Synthesis and characterization of functionally graded nickel‐nickel coated ZrO2 composite coating

Electroless‐nickel plated ZrO₂ (NCZ) particles have been used to produce a functionally graded nickel‐electroless‐nickel plated ZrO₂ composite coating. So, electroless‐nickel plated ZrO₂ particles concentration was continuously increased from 0 to an optimum value in the electroplating bath (Watt's bath). The substrate was ST37 steel and the thickness of the coating was approximately 50 μm. Also a uniformly distributed nickel‐electroless‐nickel plated ZrO₂ composite coating has been manufactured as comparison. The composite coatings were characterized by scanning electron microscopy and energy‐dispersive X‐ray spectroscopy. Structure and phase composition were identified by X‐ray diffraction analysis. Microhardness of the coatings was evaluated by employing a Vickers instrument. Three‐point bend test was carried out to compare the adhesion strength of the coatings. Dry sliding wear tests were performed using a pin‐on‐disk wear apparatus. The electrochemical behavior of the coatings was studied by electrochemical impedance spectroscopy. The microhardness measurements showed that, with increasing the co‐electrodeposited electroless‐nickel plated ZrO₂ particle content in the nickel matrix, the microhardness increases from interface towards the surface of the functionally graded composite coating. Bend, wear and electrochemical test results confirmed that the functionally graded composite coating has higher adhesion, wear resistance and corrosion resistance as compared with the uniformly distributed coating. This has been attributed to lower mechanical mismatch between coating and substrate in functionally graded composite coating with respect to the uniformly distributed one.     

Biocompatible and mechanical properties of low temperature deposited quaternary (Ti, Al, V) N coatings on Ti6Al4V titanium alloy substrates

A series of quaternary (Ti, Al, V) N coating layers were obtained by low temperature reactive plasma sputtering in differing deposition conditions to improve the wear resistance and the biocompatibility of a titanium surgical alloy, specifically Ti-6Al-4V. Characterization of the mechanical properties, structure and the chemical composition of the coating layer was explored by microhardness test, ball against flat wear test, scanning electron microscopy and X-ray diffraction. The biocompatibility of the optimum coating layer (as determined by mechanical performance) was examined by a modified MTT toxicity test and by monitoring cell growth assessed by quantitative stereological analysis. The experimental results are encouraging, indicating that this low temperature deposited, dense, quaternary (Ti, Al, V) N coating layer exhibits improved mechanical properties such as high hardness and excellent adhesion to a Ti alloy substrate and is highly biocompatible.     

溅射方式对氧化铌涂层微观结构与性能的影响

分别采用射频溅射和射频反应溅射方式在AZ31镁合金表面制备了氧化铌涂层,并利用扫描电子显微镜、X射线衍射仪、X射线光电子能谱仪、多功能材料表面性能试验仪和电化学工作站对比研究了两种涂层的微观形貌、物相组成、附着力和耐腐蚀性能。研究结果表明,两种涂层都呈非晶柱状结构,铌的价态为Nb⁵⁺,对AZ31镁合金的腐蚀保护率达93%以上;与射频溅射沉积的氧化铌涂层相比,射频反应溅射沉积的氧化铌涂层的表面致密性和耐蚀性能更强,附着力提高约7.4倍。     

碱性条件下Fe-P-B合金电镀

研究了碱性溶液中镀液组成、阴极电流密度、温度、pH值对Fe-P-B合金电镀层沉积速率和组成的影响,优化了工艺,在最佳工艺条件下获得Fe-P-B镀层,并对镀层的耐腐蚀性、结构和结合力进行了分析.结果表明:提高镀液中硫酸亚铁铵含量、溶液pH值、温度和电流密度,镀层沉积速率增加;提高镀液中次亚磷酸钠、丙二酸和硼氢化钠含量,镀层沉积速率先增后降低,出现一个极大值;镀层中B含量的增加会使P含量降低,但提高电流密度和镀液温度时二者都有所增加;在最佳工艺条件下获得的Fe-P-B合金镀层为非晶态结构,和基体结合力优良,耐蚀性良好,在15%NaoH溶液中的耐腐蚀性优于在5%NaCl溶液中.     

