Niederenergie-IBAD: Zusammenhang zwischen Prozeßparametern und Schichteigenschaften bei ionenstrahlunterstützten Aufdampf-und Sputtertechniken

Low energy IBAD: correlation between process parameters ans film properties for ion beam assisted evaporation and sputter deposition Binary nitride films with Al, Cr and Ti as metal components have been deposited with ion beam assisted evaporation and sputtering (IBAD) and the film properties are investigated in terms of the individual deposition parameters. In the case of ion beam assisted evaporation the flux ratio between the film forming metal atoms and the nitrogen ions from the ion source was shown to enable a quantitative control of the composition and the chemical phases of the films. Detailed studies for TiN reveal the possibilities to manipulate texture and stress, the average grain size and the morphology of the films. Such results are discussed with an extended structure zone model, introducing the energy input per film forming particle as the relevant parameter. Also, the structural film properties and the deposition parameters are quantitatively correlated with the hardness and the beginning of TiN deposition on stainless steel resulted in distinctly improved adhesion properties. For the deposition of TiN with a dual ion beam arrangement in which one beam bundle was directed onto a Ti-target and an other onto the substrate with the growing film, a strong influence of the particle energies and the incidence angles on the film texture and its directional orientation was found. Such effects are quantitatively related to the minimization of the free energy of the films and the influence of preferential re-sputtering effects. For ion beam sputter deposition without simultaneous ion bombardment of the growing film, the texture and the film stress are found to be controlled by energetic particles resulting from elastic backscattering at the target surface.     

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.     

离子束辅助沉积TiN薄膜的结构和成分

用离子束辅助沉积合成了TiN薄膜,背散射、X射线衍射和透射电镜实验的结果表明,在本实验条件下,薄膜Ti/N比接近于TiN的化学计量比,和氮离子束流密度无关。薄膜存在<100>择优取向,在一定条件下,可以形成只有(100)取向的TiN薄膜。     

Deposition of diamond like carbon (DLC) and C-N films using ion beam assisted deposition (IBAD) technique and evaluation of their properties

Diamond like carbon films and C-N films were prepared using ion beam assisted deposition technique (IBAD). Tribological properties were studied by subjecting DLC coated films to the accelerated wear tests. These tests indicated a significant improvement in the mechanical surface properties of glass by DLC coating. Better wear features were obtained for thinner DLC coating as compared to the thicker ones. We also studied the optical properties and obtained a band gap of 1·4 eV for these films. An attempt was made to prepare C₃N₄ films by using IBAD. We observed variation in the nitrogen incorporation in the film with the substrate temperature.     

Nematic liquid crystal alignment on the ion beam-exposed ZnO film

This paper investigates the nematic liquid crystal (NLC) alignment on ion beam-exposed zinc oxide (ZnO) films. The ZnO films are deposited by a radio frequency magnetron sputtering. During the deposition of ZnO film, we supplied sufficient oxygen gas for high resistivity and transmittance. The deposited films show a high transmittance of over 90% and high resistivity of over 10¹⁰ Ω cm. The ZnO films show a high deposition rate of 26.7 Å/min. Images obtained via scanning electron microscopy of the ZnO film surfaces, before and after the ion beam exposure, show that groove patterns are formed being to be parallel to the ion beam exposure direction. LC cells are fabricated with the ion beam-exposed ZnO films. The NLC molecules align parallel to the ion beam exposure direction. The electro-optic and response characteristics of fabricated cells show the possibility of application to liquid crystal displays.     

The effect of the ion beam energy on the properties of indium tin oxide thin films prepared by ion beam assisted deposition

Indium tin oxide (ITO) thin films have been deposited onto polycarbonate substrates by ion beam assisted deposition technique at room temperature. The structural, optical and electrical properties of the films have been characterized by X-ray diffraction, atomic force microscopy, optical transmittance, ellipsometric and Hall effect measurements. The effect of the ion beam energy on the properties of the films has been studied. The optical parameters have been obtained by fitting the ellipsometric spectra. It has been found that high quality ITO film (low electrical resistivity and high optical transmittance) can be obtained at low ion beam energy. In addition, the ITO film prepared at low ion beam energy gives a high reflectance in IR region that is useful for some electromagnetic wave shielding applications.     

DLC膜厚度对镁基表面DLC/MAO复合膜层性能的影响

采用线性离子束沉积技术于AZ80镁合金微弧氧化(MAO)陶瓷层表面沉积不同厚度的类金刚石碳(DLC)膜,形成DLC/MAO复合膜层。对比研究4种膜基系统的表面结构特征、力学性能以及摩擦学性能差异。结果表明:随DLC膜厚度增加,复合膜层表面微孔数量减少,孔径减小,但凹凸不平趋势增加,且DLC膜表面颗粒特征更加明显,表现为DLC-80min/MAO/AZ80膜基系统具有最小的表面粗糙度,最大的硬度H、弹性模量E及H/E值;不同厚度DLC/MAO/AZ80膜基系统平均摩擦因数较MAO/AZ80显著降低;DLC膜厚度增加导致3种复合膜基系统的表面微观结构改变,使得摩擦因数与磨痕形貌存在差异;各膜基系统表面磨痕处均形成了Fe的转移层,由于表层DLC膜"裸露"的大量C对磨损界面具有很好的润滑作用,而使得镁合金基体获得有效保护。     

