Surface characterisation and electrochemical behaviour of porous titanium dioxide coated 316L stainless steel for orthopaedic applications

Porous titanium dioxide was coated on surgical grade 316L stainless steel (SS) and its role on the corrosion protection and enhanced biocompatibility of the materials was studied. X-ray diffraction analysis (XRD), atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX) were carried out to characterise the surface morphology and also to understand the structure of the as synthesised coating on the substrates. The corrosion behaviour of titanium dioxide coated samples in simulated body fluid was evaluated using polarisation and impedance spectroscopy studies. The results reveal that the titanium dioxide coated 316L SS exhibit a higher corrosion resistance than the uncoated 316L SS. The titanium dioxide coated surface is porous, uniform and also it acts as a barrier layer to metallic substrate and the porous titanium dioxide coating induces the formation of hydroxyapatite layer on the metal surface.     

The microstructure, mechanical and friction properties of protective diamond like carbon films on magnesium alloy

Protective hard coatings deposited on magnesium alloys are believed to be effective for overcoming their poor wear properties. In this work, diamond-like carbon (DLC) films as hard protective films were deposited on AZ91 magnesium alloy by arc ion plating under negative pulse bias voltages ranging from 0 to −200 V. The microstructure, composition and mechanical properties of the DLC films were analyzed by scanning electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy and nanoindentation. The tribological behavior of uncoated and coated AZ91 magnesium alloy was investigated using a ball-on-disk tribotester. The results show that the negative pulse bias voltage used for film deposition has a significant effect on the sp³ carbon content and mechanical properties of the deposited DLC films. A maximum sp³ content of 33.3% was obtained at −100 V, resulting in a high hardness of 28.6 GPa and elastic modulus of 300.0 GPa. The DLC films showed very good adhesion to the AZ91 magnesium alloy with no observable cracks and delamination even during friction testing. Compared with the uncoated AZ91 magnesium alloy, the magnesium alloy coated with DLC films exhibits a low friction coefficient and a narrow, shallow wear track. The wear resistance and surface hardness of AZ91 magnesium alloy can be significantly improved by coating a layer of DLC protective film due to its high hardness and low friction coefficient.     

An updated overview of diamond-like carbon coating in tribology

During the last two decades, the industry (including scientists) has focused on diamond-like carbon (DLC) coating because of its wide range of application in various fields. This material has numerous applications in mechanical, electrical, tribological, biomedical, and optical fields. Severe friction and wear in some machine parts consumes high amount of energy, which makes the process energy inefficient. Thus, DLC coating can be an effective means to lower the friction and wear rate. Some important process variables that affect the tribological characteristics of DLC coating are adhesion promoter intermediate layer, substrate surface roughness, hydrogen incorporation or hydrogen non involvement, and coating deposition parameters (e.g., bias voltage, etching, current, precursor gas, time, and substrate temperature). Working condition of DLC-coated parts also affects the tribological characteristics, such as temperature, sliding speed and load, relative humidity, counter surface, and lubrication media (DLC additive interaction). Different types of lubricated oils and additives are used in engine parts to minimize friction and wear. DLC can be coated to the respective engine parts; however, DLC does not behave accordingly after coating because of lubricant oil and additive interaction with DLC. Some additive interacts positively and some behave negatively because of the tribochemical reactions between DLC coating and additives. Numerous conflicting views have been presented by several researchers regarding this coating additive interaction, resulting in unclear determination of true mechanism of such interaction. However, lubricant additive has been established to be more inert to DLC coating compared with uncoated metal surface because the additive is fabricated in such a way that it can react with metal surfaces. In this article, the tribological characteristics of different types of DLC coating in dry and lubricated conditions will be presented, and their behavior will be discussed in relation to working condition and processing parameters.     