钛合金着色技术的研究

利用正交试验法研究了在磷酸-冰乙酸体系中磷酸、冰乙酸、添加剂、氧化电压、电解液温度、氧化时间等对钛阳极氧化膜的影响,确定了最佳工艺条件.结果表明,在采用以Ce作为添加剂的电解液中处理后所得到的钛合金着色膜呈蓝色、光亮美观,具有优良的耐蚀性、耐磨性和良好的附着力.     

A comparative study of a vitreous biological composition suitable for coating steel prostheses

A correlation between composition and quality of a biological glass used as a bioglaze and an industrial glaze for sheet-steel coating was carried out. Apart from the extremely different conditions, particularly relative to the temperature for application of the coating to the metallic substrate, it was noted that the compositions are not very much different; this led us to think that the doping of the vitreous system with substances favouring the bonding of glaze to support (according what has been suggested by enamellists) is trustworthy in this case too. Some hypotheses relative to the role of nickel and the fluidity of the vitreous system were made to explain the observations, and to suggest the best way to improve the adhesion of metal to glaze.     

Glass-ceramic-metal composites for making graded seals in prosthetic devices

The possibility of using glass-ceramic-metal composites as graded seals between dense cores of prostheses and a porous glass-ceramic coating, which would promote a direct bond with the bone has been investigated, particularly with respect to thermal and elastic properties. Before binding them to a core, bulk composite materials have been prepared in order to study their properties.These materials have been obtained from powdered mixtures of a calcium alumino-phosphate glass (CAP) with increasing volume fractions (3.5–50%) of various metals or alloys: titanium, 316 L stainless steel, cobalt-chromium 788 alloy. They have been synthesized by hot pressing immediately followed by a heat treatment to obtain ceramicization of the glass matrix.Elastic and thermal properties have been determined. The values of elastic moduli and average linear thermal expansion coefficients lie within those of glass-ceramic CAP and those of the corresponding metal. Mechanical properties have been also measured. The material can withstand about four times the body weight when materials are bound to a more rigid metal or alloy.     

An investigation into the mechanical and tribological properties of plasma electrolytic oxidation and hard-anodized coatings on 6082 aluminum alloy

A ceramic coating on AA6082 aluminum alloy prepared by plasma electrolytic oxidation (PEO) has been studied and compared against a sulphuric acid hard-anodized coating on the same alloy. Surface morphology and microstructures of the coatings have been examined by scanning electron microscopy. X-ray diffraction is used to determine the phase composition of the coatings. The adhesion strength of the coatings has been evaluated using a scratch test method. The coating's mechanical properties such elastic modulus and hardness data have been generated using a dynamic ultra-microhardness tester. Sliding wear tests with different loading rates are performed on the coatings in order to assess their wear resistance. Test results show that the PEO treated samples exhibit significantly better mechanical properties compared to hard anodized samples. The elastic modulus and hardness of the PEO coating are 2-3 times greater than of the hard anodized coating and subsequently, an improved wear resistance of the PEO coating has been achieved. The mechanical properties of the coatings and their relations to their tribological performance are discussed.     