Bactericidal and biocompatible properties of TiN/Ag multilayered films by ion beam assisted deposition

Nanoscale TiN/Ag multilayered films of thickness 500 nm were synthesized on AISI317 stainless steel by ion beam assisted deposition (IBAD) with the modulation period of 4, 5, 6, 7.5, and 12 nm. The bactericidal and biocompatible properties of TiN/Ag multilayered films were investigated through Gram negative E. coli bacteria and L929 cells (mice fibroblast) as well as human umbilical vein endothelial cells (HUVEC). The results show that the TiN/Ag multilayered films with the modulation period of 7.5 nm possess the strongest bactericidal property. The cytotoxicity grade of TiN/Ag multilayered coating with the modulation periods of 7.5 nm, 12 nm is in 0-1 scope, which indicates this film has no cytotoxicity to L929. HUVEC on TiN/Ag multilayered film grows well and shows good cellularity. Auger electronic spectroscopy reveals the relationship between the structure of TiN/Ag multilayered film and the biomedical properties.     

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.     

离子辅助蒸发TixOy制备氧化钛薄膜及特性

采用离子辅助沉积的方法,分别以TiO2和Ti3O5为初始膜料在K9玻璃上制备了氧化钛薄膜,并研究了离子束流密度对以Ti3O5为膜料制备的薄膜透射性能的影响.实验结果表明,热处理前薄膜都为无定形结构;热处理后有明显的锐钛矿结构(101)择优取向,以Ti3O5为初始膜料制备的薄膜吸收优于以TiO2为膜料制备的薄膜;薄膜透射率极值随束流密度增大有临界值.     

Bactericidal and biocompatible properties of TiN/Ag multilayered films by ion beam assisted deposition

Nanoscale TiN/Ag multilayered films of thickness 500 nm were synthesized on AISI317 stainless steel by ion beam assisted deposition (IBAD) with the modulation period of 4, 5, 6, 7.5, and 12 nm. The bactericidal and biocompatible properties of TiN/Ag multilayered films were investigated through Gram negative E. coli bacteria and L929 cells (mice fibroblast) as well as human umbilical vein endothelial cells (HUVEC). The results show that the TiN/Ag multilayered films with the modulation period of 7.5 nm possess the strongest bactericidal property. The cytotoxicity grade of TiN/Ag multilayered coating with the modulation periods of 7.5 nm, 12 nm is in 0–1 scope, which indicates this film has no cytotoxicity to L929. HUVEC on TiN/Ag multilayered film grows well and shows good cellularity. Auger electronic spectroscopy reveals the relationship between the structure of TiN/Ag multilayered film and the biomedical properties.     

空心阴极电子束对多弧离子镀TiAlN薄膜组织形貌及摩擦学性能的影响

采用空心阴极电子束辅助多弧离子镀的方式在WC基体上制备了TiAlN薄膜,讨论了电子束能量的大小对膜层组织形貌及摩擦学性能的影响。利用X射线衍射仪、扫描电子显微镜、表面轮廓测试仪及材料表面微纳米力学测试系统对薄膜的相组成、微观结构、三维形貌及摩擦学性能进行了检测和分析。结果表明:在未施加空心阴极电子束作用时薄膜具有明显的(112)择优取向,随着空心阴极电流的提高,薄膜逐渐朝着多晶面生长,择优取向减弱。电子束对膜层的形貌及摩擦学性能有显著影响,随着电子束能量的提高,膜层逐渐变得致密、平整,表面粗糙度和摩擦系数均降低,抗磨损性能提高。     

Structure and tribological properties of Ag films deposited at low temperature

The effects of substrate temperature on the structure and tribological properties of Ag films deposited at low temperatures (LT, 130-217 K) by arc ion plating (AIP) have been studied. The structure and morphology of the Ag films were analyzed by X-ray diffraction (XRD), transmission electron microscopy (TEM) and field emission scanning electron microscope (FESEM). The results showed that there exist (1 1 1) and (2 0 0) preferred orientation transitions for decreasing temperature at different bias voltages. The tribological properties were evaluated by a ball-on-disk tribometer and wear tracks were analyzed by means of scanning electron microscopy (SEM). The results show that substrate deposition temperature significantly affected the wear of LT Ag films. For each bias voltage studied, the film showing the highest wear rate was deposited at the lowest temperature and the film with the lowest wear rate, (significantly lower than room temperature (RT) deposited Ag films), was deposited at a temperature between the highest and the lowest temperatures examined. The wear mechanism was discussed in terms of lubrication effect of film material transferred to the counterpart and its dependence on the microstructure of the original deposited film.     

