.6 ± 2.8 GPa).     

TiN/TiC multilayer films deposited by pulse biased arc ion plating

TiN/TiC multilayer films were deposited on high-speed-steel (HSS) substrates using pulse biased arc ion plating. For comparison, TiN and TiC films were also deposited. Scanning electron microscopy (SEM), X-ray diffraction (XRD) and Auger electron spectroscopy (AES) were applied to investigate the modulation period thickness, microstructure and content depth distribution of the films, respectively. And microhardness and film/substrate adhesion were also analyzed using knoop tester and scratching method. The results showed that the multilayer films with different modulation period of 40-240 nm exhibit a modulation structure and the interface width is about 20∼30 nm. Microhardness of the multilayer films were not obviously improved compared to that of TiN and TiC film, and the reason was analyzed. In comparison to TiN film, film/substrate adhesion values of the multilayer films were deteriorated with the increasing of modulation period due to the brittle characteristics of TiC film.     

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.     

对LY12铝合金离子镀氮化钛涂层的增强结合力的研究

在LYl2铝合金上,用离子镀设备进行了增强氮化钛涂层结合力的研究。通过镀前表面处理工艺技术及镀膜过程中控制烘烤温度、加镀过渡层、延长沉积时间等主要工艺技术,最终得到了令人满意的、涂层结合力增强的氮化钛涂层。     

TC4钛合金表面电弧离子镀TiN/CrN纳米多层薄膜研究

用电弧离子镀技术在TC4钛合金基体上通过改变偏压制备了4组TiN/CrN薄膜,对薄膜的表面形貌、厚度、相结构、硬度、膜基结合力和摩擦系数等组织、性能进行了测试表征。结果表明,薄膜是由TiN相和CrN交替叠加构成的纳米多层薄膜,薄膜的调制周期为60 nm,总的厚度约为480 nm。与基体钛合金相比,镀膜后样品的表面性能与偏压幅值密切相关并有显著提高:显微硬度从基体的3 GPa提高到16.5~24.7 GPa;摩擦系数从基体的0.35大幅度降低到0.14~0.17;薄膜与基体结合牢固,膜基临界载荷在60~80N之间。经电弧离子镀TiN/CrN纳米多层薄膜处理后,TC4钛合金可以满足沙粒和尘埃磨损条件下的耐磨性能要求。