Erosions‐Korrosions‐Untersuchungen an gradierten Multilayer‐Chromkarbidschichten

Erosion corrosion of graded chromium carbide coatings in multi layer structure So far PVD‐ and PECVD‐Layers have proved their value as wear protection mainly on cutting tools for machining. Depending on the composition of the layers not only a reduction in wear but also a reduction in friction is possible, e.g. by integration of hydrogen containing carbon. Furthermore such carbon containing layers use to be electrochemically inert. Thus they don’t corrode in aqueous media. Because they do also have a very dense structure, an application as corrosion protection seems to be promising. For the intended investigations under service‐like erosiv‐corrosiv loading a new testing rig was developed and constructed. The erosiv‐corrosiv loading was achieved by exposure of coated specimen to a flowing medium, that contains abrasive corund‐particles. Thus the erosion‐corrosion‐behaviour of new graded Multilayer‐Chromiumcarbide‐Coatings should be investigated. The aim was to identify the mechanisms of deterioration to promote a further developement of these layers. In addition the potential of PVD/PECVD‐coated low‐alloy steel to be in‐service under such conditions should be evaluated. For comparison an up‐to‐date industrial DLC‐coating and a high‐alloy duplex‐steel were also investigated. As a result of the conducted investigations an application of PVD‐/PECVD‐coated low‐alloy steel under erosive‐corrosive conditions with impingement wear could not yet be recommended. However the graded Multilayer‐Chromiumcarbide‐Coatings have the potential for a good erosion‐corrosion‐protection, if erosion promoting flaws are avoided. Because hard PVD‐ and PECVD‐coatings are relative brittle, a loading with hard particles, which hit the surface under a high angle, is very tough. Hence the question is, if the investigated layers possibly have a better wear behaviour under more abrasive loading in a more tangential flowing medium, which is also typical for in‐service‐conditions. This is intended to be investigated in future tests.     

Modeling of Substrate-Coating Thermal Interaction During High Velocity Oxy-Fuel (HVOF) Spraying of WC-Ni Powder

The mathematical simulation of thermal processes occurring during the formation of a WC-Ni coating on a low alloy steel by HVOF spraying has been carried out. The factors assessed during the simulation include overall temperature changes, the solidification of the coating, the melting and subsequent solidification of the interface regions of the substrate and the thermal interactions between different layers of the coating

The mathematical simulation of parameters which could influence the structural characteristics of the coating and the interfacial region of the substrate has also been undertaken. The variations in the solidification velocity, the thermal gradients and the cooling velocity in the first layer of the coating have been determined. Similar parameters have been determined for the substrate but in this case attention has also been given to the melting velocity. The influence of these parameters on the formation of amorphous and noncrystalline structure in the coating is discussed together with the development of fine crystalline structures in the interfacial region of the substrate. The results obtained agree well with those obtained by direct metallographic examination of the coating and the substrate interfacial regions

The optimum conditions for the formation of good structures in the coating and the adjacent substrate are estimated.     

Hochreflektierende Beschichtungen auf Kunststoffoptiken

Metallized polymer substrates offering highest reflectance are not yet state of the art. Coating organic substrate materials is still a task that is connected with multiple problems. Insufficient adhesion of coatings on polymer substrates represents one of the main difficulties. We could show by experiment that aluminium and silver layers indicate good coating adhesion on many different polymers if they are deposited by vacuum evaporation considering certain process parameters. High reflectance values and a good climatic stability of the metal coated polymer parts are other important challenges to plastic mirrors. By performing roughness measurements on the different polymer samples and by comparing reflection values obtained after coating these samples the impact of the polymers surface quality on the reflectance after metal coating has been investigated. Particularly high reflectance above 97% was realized with a protected silver mirror as well as with dielectric enhanced aluminium. Applying these layer systems excellent reflection properties has been obtained on several plastic substrates comparable to those on glass mirrors. Furthermore the dielectric layers used for reflection enhancement showed the ability to protect the aluminium coating against climatic influences.     

Corrosion protection of AM60B magnesium alloy by application of electroless nickel coating via a new chrome-free pretreatment

Cerium–vanadium (Ce–V) conversion coating was proposed as a new pretreatment for application of electroless Ni–P coating on AM60B magnesium alloy to replace the traditional chromium oxide pretreatment. Morphology and chemical composition of the conversion coating were investigated. The subsequent Ni–P coating deposited on the conversion coating was also characterized by morphology, chemical composition, microstructure, corrosion protection performance and micro-hardness. A uniform, compact and pore-free electroless coating with a moderate concentration of phosphorus (7.78 wt%) was obtained. The electroless coating showed a nobler open-circuit potential than that of the bare alloy during the first 13 h of immersion in 3.5 wt% NaCl solution. Also, the sample plated with the Ce–V conversion coating showed lower corrosion current density than the sample plated with traditional chromium oxide pretreatment. The micro-hardness of the bare alloy was significantly increased after electroless coating. The electroless coating is pore-free and there is suitable adhesion between the coating and alloy substrate.     

