Dip Coating of Calcium Hydroxyapatite on Ti-6Al-4V Substrates

Ti-6Al-4V alloy is the most commonly used metallic material in the manufacture of orthopedic implants. The main inorganic phase of human bone is calcium hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂, HA). To achieve better biocompatibility with bone, metal implants made of Ti-6Al-4V are often coated with bioceramics. Dip-coating techniques scarcely are used to apply HA onto metallic implants. New dipping-solution recipes to be used for HA coatings are described in this work. Scanning electron microscopy and X-ray diffractometry have been used for sample characterization.     

Reaction Between Ti-6Al-4V and Boron

The present report describes the investigation by electron diffraction of the reaction between boron and Ti-6Al-4V. Plates that are intergrowths of TiB and VB were discovered.     

The Durability of Adhesively-bonded Ti-6Al-4V

The durability of chromic acid-anodized Ti-6Al-4V alloy, adhesively-bonded with FM-5 supported polyimide adhesive has been studied. The performance tests compared titanium samples that had been thermally treated and bonded, and samples that were bonded and thermally treated. Following the thermal treatment, the durability was examined (1) by immersing wedge-type specimens in boiling water and measuring the crack growth and (2) by measuring the lap shear strength for single lap specimens. In the wedge tests, failure occurs within the adhesive for specimens treated at temperatures below 371°C for less than one hour. For treatments at higher temperatures and for longer periods of time, failure occurs within the anodic oxide. From the lap shear tests, the principal finding is that the lap strength decreases with increasing treatment time at constant temperature and with increasing temperature at a fixed time. For the lap specimens, failure occurs to a greater extent within the oxide as the treatment time and temperature increase. Surface analysis results indicate the formation of an aluminum fluoride species. It is reasoned that the formation of fluorine-containing materials weakens the oxide and promotes failure within the anodic oxide.     

The Durability of Adhesively-bonded Ti-6Al-4V

The durability of chromic acid-anodized Ti-6Al-4V alloy, adhesively-bonded with FM-5 supported polyimide adhesive has been studied. The performance tests compared titanium samples that had been thermally treated and bonded, and samples that were bonded and thermally treated. Following the thermal treatment, the durability was examined (1) by immersing wedge-type specimens in boiling water and measuring the crack growth and (2) by measuring the lap shear strength for single lap specimens. In the wedge tests, failure occurs within the adhesive for specimens treated at temperatures below 371°C for less than one hour. For treatments at higher temperatures and for longer periods of time, failure occurs within the anodic oxide. From the lap shear tests, the principal finding is that the lap strength decreases with increasing treatment time at constant temperature and with increasing temperature at a fixed time. For the lap specimens, failure occurs to a greater extent within the oxide as the treatment time and temperature increase. Surface analysis results indicate the formation of an aluminum fluoride species. It is reasoned that the formation of fluorine-containing materials weakens the oxide and promotes failure within the anodic oxide.     

Cold compaction study of Armstrong Process® Ti-6Al-4V powders

The Armstrong Process® developed by Cristal US, Inc./International Titanium Powder, is an innovative, low-cost technology for producing Ti and Ti alloy powders in a one-step, continuous process. In this work, Armstrong Ti-6Al-4V powders were characterized and the cold compaction behavior of the powders were investigated in detail. As-received as well as milled powders were uniaxially die-pressed at designated pressures up to 690 MPa to form disk samples with different aspect ratios. Samples with high aspect ratio exhibited non-uniform density along the pressing axis and the density distribution was consistent with the result predicted by finite element analysis. The model developed from the linear regression analysis on the experimental density data can be used to predict density of compacts with different aspect ratios. In the studied pressure range, an empirical powder compaction equation was applied to linearize the green density — pressure relationship. Cold compaction parameters were obtained for the as-received and milled Armstrong Ti-6Al-4V powders.     

