Hydrothermal calcification surface modification of biomedical tantalum

Tantalum (Ta) as a new type of medical metal is now utilized in several orthopedic applications due to its excellent fracture toughness and workability,high cor...     

甲酰胺浓度对38CrMoAl钢液相等离子电解渗氮过程的影响

采用液相等离子电解渗氮技术,研究了不同甲酰胺浓度对38CrMoAl钢渗氮层组织及性能的影响。利用OM、SEM、XRD观察分析渗氮层的微观组织结构和物相构成,RF-GDOES和Parstat2273电化学工作站分别表征渗氮层的元素分布和耐蚀性,并测试分析了渗层截面的显微硬度。结果表明,随着电解液中甲酰胺浓度的升高,渗氮致密层、白亮层、扩散层厚度呈先增加后降低的趋势,渗氮层最大显微硬度值呈增加的趋势;当甲酰胺浓度升高至70%时渗氮层达到最大,为125μm,白亮层为51μm;渗氮后扩散层硬度值较高,而心部组织硬度较未处理试样提升约2倍;渗氮层表层主要含Fe2N和Fe3N相,扩散层以Fe16N2、FeN相为主,过渡层主要为α-Fe、FeN0.097相;渗氮层的耐蚀性优于未经处理试样。     

Flake tantalum powder for manufacturing electrolytic capacitors

The FTP200 flake tantalum powder was introduced.The microstructures of the powder with leaf-like primary particles having an average flakiness of 2 to 20 and porous agglomerated particles were observed.The chemical composition,physical properties,and electrical properties of the FTP200 powder were compared with those of the FTW300 nodular powder.The FTP200 powder is more sinter-resistant,and the surface area of the flake tantalum powder under sintering at high temperature has less loss than that of the nodular tantalum powder.The specific capacitance of the flake tantalum powder is higher than that of the nodular tantalum powder with the same surface area when anodized at high voltage.Thus,the flake tantalum powder is suitable for manufacturing tantalum solid electrolytic capacitors in the range of median and high（20-63 V） voltages.     

Surface characterisation of DC plasma electrolytic oxidation treated 6082 aluminium alloy: Effect of current density and electrolyte concentration

Plasma electrolytic oxidation (PEO) is a specialised but well-developed process which has found applications in aerospace, oil/gas, textile, chemical, electrical and biomedical sectors. A novel range of coatings having technologically attractive physical and chemical properties (e.g. wear- and corrosion-resistance) can be produced by suitable control of the electrolyte as well as electrical parameters of the PEO process. Oxide ceramic films, 3 to 40 μm thick, were produced on 6082 aluminium alloy by DC PEO using 5 to 20 A/dm² current density in KOH electrolyte with varied concentration (0.5 to 2.0 g/l). Phase analysis (composition and crystallite size) was carried out using X-ray diffraction and TEM techniques. Residual stresses associated with the crystalline coating phase (α-Al₂O₃) were evaluated using the X-ray diffraction Sin²ψ method. Nanoindentation studies were conducted to evaluate the hardness and elastic modulus. SEM, SPM and TEM techniques were utilised to study surface as well as cross-sectional morphology and nano features of the PEO coatings. Correlations between internal stress and coating thickness, surface morphology and phase composition are discussed. It was found that, depending on the current density and electrolyte concentration used, internal direct and shear stresses in DC PEO alumina coatings ranged from − 302 ± 19 MPa to − 714 ± 22 MPa and − 25 ± 12 MPa to − 345 ± 27 MPa, respectively. Regimes of PEO treatment favourable for the production of thicker coatings with minimal stress level, dense morphology and relatively high content of α-Al₂O₃ phase are identified.     

Influence of electrolyte on corrosion properties of plasma electrolytic conversion coated magnesium alloys

The synthesis of oxides in a low-temperature electrolytic plasma allows to cover surfaces of magnesium and its alloys with multifunctional protective oxide-ceramic coatings. The corrosion properties of these layers are strongly dependent on their porosity. In order to minimize the porosity and to optimize the corrosion properties of the layers, the electrolyte concentration and composition (addition of CrO₃ as corrosion inhibitor) were varied, and the influences on layer structure, composition, and properties with a main focus on corrosion behaviour were studied.The corrosion properties of various layers thus generated were studied in 5% NaCl solution by measuring electrochemical polarization curves and by electrochemical impedance spectroscopy (EIS) at pH 3 and 6. Using XRD, LM, SEM and EDX to evaluate the composition and microstructure of the modified surfaces, the corrosion results were related to the microstructure and composition of the specific layer. The better results were obtained for layers produced at higher electrolyte concentration, whereas the addition of CrO₃ had no significant beneficial effect.     

