Tribological properties of multilayer DLC/W-DLC films on Si

Multilayer films of diamond-like carbon (DLC) and tungsten-containing diamond-like carbon (W-DLC) films were deposited onto silicon wafers using radio frequency chemical vapor deposition (RFCVD) and a magnetron sputtering method. The W-DLC layer was deposited on the silicon wafer with less than 60 W magnetron output. The DLC layer was then deposited on the W-DLC layer.Surface morphology was investigated by atomic force microscopy and the film structure by transmission electron microscopy. Friction tests for multilayered films were performed in a nitrogen atmosphere at room temperature using a ball-on-disk tribometer. A conventional stainless steel ball was used for the test.The surface profiles seen by atomic force microscopy showed that round-shaped clusters of around 100 nm were observed in just the single W-DLC layer. These clusters were considered to be tungsten or tungsten-carbon composites. In the case of the DLC/W-DLC multilayered structure, the top DLC layer covered the W-DLC single layer and smoothed the surface of the W-DLC film.Friction tests demonstrated that the friction coefficient of the W-DLC single layer was above 0.6 and increased gradually as the number of cycle increased. The W-DLC films partially broke down during our measurements. However the DLC/W-DLC multilayer films showed stable friction properties and were observed for up to 100,000 cycles. Their friction coefficient was typically less than 0.1 at 10 cm/s rotating speed. The DLC/W-DLC multilayer films exhibited stable low friction properties in a long term test under a nitrogen atmosphere.     

The effects of plasma pre-treatment and post-treatment on diamond-like carbon films synthesized by RF plasma enhanced chemical vapor deposition

Diamond-like carbon (DLC) films were synthesized by RF plasma enhanced chemical vapor deposition and the effects of plasma pre-treatment and post-treatment on the DLC films were investigated. Experimental results show that the surface roughness of the substrate, ranging from 0.2 to 1.2 nm, created by the plasma pre-treatment, will affect the surface roughness of the DLC films deposited using methane as the carbon source. However, the film surface roughness (0.1-0.4 nm) is much smaller than that of the substrate. Raman analysis and hardness measurement by nanoindentation indicate that the structure and the hardness of the DLC films are relatively unchanged for the film surface roughness investigated. For the argon or hydrogen plasma post-treatment of the DLC films deposited using acetylene as the carbon source, it is found that surface roughness decreases with the post-treatment time. Although the hardness decreases after post-treatment, it remains relatively constant with increasing post-treatment time.     

超高分子量聚乙烯表面金属化及类金刚石薄膜沉积复合处理研究

采用超高分子量聚乙烯(UHMWPE)表面金属化及类金刚石薄膜沉积复合处理工艺,提高超高分子量聚乙烯的耐磨性.首先采用磁过滤阴极真空弧源沉积技术(FCVA)在UHMWPE表面制备约30nm钛金属层,使UHMWPE表面金属化,然后再沉积DLC薄膜,研究结果表明,UHMWPE表面金属化后,DLC薄膜沉积过程中,电荷累积效应消...     

Deposition of diamond-like carbon films on the inner surface of narrow stainless steel tubes

Diamond-like carbon (DLC) films were deposited on the inner surface of 304-type stainless steel tube with an inner diameter of 10 mm by DC glow discharge plasma. The influence of the deposition time, pressure and the ratios of CH₄ in CH₄/Ar gas mixture on the DLC film deposition were investigated. The images of Scanning Electron Microscopy (SEM) show that the DLC films are featureless and free of porosity. Fibre-like structure was recognized on the film surface by Atomic Force Microscopy (AFM). The film deposition rate decreases with increasing the deposition time. Relative higher deposition rate (40 nm/min) can be obtained at 20-30 Pa, higher and lower pressure will significantly decrease the deposition rate. Raman spectrum analysis shows that the films deposited in 30 min at 20-30 Pa have more sp³ content. The corrosion resistance of the films was measured by potentiodynamic polarization test. The DLC films deposited on the inner surface of the 304-type stainless steel tube significantly improve its corrosion resistance.     

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.     

SiOx-doped DLC films: Charge transport, dielectric properties and structure

In the present study, SiO_x-doped diamond-like carbon (DLC) films were synthesized by ion beam deposition on different substrates. Electrical properties, morphology and structure of the DLC films were investigated. Poole-Frenkel emission was the main carrier transport mechanism in all investigated metal-SiO_x-doped DLC-metal samples. Dielectric properties of the samples were dependent on both the bottom and top electrode metal. The trans-polyacetylene chain vibrations detected from the Raman spectra have been observed for all the SiO_x-doped DLC films. Different dielectric properties of the film deposited onto the different metal interlayers were explained both by different roughness of the metal films and by different structure of the ion beam-synthesized SiO_x-doped DLC films.     