Sintering characteristics of nano-sized Ag–Pd–glass composite powders with high Pd content

Nano-sized Ag–Pd (50–50) alloy powders coated with Pb-based glass material with low and high glass transition temperature are directly prepared by high-temperature flame spray pyrolysis. Nano-sized Ag–Pd–glass composite powder is formed from the evaporated vapors by nucleation and growth process, and then glass material moves out to the outside of the powder by crystallization process of alloy. The thickness of the glass coating layer measured from the TEM image is 2.8 nm. The mass changes of the Ag–Pd alloy and Ag–Pd–glass composite powders in the TG analysis under 900 °C are 10.9 and 6.8%, respectively. Glass materials improve the uniformity and density of the Ag–Pd electrode layers by act as sintering agent and adhesion improvement. The Ag–Pd electrode formed from the composite powders with high glass transition temperature glass material has thin and uniform thickness. The specific resistances of the electrodes formed from the nano-sized Ag–Pd–glass composite powders are 0.27, 0.09, and 0.03 mΩ cm at firing temperatures of 700, 800, and 900 °C, respectively.     

AZ91D镁合金表面Ni-P化学镀层的微观组织与性能

以直接化学镀的方法在AZ91D镁合金表面制备了光亮、均匀、致密、厚度达40μm的Ni-P合金镀层,用现代分析技术分析了镀层的微观形貌、组织成分、显微硬度、结合力以及耐蚀性能.结果表明:Ni-P镀层属于中磷镀层,微晶结构,表面形貌呈胞状;镀层与基体结合良好;镀层的显微硬度比基体提高了4倍;镀层与抛光基体的结合力比未抛光的高,基体表面保持机加工状态的镀层破坏临界载荷为80.6 N;镀层具有较好的耐蚀性能.     

Nano-crystallization and surface analysis of electrolytic ZrO2 coatings on Co-Cr alloy

Zirconia coatings were formed on Co-Cr substrates by electrolytic deposition. The microstructure of electrolytic zirconia-coated films on Co-Cr substrates was examined. According to the results of ESCA, the bonding energies of ZrO₂ coating surface layer which changed with the annealing temperature from 400 °C, 500 °C to 600 °C are attributed to amorphous (a), tetragonal (t) and monoclinic (m) structure, respectively. The X-ray diffraction (XRD) of the coatings on the Co-Cr substrates annealed at 400, 500 and 600 °C revealed the major crystallization from m through t and then to m+t. However, TEM observations clearly showed that the interface layer of the coatings were nanosize crystallites, first the formation of tetragonal and monoclinic ZrO₂ structures. These different phase transformations are mainly due to the different surface energy of ZrO₂ coating in air, in bulk or on Co-Cr alloy. © 2001 Kluwer Academic Publishers     

Surface effect of flame treatments on polypropylene

A study of the effects of flame treatments on a high-impact polypropylene has been performed. Both physico-chemical and mechanical properties have been investigated. The surface chemical composition has been determined by XPS, while the surface tension and the polarity were obtained through contact angle measurements. A remarkable agreement in the behaviour of chemical composition and polarity has been found, emphasizing the role of carbonyl and carboxyl groups. The adhesion of treated and untreated samples to paint coatings hua been mechanically tested. The force of adhesion remains quite constant after the first flame treatment. This suggests the importance of chemical interactions of the coating with the first layers of the polymer.     