Corrosion susceptibility of implant materials Ti-5Al-4V and Ti-6Al-4Fe in artificial extra-cellular fluids

The paper is aimed at detecting the corrosion susceptibility (generated by the potential gradients, due to the pH changes) of implant materials Ti-5Al-4V and Ti-6Al-4Fe alloys exposed in extra-cellular fluids for long term (10 000 exposure hours) in comparison with pure titanium. The titanium and its ternary alloys exhibited spontaneous passivity in Ringer’s solutions of pH=6.98, 4.35 and 2.5, simulating the real situations that can arise in surgical applications. Potential gradients determined in presumptive extreme pH conditions indicate that there is no probability for local corrosion. Impedance spectra were fitted with one time constant equivalent circuit, typically for protective, compact oxide film. The fitting parameters indicate long-term stability of the passive layers in surgical implant conditions. Atomic force microscopy (AFM) and spectral infrared (IR) data are important arguments in supporting the conclusion that titanium and its ternary alloys have a very good corrosion resistance in long-term functional conditions.     

Ti-6Al-4V合金表面激光熔覆NiCrBSi＋5%BN涂层组织和性能

Ti-6Al-4V合金具有比强度高、耐蚀性能好等优点,在航天、航空、石油和化工等新科技工业部门广泛使用。在表面激光熔覆金属-陶瓷复合涂层是改善钛合金性能的重要方式,利用XRD、SEM和EDS等分析手段对NiCrBSi＋5%（质量分数）BN熔覆层的微观组织进行分析。利用HV-1000型显微维氏硬度计测试激光熔覆试样的硬度。     

Ti-6Al-4V钛合金脉冲阳极氧化工艺

研究了Ti-6Al-4V钛合金脉冲阳极氧化工艺,并对影响阳极氧化膜厚度的主要因素(如温度、电流密度、时间等)进行了研究,得到了满足膜厚要求的工艺参数。将优化得出的工艺参数应用于零件的仿形试件生产,得到厚度均匀的阳极氧化膜,并对其表面形貌、成分等进行了分析。     

Corrosion behaviour of Ti-6Al-4V in phosphoric acid

Ti-6A1-4V shows distinct active-passive behaviour in phosphoric acid over a wide concentration range. The cathodic polarization curves are similar over a wide range of acid concentration and temperatures. The alloy undergoes active dissolution and turns passive in the negative potential region followed by a wide range of passivity at all acid concentrations at different temperatures. Increasing acid concentration up to 11 M results in an increase in critical current density (i _cr). The passive current density (i _p) increases up to an acid concentration of 9 M while at 13 M i _cr and i _p decrease appreciably. A significant increase in both i _cr and i _p occurs with increase in solution temperature. The passive specimen remained stable for a long time when exposed to phosphoric acid under open circuit conditions.     

Gas nitriding and subsequent oxidation of Ti-6Al-4V alloys

Ti-6Al-4V alloys consisting of α-Ti grains and intergranular β-Ti islands were nitrided at 850°C for 1 to 12 h under a nitrogen pressure of 1 Pa. With increasing nitriding time, the Ti-N compound layer became thicker, and the α-Ti diffusion zone containing dissolved nitrogen became wider. In the Ti-N compound layer, the initially formed Ti₂N became TiN as the nitriding progressed. The nitride layers were oxidized to rutile-TiO₂ after oxidation at 700°C for 10 h in air.     

Effects of Tool Electrode on EDM Performance of Ti-6Al-4V

Due to widespread application of Ti-6Al-4V especially in automotive, aerospace, defense, and biomedical industries; machinability of this alloy is of immense importance. Very low thermal conductivity of Ti-6Al-4V is mainly responsible for its poor machinability. During Electro-Discharge Machining (EDM), conductivity of the workpiece as well as electrode plays a vital role affecting process performance. In this context, choice of electrode also influences the machining efficiency. Therefore, selection of an appropriate electrode to enhance performance of EDM on Ti-6Al-4V alloy is indeed necessary. In the present reporting, an experimental work has been carried out to investigate ease of machining of titanium alloy (Ti-6Al-4V) for electro-discharge machining using Tungsten and Copper (normal and cryogenically treated) electrodes. Experiments have been performed at different values of peak discharge current to study EDM performance on Ti-6Al-4V in terms of material removal efficiency, surface roughness, surface crack density and white layer thickness observed for the EDMed end product prepared from Ti-6Al-4V work material. Influence of peak discharge current on topography of the EDMed work surface has been examined. EDS analysis followed by micro-indentation hardness test has been performed to examine the extent of carbon enrichment onto the machined surface during EDM operation. XRD tests have been carried out to comprehend metallurgical aspects of the EDMed work surface which are supposed to be affected by the thermo-electrical phenomenon of EDM operation. Results obtained thereof, have been analyzed in detail to understand effects of electrode in persuading machinability of Ti-6Al-4V while machining though EDM route. It has been found that among three tool electrodes selected (Tungsten, normal Copper and cryogenically treated Copper), cryogenically treated Copper electrode has been found the most superior in purview of EDM performance.