多腔耦合微波表面波PECVD法沉积 DLC薄膜研究

报道了利用多腔耦合微波表面波等离子体增强化学气相沉积(PECVD)的方法制备类金刚石(DLC)薄膜。通过发射光谱(OES)测量,对Ar等离子体中的各种放电参数以及全部四个腔室内放电的均匀性作出评估。采用表面轮廓仪测量了薄膜的厚度;薄膜的表面形貌、组成结构通过原子力显微镜(AFM)、激光拉曼光谱和X射线衍射光谱(XPS)进行了表征。在12.5μm厚度的有机薄膜聚酯(PET)表面沉积一定厚度DLC后,通过测量水蒸气透过率(WVTR)对DLC薄膜的阻隔性能进行了研究。结果表明,这种多腔耦合微波表面波等离子体装置,不仅能够实现四个腔室同时相对均匀的放电,也能够实现单个腔室的轴向均匀放电。制备的DLC薄膜结构致密、成分均匀,可以使PET薄膜阻隔性能提高约20倍。     

大口径光学元件薄膜厚度均匀性修正

 研究了2.2 m高真空箱式镀膜机镀膜时的实际膜厚分布情况。对非球面和平面光学元件,分别采用行星夹具和平面公转夹具并利用修正板调节膜厚均匀性。从实验上实现了大口径薄膜均匀性的调节,并获得较为理想的结果。口径在700 mm范围内,对于凹面均匀性可以控制在0.7%以内,平面均匀性在1%以内;口径在1 200 mm范围内凹面元件均匀性可控制在1%以内,平面1 300 mm口径以内窗口均匀性可控制在1%以内。镀制了口径在400~1 300 mm的多种天文观测上使用的反射镜、增透膜等,获得了理想的光谱曲线与较好的使用效果。     

锗红外光学窗口海洋潮差区腐蚀特性研究

对未镀膜及表面镀类金刚石（DLC）膜锗（Ge）红外光学窗口在中国南海海域进行了海洋潮差区腐蚀试验研究,观察测试海洋腐蚀试验前后Ge窗口及膜层的表面形貌和腐蚀速率,报道了腐蚀结果,分析了Ge窗口在海洋潮差区腐蚀特性,探讨了Ge窗口在海洋腐蚀破坏机理,得出了延长Ge窗口在海洋环境下使用寿命的研究方向。研究结果对于了解Ge窗...     

Gas barrier properties of diamond-like carbon films coated on PTFE

Diamond-like carbon (DLC) films were deposited on polytetrafluoroethylene (PTFE) using radio frequency (RF) plasma-enhanced chemical vapour deposition (PE-CVD). Before the DLC coating, the PTFE substrate was modified with a N₂ plasma pre-treatment to enhance the adhesive strength of the DLC to the substrate. The influences of the N₂ plasma pre-treatment and process pressure on the gas permeation properties of these DLC-coated PTFE samples were investigated. In the Raman spectra, the G peak position shifted to a lower wave number with increasing process pressure. With scanning electron microscopy (SEM), a network of microcracks was observed on the surface of the DLC film without N₂ plasma pre-treatment. The density of these cracks decreased with increasing process pressure. In the film subjected to a N₂ plasma pre-treatment, no cracks were observed at any process pressure. In the gas barrier test, the gas permeation decreased drastically with increasing film thickness and saturated at a thickness of 0.2 μm. The DLC-coated PTFE with the N₂ plasma pre-treatment exhibited a greater reduction in gas permeation than did the samples without pre-treatment. For both sample types, gas permeation decreased with increasing process pressure.     

空心阴极辉光放电包覆铜纳米粉末

 简要叙述了自悬浮定向流方法制备铜纳米粉末的原理和包覆层薄膜的生长机理，采用空心阴极辉光放电对铜纳米粉末进行有机包覆，实验中CH4和H2的流量分别为6 ml/min和12 ml/min，工作电压为450 V，衬底与空心阴极的底端距离为2 cm，背景真空和工作气压分别为6 Pa和100 Pa，沉积速率为7.5 nm/min。用透射电镜(TEM)对铜纳米粉末进行了观察和分析，结果表明：铜纳米粉末呈球状，其粒径分布在10～100 nm之间, 平均粒径大小为50 nm；其包覆层的厚度大约为15 nm，而且该厚度可以通过调节空心阴极辉光放电的参数来控制。     