锌合金表面涂装前磷化处理对膜层结合力的影响

锌合金活泼、易腐蚀,在其表面直接喷涂涂层的结合力较差,为了提高锌合金表面与涂层的结合力,对锌合金基材作磷化处理和磷化后封闭处理再喷涂聚氨酯漆膜,探讨了磷化处理及封闭处理对锌合金表面膜层间结合力的影响,并应用扫描电镜(SEM)和X射线衍射仪(XRD)对磷化膜表面形貌、物相组成及成分等进行研究。结果表明:锌合金表面直接喷涂聚氨酯漆膜,漆膜与锌合金基材的结合力差,结合力等级大于5级;而锌合金表面不管是磷化后直接喷漆还是磷化后封闭处理再喷漆均能极大提高涂层与基体的结合力,其结合力等级均小于2级;封闭处理有助于降低磷化膜的孔隙率,磷化膜经封闭处理后孔隙率由13.9%降到3.5%;封闭处理会降低磷化膜与漆膜的结合力。     

Deposition of biomimetic biocompatible oxides on metallic glass surface by electro-discharge coating process

Bulk metallic glass demonstrates superior mechanical properties and excellent bio-mechanical stability compared to routinely used biomaterials like titanium, cobalt-chromium, stainless steel, et cetera. However, the metallic glass surface do not easily adhere to the leaving tissues due to native bio-inert oxide layer, which have poor wear resistance and low hardness. In this current study an innovative method for surface coating of bulk metallic glass by mixing hydroxyapatite powder during electro-discharge machining has been employed. A biomimetic nano-porous bio-ceramic layer of oxides and carbides was deposited on metallic glass surface. The modified surface integrity and composition were investigated by scanning electron microscopy, energy-dispersive x-ray spectroscopy, and x-ray diffraction characterization techniques. The characterization results confirmed the formation of a natural bone-like nano-porous surface topography on the metallic glass surface using a novel hydroxyapatite-mixed electro-discharge coating process. In addition, a favourable surface chemistry in the form of bioceramic carbides (zirconium carbide, titanium carbide) and zirconium oxide layers, was achieved.     

PVD‐Schutzschichten für Werkzeuge des Präzisionsblankpressens

PVD protective coatings for precision molding tools Precision glass molding (PGM) is a replicative hot forming process for the production of complex optical components, such as aspherical lenses for digital and mobile phone cameras or optical elements for laser systems. The efficiency and thus also the profitability of the PGM depend on the unit price per pressed component, which correlates primarily with the service lifetime of the pressing tools. To increase tool lifetime, the tool surfaces are coated with protective coatings based on precious metals or carbon using physical vapour deposition (PVD). The PVD coating technology enables the deposition of thin coatings, which also follow more complex surface geometries and achieve a high surface quality. PVD coatings are also commonly used to protect tools from wear and corrosion. This paper presents two chromium‐based nitride hard coatings produced by an industrial PVD unit and investigated for their applicability for PGM. Two different coating architectures were implemented, on the one hand a single coating chromium aluminium nitride (Cr,Al)N coating and on the other hand a nanolaminar CrN/AlN coating with alternating layers of chromium nitride and aluminium nitride. The latter is a coating consisting of hundreds of nano‐layers, only a few nanometers thick. Both coatings, (Cr,Al)N and CrN/AlN, each have a thickness of s ～ 300 nm in order to follow the tool contour as closely as possible. The properties of the coating systems, which are of particular relevance for PGM, are considered. These include on the one hand the adhesion of glass, the roughness and topography of the surface and the adhesion between the coating and the tool material. In addition, the barrier effect of the coatings against diffusion of oxygen was investigated. In order to reproduce the thermal boundary conditions of the PGM, thermocyclic aging tests are performed and their influence on the different properties is described.     

Stepwise graded refractive-index profiles for design of a narrow-bandpass filter

A combination of stepwise graded refractive-index profiles and a cavity structure is used for designing narrow-bandpass filters of TiO(2)/SiO(2) multilayer films upon BK7 glass substrates. Symmetrical profiles of stepwise graded refractive indices result in high transmittance of passbands for the designed filters. The bandwidth of the narrow-bandpass filter is controlled by adjustment of parameters such as the thickness and the number of layers in the multilayer stack. This design is proposed as a new and simple method for coating synthesis of optical filters.