Abscheidung superharter Kohlenstoffschichten mittels Laser‐Arco® auf dem Weg vom Labor in die industrielle Serienfertigung

Superhard carbon film deposition by means of Laser‐Arco® on the way from the Laboratory into the industrial series coating Diamond‐like carbon films (DLC) are more and more applied as wear protection coatings for components and tools due to their unique combination of high hardness, low friction and sticking tendency to metallic counter bodies. Up to now applied DLC films are hydrogen containing (a‐C:H) or metal carbon films (Me‐C:H) deposited by a plasma assisted CVD process from carbon‐hydrogen gas mixtures. Their wide industrial effort results from that the can be deposited with slowly modified coating machines for classical hard coating (e.g. TiN or CrN). A new generation DLC films are the hydrogen‐free ta‐C films (ta‐C = tetrahedral bounded amorphous carbon) with a between two and three‐times higher hardness and with a resulting higher wear resistance under extreme condition than classical DLC films. They have excellent emergency running properties at lubrication break down. Their industrial application is more difficult due to that they cannot deposited with modified coating machines for classical hard and DLC coating and a new technology with corresponding equipment was not available up to now. The laser controlled, pulsed arc deposition technology (Laser‐Arco®) of the Fraunhofer IWS Dresden has this potential. In kind of a Laser‐Arc‐Module‐source the ta‐C film deposition can be integrated in every industrial used deposition machine.     

Microstructure of interface for high-adhesion DLC film on metal substrates by plasma-based ion implantation

The diamond-like carbon (DLC) film was prepared on various metal substrates with a plasma-based ion implantation and deposition using superimposed RF and negative high-voltage pulses. The adhesion strength of DLC film was enhanced above the epoxy resin strength by implantation of carbon ions or mixed ions of carbon and silicon to the substrate surface before DLC deposition. In order to clarify the mechanism for improvement in adhesive strength, the microstructure of an interface between DLC film and substrate was examined in detail by transmission electron microscopy (TEM) observations in combination with EDS analysis. As a result, the enhancement in adhesion strength of DLC film by C ion implantation resulted from the formation of amorphous-like phase in the ion-implanted region of substrate, the production of carbon-component graded interface, the destruction of the oxide layer on the top surface of substrate, and the reduction of residual stress in DLC film by ion implantation during the deposition. The production of stress-free DLC film allowed us to demonstrate a supra-thick DLC film of more than 400 μm in thickness.     

Tribocorrosion behavior of DLC-coated CoCrMo alloy in simulated biological environment

Due to renewed interest in hard-on-hard prosthetic joint replacements, especially metal-on-metal (MOM) and ceramic-on-metal joints (COM), concerns about debris and released metal ions from wear and mechanical-enhanced electrochemical (tribocorrosion) processes have raised. In order to reduce the metal debris quantity and the release of metal ions, a diamond like carbon (DLC) film is deposited on CoCrMo alloy by using a filtered cathodic vacuum arc technique (FCVA). The tribocorrosion behavior of DLC coated CoCrMo alloy is studied in bovine calf serum and 0.9% NaCl solution by using a linear reciprocating pin-on-plate tribometer with an integrated electrochemical cell. The open circuit potential (OCP) and the polarization test are monitored during the reciprocating pin-on-plate test. The results show that the absorbed protein layer on DLC surface play a positive role in reducing wear and metal ion release. The presence of DLC layer improves the tribocorrosion resistance of CoCrMo alloy. And The DLC film has a potential application on hard-on-hard prosthetic joint replacements and it can effectively reduce the metal debris quantity and the release of metal ions.     

Study of diamond-like carbon films on LiNbO3

Diamond-like carbon (DLC) films have been successfully deposited on Y-cut LiNbO₃ substrates using the plasma enhanced CVD technique. A thin interlayer of SiC between the DLC films and the LiNbO₃ is necessary to ensure a good adhesion of the DLC films to the LiNbO₃ substrate. The physical properties and structural network of the DLC films have been investigated in detail. It is observed that the film hardness is increased with increasing the film thickness, as is the adhesion of the DLC films to the LiNbO₃ substrates. The effect of accelerating surface acoustic wave by the DLC films has been confirmed.     

