Plain fatigue and fretting fatigue behaviour of plasma nitrided Ti-6Al-4V

Fatigue tests with and without fretting against unnitrided fretting pads were conducted on unnitrided and plasma nitrided Ti-6Al-4V samples. Plasma nitrided samples exhibited higher surface hardness, higher surface compressive residual stress, lower surface roughness and reduced friction force compared with the unnitrided specimens. Plasma nitriding enhanced the lives of Ti-6Al-4V specimens under both plain fatigue and fretting fatigue loadings. This was explained in terms of the differences in surface hardness, surface residual stress, surface roughness and friction force between the unnitrided and nitrided samples.     

Corrosion behavior of PIRAC nitrided Ti-6Al-4V surgical alloy

Hard titanium nitride (TiN) coatings were obtained on the surface of Ti-6Al-4V alloy using an original PIRAC nitriding method, based on annealing the samples under a low pressure of monatomic nitrogen created by selective diffusion of N from the atmosphere. PIRAC nitrided samples exhibited excellent corrosion resistance in Ringer's solution in both potentiodynamic and potentiostatic tests. The anodic current and metal ion release rate of PIRAC nitrided Ti-6Al-4V at the typical corrosion potential values were significantly lower than those of the untreated alloy. This, together with the excellent adhesion and high wear resistance of the TiN coatings, makes PIRAC nitriding an attractive surface treatment for Ti-6Al-4V alloy surgical implants.     

Nanoscale characterization of anodic oxide films on Ti-6Al-4V alloy

The paper analyses, at nanoscale levels, the chemical composition and mechanical properties of the anodic oxide films formed on Ti-6Al-4V alloy by galvanostatic polarization at maximum final voltages of 12-100 V. For the investigations Auger Electron Spectroscopy, Photoelectron Spectroscopy and nanoindentation measurements have been used. The results have shown that anodizing the Ti-6Al-4V alloy produces an oxide film whose thickness depends on the final voltage. The chemical composition is not significantly dependent on the thickness, the film consists of TiO₂ and Al₂O₃. However, the best insulating properties of the films, determined from the growth parameter nm/V, are achieved with a final voltage between 30 and 65 V. Nanohardness and Young's modulus measurements have shown that the anodic films formed by different voltages exhibit similar mechanical properties which is consistent with the results of the surface analysis.     

Evaluation of the efficiency of TiB2 and TiC as protective coatings for SiC monofilament in titanium-based composites

The vigorous interfacial reactions in SiC/Ti-6Al-4V composites at elevated temperatures lead to the deterioration of the mechanical properties of the composites. TiB₂ and TiC were selected as potential protective coatings for SiC fibres in titanium-based composites. These coatings were deposited on to fibres by the chemical vapour deposition technique. Comparisons and evaluations have been made of the effectiveness of these ceramics as protective coatings for SiC fibres by incorporating the coated fibres into a Ti-6Al-4V matrix using the diffusion bonding method. Emphasis has been placed on the chemical compatibility of the candidate coating with SiC and Ti-6Al-4V by examining the interfaces of the fibre/coating/matrix using microscopic methods and chemical analysis. A stoichiometric TiB₂ coating was found to be stable with SiC and has proved an effective barrier to prevent the SiC fibre from reacting with the Ti-6Al-4V. The TiC coating showed no apparent reaction with a titanium-alloy matrix under the conditions studied, but was found to react with the SiC fibre substrate.     

Nanocrystalline diamond growth on different substrates

Nanocomposite films consisting of diamond nanoparticles of 3-5 nm diameter embedded in an amorphous carbon matrix have been deposited by means of microwave plasma chemical vapour deposition (MWCVD) from CH₄/N₂ gas mixtures. Si wafers, Si coated with TiN, polycrystalline diamond (PCD) and cubic boron nitride films, and Ti-6Al-4V alloy have been used as substrates. Some of the substrates have been pretreated ultrasonically with diamond powder in order to enhance the nucleation density n_nuc. It turned out that n_nuc depends critically on the chemical nature of the substrate, its smoothness and the pretreatment applied. No differences to the nucleation behaviour of CVD PCD films were observed. On the other hand, the growth process seems to be not affected by the substrate material. The crystallinity (studied by X-ray diffraction) and the bonding environment (investigated by Raman spectroscopy) show no significant differences for the various substrates. The mechanical and tribological properties, finally, reflect again the influence of the substrate material: on TiN, a lower hardness was measured as compared to Si, PCD and c-BN, whereas the adhesion of c-BN/nanocrystalline diamond (NCD) system was determined by that of the c-BN film on the underlying Si substrate.     

Laser Gas Nitriding of Ti-6Al-4V Part 2: Characteristics of Nitrided Layers

The characteristics of laser nitrided layers formed on Ti-6Al-4V are presented in this investigation. It has been determined that titanium nitride (TiN) is formed, which significantly increases the hardness of the nitrided surfaces. The amount of titanium nitride produced depends on the processing parameters such as laser pulse energy and nitrogen concentration. Nitrided layers are much smoother along the laser pass direction than perpendicular to this direction. The shrinkage effect in the laser melt zone produces surface residual tensile stresses in Ti-6Al-4V samples regardless of whether the processing environment is Ar, N₂, or a mixture of these gases. Pre-heating or stress relieving after laser nitriding significantly reduces the residual tensile stress level.     

Adhesive B-doped DLC films on biomedical alloys used for bone fixation

The long-term failure of the total hip and knee prostheses is attributed to the production of wear particles at the articulating interface between the metals, ceramics and polymers used for surgical implants and bone-fixtures. Therefore, finding an adhesive and inert coating material that has low frictional coefficient should dramatically reduce the production of wear particles and hence, prolong the life time of the surgical implants. The novel properties of the non-toxic diamond-like carbon (DLC) coatings have proven to be excellent candidates for biomedical applications. However, they have poor adhesion strength to the alloys and biomaterials. The addition of a thin interfacial layer such as Si, Ti, TiN, Mo and Cu/Cr and/or adding additives such as Si, F, N, O, W, V, Co, Mo, