Hardness and microplasticity of nanocrystalline and amorphous calcium phosphate coatings

The hardness of thin (1.0–4.0 μm) hydroxyapatite coatings with different structures (nanocrystalline, amorphous-crystalline, and amorphous) grown by rf magnetron sputtering on Ti and Si plates has been studied using the nanoindentation method. All the grown structures are characterized by the strain which has reversible and irreversible components. The hardness of nanocrystalline coatings (about 10 GPa) corresponds to the average hardness of hydroxyapatite single crystals. The structure of nanocrystalline coatings in the indentation zone and outside it has been investigated and changes in the structure under the indenter have been revealed using high-resolution transmission electron microscopy. From a comparison of the hardnesses of coatings with different structures and based on an analysis of the intragranular structure, it has been assumed that the plastic deformation occurs according to a dislocation-free mechanism. The plastic deformation is interpreted in terms of the cluster representation of the hydroxyapatite structure and amorphous calcium phosphates of the same elemental composition and cluster-boundary sliding during the deformation.     

Adhesion properties of a silicon-containing calcium phosphate coating deposited by RF magnetron sputtering on a heated substrate

Silicon-containing hydroxyapatite coatings 400–700 nm in thickness are prepared by means of radio-frequency (RF) magnetron sputtering on a heated (to 200°C) titanium substrate chemically etched and treated with a pulsed electron beam. The morphology and phase composition of the coating are studied. The morphology and roughness of the composite “calcium-phosphate coating-titanium substrate” differ depending on the treatment procedure of the substrate before deposition. The scratch test method is used to assess the adhesion strength of the coatings formed at different values of bias potential applied to the substrate. It is observed that the adhesion strength of the coating changes with decreasing crystallite size.     

磁控溅射制备微球表面金属Mo涂层的研究

利用磁控溅射制备了各种工艺参数不同的微球表面金属Mo涂层样品,并通过白光干涉仪和扫描电子显微镜对样品的表面及剖面进行了系统的测试分析。分别探究了溅射工作气压和沉积制备时间对微球表面Mo涂层表面形貌以及结晶质量的影响规律。结果表明通过优化工艺参数可制备微球直径约为800μm、涂层厚度为3.5μm到14.1μm、厚度均匀性良好的微球表面Mo涂层。Mo涂层中的晶粒呈现出柱状结构致密堆积在一起,且随涂层的厚度增加晶粒间空隙增大。     

Application of high-frequency magnetron sputtering to deposit thin calcium-phosphate biocompatible coatings on a titanium surface

Thin calcium-phosphate coatings were deposited on titanium substrates by high-frequency magnetron sputtering. The elemental composition of coatings and types of chemical bonds were studied by Rutherford backscattering (RBS) and Fourier transform infrared spectroscopy (FTIR), respectively. An analysis of the IR spectra detected absorption bands caused by vibrations of phosphate PO ₄ ^3? groups and pyrophosphate H₂PO ₄ ^? anions, which are typical of apatites. The RBS results showed that the coating contains elements typical of calcium phosphates, i.e., Ca, P, and O; 45.4 ± 1.1, 3.6 ± 0.5, and 41.1 ± 0.7 at %, respectively. The Ca/P atomic ratio depends on sputtering conditions and varies in the range 1.7–4.0. The physicomechanical characteristics of the coatings and their solubility in a biological liquid were studied. The grown coatings can significantly reduce dissolution of substrates and extraction of dopants into the surrounding solution.     

Effect of pulsed plasma and high-current electron beam treatments on the structure and properties of nickel-based coatings

Using plasma-detonation technology (PDT), nickel-based powder (PGAN-33, PG-10N-01 and PG-19N-01) coatings 80–300 μm thick were deposited on a low-carbon St-3 steel substrate. Coatings were then subjected to additional treatment either by a high-current electron beam (HCEB) or by a high-velocity pulsed plasma jet until melting. The structure was analyzed using x-ray diffraction and conversion Mössbauer spectroscopy in the transmission and scattering modes. The morphology and elemental composition were studied using scanning electron microscopy and microanalysis. The micro-and nanohardness, volumetric wear, and corrosion resistance of the grown coatings were measured. It was found that, as the HCEB and PDT energy density increase, the phase composition changes, phase redistribution occurs, and new phases are formed. The last process is caused by mass transfer from the erosion plasmatron electrode and from a gas plasma jet, and interdiffusion of coating and substrate elements. After the exposure to concentrated energy fluxes, the coating surface roughness decreased. It is shown that physicochemical and mechanical characteristics of modified coatings improve in the case of optimum treatment conditions.     