Formation of Al2O3 coatings on NiTi alloy by micro-arc oxidation method

Rough and porous Al₂O₃ coatings containing Ca and P were prepared on Ti–50.8 at.% Ni alloy by micro-arc oxidation (MAO) technique. The microstructure, elemental and phase composition of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS) and thin-film X-ray diffraction (TF-XRD). The thickness of the coatings was measured by eddy current coating thickness gauge. The corrosion resistance and the nickel release of the coated and uncoated samples were examined by potentiodynamic polarization tests and immersion tests in Hank’s solution, respectively. The results show that the coatings are mainly composed of γ-Al₂O₃ crystal phase. The Ni content of the coatings is about 3.5 at.%, which is greatly lower than that of NiTi substrate. With increasing treatment time, both thickness and roughness of the coatings increase. The corrosion resistance of the coated samples is about two orders of magnitude higher than that of the uncoated NiTi alloy. The concentration of Ni released from coated NiTi samples is much lower than that of uncoated NiTi sample. It can be reduced in the factor of one-seventh compared with the uncoated NiTi sample after 3 weeks immersion in Hank’s solution.     

Characterization of coated optical fibers by Fourier-domain optical coherence tomography

Fourier-domain optical coherence tomography is used to image the cross sections of coated optical fibers. A standard single-mode fiber with a dual coating and a hard-clad silica fiber with a single thin low-index coating are studied. The individual coating dimensions, coated and uncoated fiber diameters, and the fiber coating's concentricity are retrieved from a single measurement.     

Interaction of intense IR laser radiation with a-C:H protective coatings

The results of a determination of the optical breakdown thresholds of air near the surface of copper laser mirrors with a-C:H protective coating by intense pulsed 10.6 μm radiation are analyzed and systematized. It is shown that there is no correlation between the breakdown threshold of a coated mirror, the reflectance of the coating, and the breakdown threshold of the initial copper surface. Experimental dependences of the threshold of optical breakdown of coated mirrors on the a-C:H thickness and deposition rate as well as the storage time of the mirrors are given. Estimates are made of the rise in the surface temperature in the irradiation zone for the case of an ideal adhesive contact and calculations are made of the damage threshold of the coating in the case that the adhesive contact between the mirror and the coating is impaired. The effect of the a-C:H coating properties and the conditions at the polished metal surface-protective coating interface on the optical breakdown threshold is discussed. Zh. Tekh. Fiz. 68, 59–66 (September 1998)     

Properties of TiN coating on 45# steel for inner surface modification by grid-enhanced plasma source ion implantation method

Using a new inner surface modification method named GEPSII (grid-enhanced plasma source ion implantation), which is designed for inner surface modification of tubular work pieces, we successfully produced polycrystalline TiN coating on 0.45% C steel (45^# steel) samples. Compared with the uncoated 45^# steel sample, the electrochemical corrosion test on the coated 45^# steel samples presents evident improvement in their corrosion resistance. Two implanted voltages, direct current (－2kV) and pulsed negative voltage (－10kV), are applied on the substrates. It is shown that the direct current implantation is more effective than the pulsed implantation in the surface corrosion resistance. AES depth profile shows that coating thickness is about tens of nanometres. The preferred orientations expressed by peaks at (111) and (200) can be seen clearly in XRD patterns.     