     

Surface Preparation of Ti-6Al-4V for High-Temperature Adhesive Bonding

The role of surface preparation in high-temperature bond durability is investigated for Ti-6Al-4V adherends. Four surface preparations, including a newly-introduced treatment, plasma-sprayed Ti-6Al-4V coatings, are evaluated using a simple tensile test and a wedge/crack-propagation test. At temperatures approaching 300°C, the oxide-metal interface of oxide preparations becomes unstable. Such exposure results in a weakening of the oxide and, hence, bond failure at low tensile strength. The plasma-sprayed coating is a microscopically-rough metallic film with only a thin, native oxide. The plasma-sprayed adherend remains strong over prolonged, high-temperature exposures, and the micro-roughness is important for crack arrest in the wedge test.     

Surface Preparation of Ti-6Al-4V for High-Temperature Adhesive Bonding

The role of surface preparation in high-temperature bond durability is investigated for Ti-6Al-4V adherends. Four surface preparations, including a newly-introduced treatment, plasma-sprayed Ti-6Al-4V coatings, are evaluated using a simple tensile test and a wedge/crack-propagation test. At temperatures approaching 300°C, the oxide-metal interface of oxide preparations becomes unstable. Such exposure results in a weakening of the oxide and, hence, bond failure at low tensile strength. The plasma-sprayed coating is a microscopically-rough metallic film with only a thin, native oxide. The plasma-sprayed adherend remains strong over prolonged, high-temperature exposures, and the micro-roughness is important for crack arrest in the wedge test.     

Adhesion Tensile Testing of Environmentally Exposed Ti-6Al-4V Adherends

The structural and bonding properties of Ti-6Al-4V adherends, prepared by chromic acid anodization (CAA), were studied as a function of exposure in high-temperature environments such as vacuum, air, boiling and pressurized water, and steam. Subsequent to the environmental exposure, bonds were produced and the adhesive tensile strengths measured. Long-term exposure to high temperature, dry environments did not cause structural changes to the adherend oxide but did result in poor bond strength. The failure mode in these cases was within the oxide, which was apparently weakened by the exposure. The water-and steam-exposed oxides underwent a transition from amorphous to crystalline TiO₂ (with an accompanying change in oxide morphology); however, bond strength was maintained for moderate exposures at T ≤ 250°C. For exposure at T = 300°C, the bond strength was degraded severely. The latter result can be explained by a lack of porosity in the transformed oxide. SEM and XPS measurements were made on debonded surfaces to determine the loci of failure.     

Experimental Investigation on Surface and Machining Characteristics of Micro ED Milling of Ti-6Al-4 V with Different Nano Powder Mixed Dielectrics

Silicon - Micro ED milling is a micro machining technique for machining of high-quality micro parts on the electrically conductive material. Achieving a good surface finish with higher material...     

Chrome-free single-step in-situ phosphatizing coatings on a Ti-6Al-4V titanium alloy

Surface pretreatment, such as chromate conversion, is generally required for the organic coating on Ti-6Al-4V titanium alloys. The surface modification process facilitates bond formation between the titanium surface and adhesives or paints. However, the hexavalent chromate used in the conversion coating is carcinogenic and must be eliminated. Recently, the “green chemistry” technique of in-situ phosphatizing coatings (ISPC) has been developed at Northern Illinois University. In this study, a polyester-melamine coating system catalyzed by p-toluene sulfonic acid is used as a control paint and applied to bare (paint 1) and chromated (paint 3) Ti alloy panels. The arylphosphonic acid employed as an in-situ phosphatizing reagent (ISPR) is used to formulate ISPC polyester-melamine paint and to react in-situ with the metal surface when ISPC paint is applied on bare Ti panels (paint 2) and chromated Ti panels (paint 4). After soaking in 3% NaCl solution for 1500 hr, the electrochemical impedance, |Z|, was measured as 10⁹, 10¹⁰, 10¹⁰, and 10¹⁰ ohm-cm² for paints, 1, 2, 3, and 4, respectively. After 1000 hr salt spray (fog) testing, a disbondment from the “X” scribe is observed as 13 and <0.5, <1, <1 mm for paints 1, 2, 3, and 4, respectively. The simultaneous reaction of the ISPR in catalyzing the polymerization of paint film and forming the metal-phosphate layer is the reason for the superior ISPC paint performance. Presented at the 79th Annual Meeting of the Federation of Societies for Coatings Technology, in Atlanta, GA, Nov. 5–7, 2001. Department of Chemistry and Biochemistry, DeKalb, IL 60115.     