半导体激光器腔面增透膜AIN薄膜的制备

提出了一种新的半导体激光器增透膜——A1N膜,并用matlab软件模拟分析了不同腔面反射率对激光器输出功率的影响,得到激光器最大输出功率时前后腔面的反射率的最佳值.采用反应磁控溅射技术,利用高纯铝靶(99.999％)和N2+ Ar的混合气体在K9玻璃基片上沉积了AlN薄膜.利用Filmetrics系统对薄膜进行光学性能...     

Diffractometric examination of the structure of heat-resisting steel-based coatings in different measurement geometries

Coatings of the composition of 310S heat-resisting steel dopped Al and Ir additions, deposited on a substrate of the same steel by the magnetron sputtering method, were examined. The measurements were made in the classical Bragg-Brentano geometry and by the GXRD method. With the fixed and different position of the coated sample by rotating the sample by angles ψ. The coating as deposited and after being soaked at 400°C for 15 minutes was subjected to examinations. The examination carried out have shown that coatings may have a unique, subtle structure which is metastable and undergoes irreversible changes in the temperatures up to 400°C. It has been found that in the outermost coating zones and zones closer to the substrate, areas occur in the coating structure, which have the different lattice parameter compared to the basic phase. Additionaly, the local period of the structure equal 5.9 nm was found.     

A study of TiMoN nano-multilayer coatings deposited by CFUBMSIP using DC and HIPIMS power

TiMoN nano-multilayer hard coatings have been deposited using the closed field unbalanced magnetron sputter ion plating (CFUBMSIP) technique. In one set of experiments, standard DC power supplies were used on four magnetrons in the CFUBMSIP system (4DC magnetrons). The second set of experiments was also in the same magnetic field configuration of CFUBMSIP, but three magnetrons were as again powered with standard DC whilst one magnetron with Ti target was supplied by a high power impulse magnetron sputtering (HIPIMS) power generator (3DC + 1HIPIMS magnetrons). Two elemental titanium sputtering targets and two of molybdenum were used to produce the TiMoN nano-multilayer coatings. Analysis of the coatings was carried out to investigate the differences in terms of properties, compositions and microstructures of the coatings deposited by these two sets of experiments. It was found that the coatings deposited by both sets of the experiments exhibited similar properties of high hardness, good adhesion and exceptional wear resistance, with a lower sliding friction than more commonly used hard coatings including TiN, CrN, TiAlN, CrTiAlN etc. Although the initial TiN coating as formed at the coating-substrate interface using the process of 3DC + 1HIPIMS magnetrons appeared to show a less oriented microstructure in comparison with that of the coating produced by the process using 4DC magnetrons, the compositions and cross sectional microstructures of the bulk of the coatings did not show significant differences, as observed by the cross sectional Transmission Electron Microscopy microstructures of these two types of TiMoN coatings.     

The structure and tribological behaviors of CrN and Cr-Ti-N coatings

The Cr-Ti-N coatings with different composition were deposited in a medium frequency magnetron sputtering system on Si (1 1 1) substrates. The structures, surface morphology and wear properties were measured. The binary CrN coatings, formed a single-phase fcc structure with nearly random (1 1 1), (2 0 0) and (2 2 0) orientation, while for the Ti was introduced, coatings show a preferred orientation of (2 0 0). Cr-Ti-N coating shows a much smoother surface than CrN coating. Cr-Ti-N coating with 31.75% Ti content shows the best wear behavior. The excellent tribological properties of this composition coating are corresponding to the solid solution nitride structures.     