Direct ion beam deposited carbon films and clusters

Carbon films and clusters have been formed by direct ion beam deposition. In all experiments crystalline n-Si 〈1 0 0〉 wafers with the 300 nm thermal SiO₂ film have been used as substrates. Effects of thermally microstructured Ni and substrate temperature were studied. Chemical structure of the carbon films was investigated using Raman spectroscopy. Surface morphology was studied by atomic force microscopy (AFM). Supplemental research on sheet resistance of the films has been performed. Rough diamond-like carbon film was grown onto the catalytic layer at 400 K temperature, and surface of the diamond-like carbon film deposited directly onto the SiO₂ layer at 400 K temperature was very smooth. At 750 K growth of the array of cylindrically shaped clusters was observed by AFM in the case of catalytically assisted deposition. Raman spectra of deposited films were typical for glassy carbon and/or carbon nanotubes with the carbonaceous deposits. Catalyticless deposition at 750 K temperature resulted in the formation of the conductive polymer-like carbon film with the graphite clusters in it.     

离子束辅助沉积碲化铅薄膜的AFM研究

利用原子力显微镜（AFM）研究了离子束辅助沉积碲化铅（Pblle）薄膜的微观结构和表面形貌。结果表明,传统热蒸发方法制备的碲化铅薄膜呈现出明显的柱状结构,离子束轰击可以显著改变薄膜的微观结构,导致柱状结构的逐渐消失和晶粒的长大。     

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 Tribological Behavior of Stripe Patterned TiN Film Prepared with Filtered Cathodic Vacuum Arc Deposition (FCVAD)

This paper describes an experimental investigation into the influence of the stripe interspace and applied load on the tribological behavior of stripe patterned TiN films. The stripe patterned TiN films are deposited on an H13 steel surface by masked deposition with the filtered cathodic vacuum arc discharge (FCVAD) technique. The surface micro morphology, chemical composition, crystal structure, and mechanical properties of the films is characterized using 3D white light interferometry, scanning electron microscopy (SEM), X‐ray diffractometry (XRD), and a nano‐indentation tester, respectively. The tribological performance of patterned TiN is measured using a UMT‐5 tribometer, and the friction and wear mechanisms are analyzed, compared with that of the full TiN film and H13 steel substrate. The results show that the stripe patterned TiN films has better tribological properties than the full TiN film. These results are attributed to the synergistic effect between the surface pattern and the TiN film. The stripe interspace and the applied load has a more significant effect on the wear rate of the stripe patterned TiN films than the coefficient of friction of their friction pairs. A further study, however, is needed to analyze the relationship between the applied load and the wear rates of the stripe patterned TiN films.

     

Texture evolution of transition-metal nitride thin films by ion beam assisted deposition

TiN, VN and CrN were systematically deposited on silicon substrates using ion beam assisted deposition (IBAD) technique at temperatures and ion (N₂⁺) energy ranging from 300 °C to 500 °C and 100 eV to 650 eV, respectively. The results showed that the texture could be controlled by the ion beam energy, flux, and its incident angle, in conjunction with the deposition temperature. For the 0° angle of ion incidence, fiber textures were formed and could be controlled between (111) and (200) surface plane orientation by adjusting ion flux or ion energy. Three types of in-plane textures were produced, when the ion beam was incident at 45° angle, for which cases ion channeling played an important role in the formation of in-plane texture. Using the strain-energy perturbation method, the stability of texture can be further understood. Among the three in-plane textures, the (200) in-plane texture is strain-energy stable, and the others are not.     

Titanium oxy-nitride films deposited on stainless steel by an ion beam assisted deposition technique

Surfaces of stainless steel SUS304 were coated with titanium oxy-nitride (TiON) films at temperatures of 400–770°C using an ion-beam assisted deposition technique constructed from an electron beam evaporator for Ti evaporation and a microwave ion source for ionizing nitrogen gas. The N ions were accelerated at energies of 0.5–2.0 keV. Most of the deposited TiON films consisted of (60–80)% TiN and (40–20)% TiO₂, and the fraction of TiO₂ increased with increasing substrate temperature. Hardness of the TiNO films varied in the range from 160 GPa to 260 GPa with increasing substrate temperature. The titanium oxy-nitride film could be deposited on stainless steel without a significant deterioration surface layer at 600°C. However, when TiNO films were deposited at temperatures higher than 700°C, the thickness of the TiNO films were significantly thinner and a thick layer containing nitride such as Cr₂N, CrFe, Fe₂N and Fe₄N was formed in a near surface region of stainless steel because more nitrogen diffused into stainless steel.     

Improvement of adhesion of DLC coating on nitinol substrate by hybrid ion beam deposition technique

Diamond-like carbon (DLC) films were prepared for a protective coating on nitinol substrate by hybrid ion beam deposition technique with an acetelene as a source of hydrocarbon ions. An amorphous silicon (a-Si) interlayer was deposited on the substrates to ensure better adhesion of the DLC films followed by Ar ion beam treatment. The film thickness increased with increase in ion gun anode voltage. The residual stresses in the DLC films decreased with increase in ion gun anode voltage and film thickness, while the stress values were independent of the radio frequency (RF) bias voltage. The adhesion of the DLC film was improved by surface treatment with argon ion beam for longer time and by increasing the thickness of a-Si interlayer.