Fabrication of high frequency ZnO thin film SAW devices on silicon substrate with a diamond-like carbon buffer layer using RF magnetron sputtering

Diamond-like carbon (DLC) film is a promising candidate for surface acoustic wave (SAW) device applications because of its higher acoustic velocity. A zinc oxide (ZnO) thin film has been deposited on DLC film/Si substrate by RF magnetron sputtering; the optimized parameters for the ZnO sputtering are RF power density of 0.55 W/cm², substrate temperature of 380 °C, gas flow ratio (Ar/O₂) of 5/1 and total sputter pressure of 1.33 Pa. The results showed that when the thickness of the ZnO thin films was decreased, the phase velocity of the SAW devices increased significantly.     

Evaluation of microstructures and mechanical properties of diamond like carbon films deposited by filtered cathodic arc plasma

Diamond-like carbon (DLC) films were deposited by a cathodic arc plasma evaporation (CAPD) process, using a mechanical shield filter combined with a magnetic filter with enhanced arc structure at substrate-bias voltage ranging from − 50 to − 300 V. The film characteristics were investigated using Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and high-resolution transmission electron microscopy (HRTEM). The mechanical properties were investigated by using a nanoindentation tester, scratch test and ball on disc wear test. The Raman spectra of the films showed that the wavenumber ranging from 900 to 1800 cm^− 1 could be deconvoluted into 1140 cm^− 1, D band and G band. The bias caused a significant effect on the sp³ content which was increased with the decreasing of I_D/I_G ratio. The XPS spectra data of the films which were etched by H⁺ plasma indicated the sp³ content are higher than those of the as-deposited DLC films. This implied that there is a sp²-rich layer present on the surface of the as-deposited DLC films. The nanoindentation hardness increased as the maximum load increased. A 380 nm thick and well adhered DLC film was successfully deposited on WC-Co substrate above a Ti interlayer. The adhesion critical load of the DLC films was about 33 N. The results of the wear tests demonstrated that the friction coefficient of the DLC films was between 0.12 and 0.2.     

The study of adhesion and nanomechanical properties of DLC films deposited on tool steels

In this study, thin diamond-like carbon (DLC) films were deposited onto a steel substrate. By using the plasma immersion ion implantation (PIII) technique, a nitrogen layer was formed on the steel surface before depositing the DLC films. This PIII formed nitrogen layer, which acts as the buffer layer, has apparently increased the adhesion between the DLC film and the steel substrate. The microstructures, the nanomechanical properties, and the adhesion of the DLC were investigated by the techniques of X-ray diffraction (XRD), transmission electron microscopy (TEM), nanoindentation, and nanoscratch. Results show that the hardness and Young's modulus were significantly improved, up to 2 to 9 times; while the implantation depth and the microstructure of the nitrogen layers vary with nitrogen/hydrogen ratio (N:H = 1:0, 1:1, 1:3). Raman analyses indicate that the I(D)/I(G) ratio increases with the thickness of DLC film. By using the PIII technique in the steel substrate, the adhesion of the DLC film onto the substrate is greatly enhanced, and wear resistance is elevated if the DLC film is sufficiently thick.     

Optical and mechanical properties of diamond like carbon films deposited by microwave ECR plasma CVD

Diamond like carbon (DLC) films were deposited on Si (111) substrates by microwave electron cyclotron resonance (ECR) plasma chemical vapour deposition (CVD) process using plasma of argon and methane gases. During deposition, a d.c. self-bias was applied to the substrates by application of 13·56 MHz rf power. DLC films deposited at three different bias voltages (−60 V, −100 V and −150 V) were characterized by FTIR, Raman spectroscopy and spectroscopic ellipsometry to study the variation in the bonding and optical properties of the deposited coatings with process parameters. The mechanical properties such as hardness and elastic modulus were measured by load depth sensing indentation technique. The DLC film deposited at −100 V bias exhibit high hardness (∼ 19 GPa), high elastic modulus (∼ 160 GPa) and high refractive index (∼ 2·16–2·26) as compared to films deposited at −60 V and −150 V substrate bias. This study clearly shows the significance of substrate bias in controlling the optical and mechanical properties of DLC films.     

Effect of silver doping on optical property of diamond like carbon films

Optical properties of silver doped diamond like carbon films (Ag:DLC) deposited by the RF reactive sputtering technique were studied in detail. The chemical binding energy and the composition of the films were investigated by using an X-ray photoelectron spectroscopy. Optical transparency and optical band gap decreased with the silver incorporation to the DLC film. Optical band gap calculated from transmittance spectra decreased from 2.55 to 1.95 eV with a variation of Ag concentration from 0 to 12.5 at.%. Urbach parameter determined from the band tail of the transmittance spectra showed to increase with the doping concentration.     