Polypyrrole as a solid electrolyte for tantalum capacitors

Tantalum/tantalum pentoxide (Ta/Ta₂O₅)-based capacitors, in which polypyrrole (PP) is used as a solid electrolyte coating, have been studied. Aromatic sulfonate salts were used as the charge-compensating dopant ions due to their ability to impart good thermal and long-term stability. The capacitors prepared showed excellent high frequency performance up to 100 kHz and stability. The capacitors were prepared by two methods. In the first method the Ta₂O₅ dielectric layer was coated with chemically synthesized PP, followed by electrodeposition of a second layer of PP to increase the thickness and integrity of the PP layer. In the second method, chemical polymerization was used alone and the process repeated several times in order to obtain complete coverage of the Ta/Ta₂O₅, anodes. The redox properties of the PP synthesized chemically and electrochemically were studied by cyclic voltammetry and indicate that the polymers have similar electrochemical properties. Compositional analyses were carried out using X-ray photoelectron spectroscopy (XPS) before and after the re-anodization process used in the capacitor preparation to enhance the integrity of the TaTa₂O₅ dielectric. UV-Vis spectroscopy was used to check the stability of the PP to spontaneous ion exchange during the re-anodization process. The results indicate that aromatic sulfonates remain as the dopant ions when the reformation is carried out in the same aromatic sulfonate solution, but are partially substituted by H₂PO₄^- when the reformation is carried out in H₃PO₄. For the chemical polymerization, different synthetic conditions were used in order to improve the conductivity of PP; specifically, the use of low temperature and the addition of p-nitrophenol reduce the equivalent series resistance (ESR) of the capacitors.     

Effect of Iron sulfate as electrolyte additive on plasma electrolytic oxidation of aluminum alloy

This study has been carried out to investigate the incorporation of Iron(II) sulfate as an additive of electrolyte on formed AA1010 aluminum alloy, using plasma electrolytic oxidation method in silicate-based electrolytes containing Iron(II) sulfate. In order to fabricate nanocomposite coating, silicon nitride nanopowder was added to electrolyte. The effects of iron(II) sulfate additive on the voltage-time trend, microstructure, compositions, wear, and corrosion resistances of PEO coatings were investigated. In addition, current density and concentration of additive were studied as parameters that were effective on coating. Results showed that although FeSO₄ enters to the coating structure, but it does not develop a new phase. The corrosion and wear behavior of coated samples with FeSO₄ indicate an improvement as compared to those without additive.     

模具复杂型腔表面的等离子束表面处理系统研制

为了实现对模具复杂型腔表面的处理,研制了一套三维等离子束表面处理系统,能完成对模具复杂型腔表面的自动化等离子束表面处理。设计了等离子束电源和机器人的实时控制系统,能保证二者的协同运行,采用机器人离线编程技术,设计了离线编程软件,提高了编程效率和精度,并开发了针对等离子电弧特性的功率闭环调节模块,实现功率的反馈调节,保证加工过程中功率的稳定。为保证加工中等离子束喷嘴方向和工件垂直,采用欧拉角控制机器人位姿。还介绍了该加工系统的硬件系统和控制系统组成以及实现离线编程、功率调节和垂直加工的软件系统,讨论了该系统的具体成形工艺,并在试验中得到了较好效果。     

Characterization of plasma electrolytic oxide formed on AZ91 Mg alloy in KMnO4 electrolyte

The aim of this work is to investigate microstructure, corrosion resistance characteristics and nanohardness of the oxide layer on AZ91 Mg alloy by applying different voltage with KMnO₄ contained solution. There are lots of closed pores that are filled with another oxide compound compared with the typical surface morphology with pore coated until 350 V of coating voltage. The thickness of oxide layer increases with increasing coating voltage. The oxide layer formed on AZ91 Mg alloy in electrolyte with potassium permanganate consists of MgO and Mn₂O₃. Corrosion potential of the oxide layer on AZ91 Mg alloy obtained at different plasma electrolytic oxidation(PEO) reaction stages increases with increasing coating voltage. The corrosion resistance of AZ91 Mg alloy depends on the existence of the manganese oxide in the oxide layer. The inner barrier layer composed of the MgO and Mn₂O₃ may serve as diffusion barrier to enhance the corrosion resistance and may partially explain the excellent anti-corrosion performance in corrosion test. Nanohardness values increase with increasing coating voltage. The increase in the nanohardness may be due to the effect of manganese oxide in the oxide layer on AZ91 Mg alloy coated from electrolyte containing KMnO₄.     