Ti-6Al-4V在氯离子环境中的耐蚀性研究

针对腐蚀性环境油气田开发实际,利用高温高压釜,研究Ti-6Al-4V在盐酸溴化锌加重溶液中的失重腐蚀速率,并利用体式显微镜及扫描电镜对试样进行腐蚀形貌观察和腐蚀膜成份分析,试验结果表明:在本文试验条件下,Ti-6Al-4V的腐蚀速率为0.1089mm/a;Ti-6Al-4V蚀坑较浅且呈开放式,未被腐蚀产物所覆盖;腐蚀膜中含有一定量Cl元素,表明Cl-是参与腐蚀反应的主要元素。     

Factors Affecting the Durability of Ti-6Al-4V/Epoxy Bonds

Factors influencing the durability of Ti-6Al-4V/epoxy interphases were studied by determining chemical and physical properties of Ti-6Al-4V adherend surfaces and by characterizing the strength and durability of Ti-6Al-4V/epoxy bonds.

Ti-6Al-4V adherend surfaces were oxidized either by chemical etch or anodization. Four principal pretreatments were studied: chromic acid anodization (CAA), sodium hydroxide anodization (SHA), phosphate fluoride acid etch (P/F) and TURCO basic etch (TURCO). The oxides were characterized by SEM, STEM, profilometry, contact angles and XPS.

All adhesive bonding was carried out using a structural epoxy, FM-300U. Both lap shear and wedge test samples were tested in hot, wet environments. The results lead to the conclusion that the interfacial area between the adhesive and adherend is the primary factor affecting bond durability.     

Corrosion resistance of pulsed laser-treated Ti-6Al-4V implant in simulated biofluids

A commercial Ti-6Al-4V alloy was treated with a pulsed-wave Nd:YAG laser under various process conditions to obtain surface oxide layer for corrosion resistance. The corrosion behaviors of bare and laser-treated Ti-6Al-4V alloy exposed to three different simulated biofluids (SBFs), namely, (1) NaCl solution, (2) Hank's solution, and (3) Cigada solution, were studied by using the electrochemical techniques like open circuit potential (OCP), Tafel analysis, and electrochemical impedance spectroscopy (EIS). The Tafel analysis showed that the laser-treated Ti-6Al-4V specimens were more corrosion resistant than the bare specimens in any of the above SBFs. The various electrical equivalent circuit models were applied to fit the EIS results to further understand corrosion mechanisms due to different surface layers formed on the alloy surface before and after the laser treatment. Optical and AFM imaging techniques were used to evaluate the topographic and morphologic features of the alloy exposed to such SBFs. The corrosion behavior of the laser-treated surfaces was explained by the melting and solid-state oxidation processes, the morphology of the surface oxide, and the underlying alloy microstructure. It is realized during the present investigation that better corrosion resistance and surface stability can be achieved by oxide growth in solid-state, under a pulsed laser condition.     

Corrosion behaviour of Ti-6Al-7Nb and Ti-6Al-4V ELI alloys in the simulated body fluid solution by electrochemical impedance spectroscopy

The corrosion behaviour of Ti-6Al-7Nb and Ti-6Al-4V ELI (extra low interstitial) was investigated as a function of immersion hours in simulated body fluid (SBF) condition, utilizing potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) techniques. Polarisation experiments were conducted after 0, 120, 240 and 360 h of immersion in SBF solution. From the polarisation curves, very low current densities were obtained for Ti-6Al-7Nb alloy compared to Ti-6Al-4V ELI, indicating a formation of stable passive layer. Impedance spectra were represented in the form of Bode plots and it was fitted using a non-linear least square (NLLS) fitting procedure, in which it exhibited a two time constant system suggesting the formation of two layers. The surface morphology of the titanium alloys have been characterized by SEM and EDAX measurements.