In-vitro dissolution and structural and electrokinetic characteristics of titanium-oxynitride coatings formed via reactive magnetron sputtering

The results of investigation into the structure and in-vitro dissolution of titanium-oxynitride coatings deposited via reactive magnetron sputtering are presented. Data on the electrostatic and ζ surface potentials enable estimation of their contribution to adsorption processes and coating dissolution in vitro. Sample cultivation in a solution simulating the composition of the inorganic part of human blood plasma leads to surface mineralization, reduces the value and sign of the surface potential, and alters the surface wettability. The coating prevents the transition of iron ions into a solution and does not induce the calcification of an artificial surface.     

Surface analysis of biocompatible coatings on titanium

The coatings of hydroxyapatite, which is widely used for orthopaedic and dental prothesis, were deposited by using the dip-coating method. The layers of hydroxyapatite were grown on commercial Ti substrates. In order to improve the adhesion of hydroxyapatite, the substrate was a priori covered with titania or calcium titanate by using the sol-gel technique. For comparison, commercial samples of hydroxyapatite coating (manufactured by means of plasma-spray apparatus) were analysed. The chemical composition and the structure of the coatings (TiO₂, CaTiO₃ and hydroxyapatite) were studied by using X-ray photoelectron spectroscopy (XPS), scanning Auger microscopy (SAM), X-ray diffraction (XRD) and secondary electron microscopy (SEM) techniques. The data of quantitative XPS analysis and the surface images (SAM and SEM) displayed the superior quality (cleanness, homogeneity, etc.) of hydroxyapatite deposited by sol-gel in comparison with commercial samples investigated.     

RB-SiC表面改性Si涂层的制备与性能

 为了获得高质量光学表面的碳化硅反射镜,利用射频磁控溅射方法,在直径70 mm的RB-SiC基片上沉积了厚约100 μm的Si改性涂层,对改性层进行超光滑加工,并对改性层的表面形貌及性能进行了测试。ZYGO表面粗糙度仪测试结果表明,抛光后Si改性涂层表面粗糙度均方根值达到了0.496 nm;X射线衍射仪测试显示,制备Si改性涂层为多晶结构;使用拉力机做附着力测试,结果表明膜基附着力大于10.7 MPa。证明采用磁控溅射技术制备的Si改性涂层均匀、致密、附着力好,能够满足RB-SiC材料表面改性要求。     

Bioactive glass thin films deposited by magnetron sputtering technique: The role of working pressure

Bioglass coatings were prepared by radio frequency magnetron sputtering deposition at low temperature (150 °C) onto silicon substrates. The influence of argon pressure values used during deposition (0.2 Pa, 0.3 Pa and 0.4 Pa) on the short-range structure and biomineralization potential of the bioglass coatings was studied. The biomineralization capability was evaluated after 30 days of immersion in simulated body fluid. SEM-EDS, XRD and FTIR measurements were performed. The tests clearly showed strong biomineralization features for the bioglass films. The thickness of the chemically grown hydroxyapatite layers was more than twice greater for the BG films deposited at the highest working pressure, in comparison to those grown on the films obtained at lower working pressures. The paper attempts to explain this experimental fact based on structural and compositional considerations.     

一种新型等离子体磁控溅射镀膜电源设计

磁控溅射镀膜电源是磁控溅射系统中的关键设备之一。根据铌靶和锡靶溅射处理装置的技术要求,研制了一套输出电压0~800 V可调、脉冲宽度5~200 μs可调、频率0~60 Hz可调、在脉冲电流最大幅值约150 A的磁控溅射镀膜电源,分别给出了该电源在铌靶负载和锡靶负载下的实验结果。设计上采用高压短脉冲预电离一体化高功率双极性脉冲形成电路方法,解决了高功率磁控溅射在重复频率工作下有时不能成功溅射粒子、电离时刻不一致、溅射起弧打火靶面中毒、溅射效率低等问题,降低了磁控溅射装置内气体的工作气压,实现低气压溅射镀膜,提高了靶材的溅射效率,减小薄膜表面粗糙度。通过大量实验论证,该电源达到了理想的溅射效果,满足了指标要求。     

极紫外多层膜技术研究进展

在极紫外波段,任何材料都表现出极强的吸收特性,因此,采用多层膜实现高反射率是构建正入射式光学系统的唯一途径。本文总结了极紫外多层膜的发展进程,叙述了制备极紫外多层膜的关键技术(磁控溅射、电子束蒸发、离子束溅射)以及它们涉及的相关设备。由于多层膜反射式光学元件主要应用于极紫外光刻与极紫外天文观测,文中重点讨论了极紫外光刻系统对多层膜性能的要求,镀膜过程中的面形精度和热稳定性等问题;同时介绍了极紫外天文观测中使用的多层膜的特点,特别讨论了多层膜光栅的制备技术和亟待解决的问题。     