大功率半导体激光器的可靠性研究

对InGaAs/AlGaAs和InGaAsP/GaAs有源区含铝的915nm和无铝的808nm腔面镀膜及未镀膜的大功率半导体激光器进行了老化实验。在老化前通过综合参数测试仪测试两种激光器的斜率效率、阈值电流，发现有腔面膜的激光器比无腔面膜的激光器的阈值电流降低25％以上。在1.2倍阈值电流下，恒流老化40h左右，老化后再分别测试它们的阈值电流、功率参数，我们发现在老化后未镀膜的激光器的阈值电流和镀有腔面膜的激光器相比增加25mA以上，输出功率也比镀过腔面膜的减小到了原来的1／2，可见腔面保护对于延长激光器的寿命是很重要的。     

The improvement of moisture resistance and thermal stability of Ca3SiO4Cl2:Eu phosphor coated with SiO2

Green-emitting phosphors Ca₃SiO₄Cl₂:Eu²⁺ were prepared by the high temperature solid-state method. Sol-gel process was adopted to encapsulate the as-prepared phosphors with tetraethylorthosilicate (TEOS) as silicon coating reagent. Fluorescence spectrometer, scanning electron microscopy (SEM) and powder X-ray diffraction (XRD) patterns were employed to characterize the emission spectra, the surface morphologies and the phase structures, respectively. The chemical stability testing was operated by the method of soaking the phosphors in deionized water and roasting them at different temperatures. The results indicated that the surfaces of the green phosphors were evenly coated by SiO₂ and the phase structure of the coated phosphors remained the same as the uncoated samples. The luminance centre of Eu²⁺ did not shift after surface treatment and the luminance intensity of coated phosphors was lower than that of the uncoated samples. The results demonstrated that the water-resistance stability of the coated phosphor was improved to some degree because the pH value and the luminance intensity variation were both smaller than the uncoated phosphor after steeping within the same time. Moreover, the thermal stability of coated phosphors was enhanced obviously compared to the original samples based on the temperature dependent emission spectra measurement.     

Investigations of Pulse‐Plasma‐Polymer Coating on TiO2 Nanoparticles and Their Dispersion

An amorphous acrylic acid (AA) polymer coating was generated on TiO₂ nanoparticles through pulse radio frequency (RF) plasma polymerization. The AA plasma synthesis mechanism was studied by its optical emission spectrum. The chemical structures of AA–plasma‐polymer were carefully investigated by Fourier transform infrared spectroscopy (FTIR). The dispersion behaviors of AA‐coated and uncoated TiO₂ nanoparticles in glycol solution were characterized by ultraviolet absorbency and particle size distribution measurements. The results showed that the aggregation of TiO₂ nanoparticles in glycol solution was effectively lowered and the dispersion was improved a lot after AA–plasma‐polymer coating. The pulse plasma coating parameters played an important role in the dispersion enhancement of TiO₂ nanoparticles. By properly regulating the pulse discharge parameters, the system could gain the highest radical–monomer reactions rate, the most compatible functional groups on the nanoparticles, and the best dispersion in the background media.     

自动聚焦激光诱导击穿光谱远程测量系统

激光诱导击穿光谱(LIBS)技术具有非接触测量、无需样品预处理以及快速多元素同时分析等特点,适合于高温、高压、真空、有毒以及敌对环境等仪器和操作人员无法靠近观测对象的应用中。LIBS技术结合望远镜系统可以实现物质成分的远距离检测与分析。搭建了一套可自动聚焦的LIBS远程测量系统。该系统中的望远镜采用Schwarzschild结构,由一块凹球面反射镜和一块凸球面反射镜组成。两块球面反射镜共轴安装。其中凸面反射镜安装在电控精密平移台上,电动平移台可带动凸面反射镜沿光轴移动。通过调整凸面反射镜的位置,改变凸面反射镜和凹面反射镜的间距,进而改变系统的焦距,实现对不同距离的样品进行光谱测量。该结构的优点在于：激光聚焦光路与信号光采集光路相同,便于安装和调试;望远镜系统采用全反射式光路,适用于紫外波段检测;只包括两个球面反射镜,结构紧凑,元件容易加工。望远镜系统调焦距离为1.5～3.6 m,聚焦光斑直径约为0.5~1.0 mm。使用该系统对铜样品进行了LIBS实验,确认了Cu元素的特征谱线。通过测量Cu元素的LIBS特征谱线(Cu Ⅰ 223.01 nm, Cu Ⅰ 224.43 nm)峰面积和反射镜间距之间关系,得到了激光的最优聚焦位置。实验结果表明,该系统能够完成样品的远程激发和LIBS光谱测量,并能够对不同距离的样品进行自动聚焦。     