Anodic plasma electrolytic nitrocarburising of VT22 titanium alloy in carbamide and ammonium chloride electrolyte

The structure of alpha- and beta-titanium alloy VT22, its microhardness, surface roughness, wear and corrosion resistance after anodic plasma electrolytic nitrocarburising in an electrolyte containing carbamide and ammonium chloride were investigated. An X-ray diffractometer and a scanning electron microscope were used to characterize the phase composition and structure of the modified surface. Tribological properties of the treated titanium alloy were evaluated using a ball-on-disc tribometer under lubricated testing conditions. The effect of processing temperature on corrosion resistance of the plasma electrolytic nitrocarburising samples was examined by means of potentiodynamic polarization in Ringer’s solution. It was shown that the anodic nitrocarburising provides saturation of the titanium alloy with oxygen, nitrogen and carbon and the formation of TiO₂ with a rutile structure and a nitrogen/carbon solid solution in titanium. The anodic plasma electrolytic nitrocarburising at all treatment temperatures diminishes the wear rate of the titanium alloy samples and the surface roughness. Friction coefficient of treated samples can be reduced by 4.7 times. The anodic nitrocarburising results in an enhanced corrosion resistance since the corrosion potential increases by an order of magnitude.     

Optimization of operating conditions and structure parameters of zinc electrolytic cell based on numerical simulation for electrolyte flow

The physical and mathematical model of an operating electrowinning cell was established, and the flow of electrolyte was numerically simulated by the commercial software Fluent. The results indicate that there are two circulations at the surface flow where part of electrolyte backflows to the inlet from the side of cell, and the rest flows directly to the outlet, and the separation of two circulations with opposite direction occurs at the 20th pair of anode-cathode. This phenomenon was observed in the real operation. The electrolyte flows into the space between anode and cathode from the side portion of the cell. Meanwhile, the interelectrode effective flow rate (IEFR) is put forward to describe quantitively the flow field characteristics and is defined as the ratio of electrolyte flow between the anode and cathode to the total flow area. The influences of structure parameters and operating conditions on IEFR, such as the inlet angle, the volumetric flow rate, the inlet position and the height of steel baffles were simulated. The inlet position has a significant influence on the IEFR and its optimal value is 0.9 m below free surface. The inlet angle should be in the range from ?10° to 10°. IEFR is in linear proportion with the volumetric flow rate, and the height of the steel baffle has little influence on the flow field.     

等离子体表面改性在材料保护研究中的进展

概述了等离子体方法在材料表面改性方面的应用原理、工艺特点和最新进展,特别综述了近年来脉冲高能量密度等离子体（PHEDP）在表面改性方面所取得了令人注目的成就,并给出部分典型实例。     

Effect of electrolyte on mechanical properties of AZ31B Mg alloy in electrolytic plasma processing

Coatings on Mg alloys were prepared using NaOH + Na₂SiO₃ as basic electrolyte containing electrolyte of Na₂SiF₆ or NaF. EPP treatment was carried out on AZ31 Mg alloys matrix under a hybrid voltage of AC of 200 V combined with DC of 260 V for 30 min. Structural and morphological analyses of ceramic coatings were analyzed by XRD and SEM. Wear and hardness of coatings were measured by pin-on disk test and Vickers hardness test. The coatings formed in Na₂SiF₆ and NaF electrolytes were mainly composed of MgO and Mg₂SiO₄. The measured micro-hardness of coating formed in Na₂SiF₆ electrolyte was found to be over HV 1100, while, coating formed in NaF electrolyte possessed micro-hardness of HV ～900. These results show that the mechanical properties of AZ31B Mg alloys can be enhanced by the proper selection of electrolyte agent.     

Characterization of the surface layers formed on titanium by plasma electrolytic oxidation

This paper is concerned with the surface modification of titanium by the PEO method (plasma electrolytic oxidation) in the solutions which contain Ca, P, Si and Na. The chemical composition of the thus formed surface layers was examined by XPS and EDS. The morphology of the surface was observed by SEM. The phase composition was determined by X-ray diffraction (XRD). The adhesive strength of the oxide layers was evaluated by the scratch-test. The corrosion resistance was determined in a simulated body fluid (SBF) at a temperature of 37 °C by electrochemical methods for various exposure times.The oxide layers obtained were porous and enriched with Ca, P, Si and Na and their properties depended on the electrolyte solution and the parameters of the oxidation process. The results of the electrochemical examinations show that the surface modification by PEO does not worsen the corrosion resistance of titanium after a 13 h exposure in SBF. The electrochemical impedance spectroscopy (EIS) results indicate that the surface layers have a complex structure and that their electric properties undergo changes during long-term exposures in SBF.     