Ion beam synthesis of the diamond like carbon films for nanoimprint lithography applications

Ion beam deposited hydrogenated undoped as well as SiO_x (SiO_x + N₂, SiO_x + Ar) doped DLC thin films were deposited and evaluated as possible anti-adhesive layers for nanoimprint lithography. Film surface contact angle with water was investigated as a measure of the surface free energy and anti-sticking properties. Contact angle of the DLC films was independent of SiO_x doping and ion beam energy. Air-annealing resistance in terms of the contact angle with water of the synthesized diamond like carbon films was investigated. Optical transmittance spectra of the DLC films in UV-VIS range were measured to investigate it as possible anti-sticking layers for UV imprint lithography applications. DLC films with the most promising combination of the UV absorption and anti-sticking properties were revealed. Preliminary imprint tests with uncoated and thin DLC film coated hot imprint stamps were performed.     

利用脉冲激光真空弧沉积技术制备类金刚石薄膜

介绍了一种新的脉冲激光真空弧沉积技术, 利用该技术在硅基片上制备了类金刚石薄膜. 利用激光拉曼分析技术对沉积膜进行了结构分析, 结果表明沉积膜为非晶结构, 具有明显的sp³ 结构特征. 同时利用纳米划痕压痕仪、原子力显微镜等分析设备对膜的表面形貌、微观摩擦学性能进行了分析, 结果表明Si<100>基片上沉积膜的表面形貌和微观摩擦学性能略优于 Si<111>基片上沉积的薄膜, 其摩擦系数平均值为0.036.     

Deuterium influence on optical gap of amorphous carbon diamond-like carbon (DLC) thin film

This present study aims to determine the hydrogen influence on the electrical gap of diamond-like carbon (DLC) film. DLC thin layers were deposited on silicon wafer by plasma enhanced chemical vapour deposition (PECVD). With this method we obtain a a-C:H film structure. To understand the mechanism of deposition, local structure and hydrogen effect in DLC we replace our methane plasma source by deuterated methane one. In this article, hydrogen rate is obtained by elastic recoil detection analysis (ERDA), electronic and bulk density is performed with X-ray reflectometry (XRR) and the determination of electrical gap is carried out using ultraviolet-visible absorption spectrometry. A specific attention is carried about the self-bias voltage and time variations to get different DLC and DDLC film compositions and also different electrical properties. We found that including deuterium in carbon increases the Tauc energy while keeping the same density. A comparison between these two sorts of film is expected to improve our understanding of the hydrogen role in the DLC films.     

The influence of fluorine doping on the optical properties of diamond-like carbon thin films

Optical properties of fluorine doped diamond-like carbon (F:DLC) films deposited by the direct current plasma enhanced chemical vapor deposition (PECVD) technique were studied in detail. Surface morphologies of the F:DLC films were studied by an atomic force microscope, which indicated surface roughness increased with increase in at.% of F in the films. The chemical binding was investigated by X-ray photoelectron spectroscopic studies. Fourier transformed infrared spectroscopic studies depicted the presence of CF_x (x = 1,2,3) and CH_n (n = 1,2) bonding within the F:DLC films. Optical transparency and the optical band gap decreased with the fluorine incorporation in the DLC film. Optical band gap calculated from the transmittance spectra decreased from 2.60 to 1.95 eV with a variation of 0-14.8 at.% of F concentration in the diamond-like carbon films. Urbach parameter determined from the band tail of the transmittance spectra showed that it increased with the doping concentration.     

Stress and strain in DLC films induced by electron bombardment

Radiation induced stress and strain have been investigated in amorphous hydrogenated DLC films after their exposure to high-energy (12 MeV) electrons, produced in the medical linear accelerator. DLC structures of different hydrogen contents and thickness, deposited from acetylene gas onto Si<111> wafers in the two-chamber plasmotron system were used in this investigation.Optically levered laser technique was used to measure the radius of curvature of the investigated DLC films and residual stress in the film was determined. Surface morphology of DLC films was defined by AFM “Nanotop-206”. Microhardness measurements were performed using MTS Nanoindenter G200. Bonding structure of the DLC films was analysed using the Raman scattering spectroscopy.It was found that the bombardment of DLC films with high-energy electrons introduced additional residual stress in all investigated samples. However, stress saturation tendency was observed after some fractions of the irradiation. Radiation induced stress was lower in the samples with well-organized networking structure, depending on technological conditions of the film growth. Significant deterioration of the mechanical properties of DLC films after their bombardment with high-energy electrons was not observed. Radiation induced changes in irradiated DLC films are discussed on the basis of the results of measurements.