Preparation and properties of ceramic coating on Q235 carbon steel by plasma electrolytic oxidation

Ceramic coating was achieved on Q235 carbon steel by PEO (plasma electrolytic oxidation, PEO) without any pretreatment in sodium aluminate system. The discharge process as well as the accompanied surface morphology evolution was analyzed. The phase and elemental composition of the coatings were also investigated. The corrosion, mechanical and tribological properties of the ceramic coating were primarily studied. It is found that the coating surface was porous and the thickness of the coating was about 120 μm. The coating mainly consisted of FeAl₂O₄, Fe₃O₄ and a little γ-A1₂O₃. The corrosion current of the coated sample was 3.082 × 10⁻⁷ A/cm², which was decreased by two orders of magnitude compared with the uncoated one. The micro hardness of the ceramic coating was 1210 Hv, which was about three times as that of the uncoated sample. The friction coefficient of coated sample was also well improved. Investigations revealed that PEO provided a promising technique for preparation of protective ceramic coatings on steels.     

FABRICATION AND APPLICATION OF NEAR-FIELD OPTICAL FIBRE PROBE

In this paper, the fabrication of a large cone angle near-field optical fibre probe, using the two-step chemical etching method and bent probe, is introduced, and the controlling parameters of the coated Cr－Al film at the probe tip are presented. The scanning electron microscopy images display that the tip diameter of the uncoated large cone angle fibre probe obtained is less than 50nm, the cone angle over 90°, and the diameter of light aperture at the coated probe tip is less than 100nm. The measured results of the optical transmission efficiency for various probe tips show that the uncoated straight optical fibre probe, film-coated straight probe and film-coated bent probe are 3×10^-1, 2×10^-3, and 1×10^-4 times that of the flat fibre probe, respectively. In addition, the force images and near-field optical images of a standard sample are acquired using a large cone angle and film-coated bent probe.     

The effect of TiN nanoparticles deposition with different number of shots on SS316L by plasma focus device

In this paper, we present the result of TiN nanocrystalline deposition on SS316L, using a 4 kJ plasma focus (PF) device for 10, 20, and 30 focus shots. The effect of different number of focus shots on micro-structural changes of thin film is characterized by field emission scanning electron microscope. Existence of grains in different size confirms the formation of TiN nanocrystals on the surface of SS316L substrate. X-ray diffraction (XRD) reveals the formation of a nanocrystalline titanium nitride coating on the surface of SS316L samples. The crystalline size of TiN obtained from XRD data is strongly dependent on the number of focus shots. Thickness of the elements found on the surface of the treated sample that obtain by Rutherford backscattering spectroscopy (RBS) analysis is in the range of 150×10¹⁵?200×10¹⁵ atoms/cm². All the existence elements in the coated samples are identified by Particle Induced X-ray Emission (PIXE) spectra. Investigation on the corrosion resistance of TiN coatings was performed using an electrochemical potentiodynamic polarization. Our results suggest that TiN nanocrystalline implantation with proper ion fluences using PF can significantly improve the corrosion resistance of SS316L.     

Characterization of atomic layer deposition coated cutting tools by X-ray photoelectron spectroscopy and examination of cutting performance

Abstract

The performance of cutting tools was examined, involving synthesis of a 10?nm thin film of Aluminum oxide using atomic layer deposition. Characterization of coated and uncoated cutting tools was done by several methods. scanning electron microscopy was used and the images were compared with each other. Chemical characterization was performed by X-ray diffraction and X-ray photoelectron spectroscopy. Coated and uncoated cutting tools were tested with steel material in turning tests. After turning, it was observed that the adhesion effect was reduced to a large extent in turning with coated tool. It was observed that the coating showed stability at high temperatures during cutting and the cutting performance was increased. The main advantage of the coating was that the tools produced were more environmentally friendly, with a longer useful life and they were easier to recycle.