Mechanical properties of the plasma-enhanced magnetron sputtering Si-C-N coatings

The mechanical properties of plasma-enhanced magnetron sputtering Si-C-N hard coatings with various compositions are characterized. The effect of chemical composition on the microstructure and properties of coating is investigated. The results show that the microstructure and mechanical properties of Si-C-N coatings are very sensitive to chemical composition. The nanocrystalline/amorphous composite structure is beneficial to the coating's mechanical properties. It also reveals that Si-C-N coating with low Si and high C concentrations has the highest hardness (≥40 GPa) and the best wear property with dry friction coefficient about 0.2.     

退火对AlTiN多层薄膜结构及力学性能影响

使用TiAl合金靶,利用中频反应磁控溅射系统,通过交替改变氮气流量的方法,在高速钢(W18Cr4V)基体上沉积了一组氮含量周期性改变的AlTiN多层薄膜,并分别在600,700和800 ℃下真空退火热处理. 利用X射线衍射仪、场发射扫描电镜和高分辨透射电镜等方法研究了沉积态和退火态AlTiN多层薄膜组织和微观结构;AlTiN多层薄膜的力学和膜基结合性能用纳米压痕硬度仪、摩擦磨损仪以及划痕试验仪得到. 研究表明,采用沉积过程中周期改变氮气流量的方法,可以制备出稳定的、力学性能良好的AlTiN多层薄膜. 80 关键词： AlTiN多层薄膜 退火 微观结构 力学性能     

Corrosion properties of aluminium coatings deposited on sintered NdFeB by ion-beam-assisted deposition

Pure Al coatings were deposited by direct current (DC) magnetron sputtering to protect sintered NdFeB magnets. The effects of Ar⁺ ion-beam-assisted deposition (IBAD) on the structure and the corrosion behaviour of Al coatings were investigated. The Al coating prepared by DC magnetron sputtering with IBAD (IBAD-Al-coating) had fewer voids than the coating without IBAD (Al-coating). The corrosion behaviour of the Al-coated NdFeB specimens was investigated by potentiodynamic polarisation, a neutral salt spray (NSS) test, and electrochemical impedance spectroscopy (EIS). The pitting corrosion of the Al coatings always began at the voids of the grain boundaries. Bombardment by the Ar⁺ ion-beams effectively improved the corrosion resistance of the IBAD-Al-coating.     

Experimental study on Ti N coated racetrack-type ceramic pipe

Ti N film was coated on the internal surface of a racetrack-type ceramic pipe by three different methods:radio-frequency sputtering, DC sputtering and DC magnetron sputtering. The deposition rates of Ti N film under different coating methods were compared. The highest deposition rate was 156 nm/h, which was obtained by magnetron sputtering coating. Based on AFM, SEM and XPS test results, the properties of Ti N film, such as film roughness and surface morphology, were analyzed. Furthermore, the deposition rates were studied with two different cathode types, Ti wires and Ti plate. According to the SEM test results, the deposition rate of Ti N/Ti film was about 800 nm/h with Ti plate cathode by DC magnetron sputtering. Using Ti plate cathode rather than Ti wire cathode can greatly improve the film deposition rate.     

磁约束磁控溅射源的磁场设计

磁控溅射镀膜机中的磁场分布对靶材利用率有着重要影响。为了提高磁控溅射源的靶材利用率,设计组抛弃了传统的"跑道环"形式的磁场设计理念,而是将永磁体或电磁体分置溅射靶的两侧,使其在溅射靶表面上方产生磁约束(磁镜)磁场。本设计使用有限元分析方法对磁场进行仿真计算,通过模拟磁场计算结果和实测结果的比较,验证有限元方法的可靠性。Ansys有限元分析软件对磁场分布进行仿真模拟,大大简化了计算并缩短了设计周期。通过实验验证,磁约束磁场大大提高了靶材的利用率。