Effect of additive concentration during copper deposition using EnFACE electrolyte

Copper deposition from solutions using high concentration of acid, metal ions and polyethylene glycol (PEG), and bis-(3-sulphopropyl) disulphide (SPS) and chloride ions (Cl^–) is well known. A recent maskless micropatterning technology, which has the potential to replace the traditional photolithographic process, called EnFACE, proposed using an acid-free, low metal ion solution which is in direct contrast to those used in standard plating technology. In this work copper has been deposited using both standard electroplating solutions and those used in the EnFACE process. In the standard electrolyte 0.63 M CuSO₄ and 2.04 M H₂SO₄ has been used, along with Gleam additives supplied by Dow Chemicals. For the Enface electrolyte, copper deposition has been carried out without any acid, and with different concentrations of additives between 17% - 200% of those recommended by suppliers. 25?µm of metal has been plated on stainless steel coupons as suggested by ASTM, peeled off and subjected to ductility and resistance measurements. Scanning electron microscopy and electron back scatter diffraction have been carried out to determine the deposit morphology. It was found that copper deposits obtained from acid-free solutions containing low concentration of metal ion and additives produced copper deposits with properties which are comparable to those obtained from standard electrolytes. The optimum additive concentration for the EnFACE electrolyte was 50% of the supplier recommended value.     

电解液成分对等离子体电解氧化TC4合金腐蚀行为和摩擦学性能的影响（英文）

在TC4合金表面制备4种典型等离子体电解氧化(PEO)涂层,研究电解质组成对PEO涂层腐蚀行为和摩擦学性能的影响。结果表明,PEO涂层的腐蚀行为和摩擦学性能与电解质成分密切相关。在含NaH₂PO₂的电解液中制备的PEO涂层由于内氧化膜较致密而具有最好的耐蚀性能,而在含NaAlO₂的电解液中制备的PEO涂层由于含有Al₂O₃而具有最好的摩擦学性能。为制备具有良好耐蚀性和耐磨性的PEO涂层,以NaH₂PO₂和NaAlO₂为电解液主要成分制备了复合PEO涂层。     

Effect of NaOH on plasma electrolytic oxidation of A356 aluminium alloy in moderately concentrated aluminate electrolyte

Plasma electrolytic oxidation(PEO) of cast A356 aluminum alloy was carried out in 32 g/L NaAlO₂ with the addition of different concentrations of NaOH. The stability of the aluminate solution is greatly enhanced by increasing the concentration of NaOH. However, corresponding changes in the PEO behaviour occur due to the increment of NaOH concentration. Thicker precursor coatings are required for the PEO treatment in a more concentrated NaOH electrolyte. The results show that the optimal NaOH concentration is 5 g/L, which improves the stability of storage electrolyte to about 35 days, and leads to dense coatings with high wear performance (wear rate: 4.1×10⁻⁷ mm³·N⁻¹·m⁻¹).     

Characterization of plasma electrolytic oxidation coatings formed on Mg–Li alloy in an alkaline polyphosphate electrolyte

Blue and white ceramic coatings have been successfully fabricated on the surface of Mg–Li alloys by plasma electrolytic oxidation (PEO) in an alkaline polyphosphate electrolyte with and without addition of titania sol. The influence of titania sol on the surface morphology, microstructure, phase composition, chemical composition, corrosion resistance, mechanical and tribological behavior of ceramic coatings was scrutinized by means of scanning electron microscopy (SEM), thin-film X-ray diffraction (TF-XRD), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization, nanoindentation measurements, and ball-on-cylinder friction testing. The blue ceramic coating containing MgO, TiO₂ and Ti₂O₃ phase exhibits better anticorrosion and tribological performance due to its higher nanohardness and lower friction coefficient.     

Preparation of ceramic coatings on inner surface of steel tubes using a combined technique of hot-dipping and plasma electrolytic oxidation

A new method for inner surface modification of steel tubes, named a combined technique of hot-dipping and plasma electrolytic oxidation (PEO) was proposed and demonstrated in this paper. In this work, metallurgically bonded ceramic coatings on inner surface of steel tubes were obtained using this method. In the combined process, aluminum coatings on steel were firstly prepared by the hot-dip process and then metallurgically bonded ceramic coatings were obtained on the aluminum coatings by PEO. The element distribution, phase composition and morphology of the aluminide layer and the ceramic coatings were characterized by SEM/EDX and XRD. The corrosion resistance of the ceramic coatings were also studied. The results show that, after hot-dip treatment, the coating layers consist of two layers, where Al, Fe_xAl _(1−x) were detected from external topcoat to the aluminide/steel substrate. Then after PEO process, uniform Al₂O₃ ceramic coatings have been deposited on inner surface of steel tubes. The ceramic coatings are mainly composed of -Al₂O₃ and γ-Al₂O₃ phase. The compound coatings show favorable corrosion resistance property. The investigations indicate that the combination of hot-dipping and plasma electrolytic oxidation proves a promising technique for inner surface modification of steel tubes for protective purposes.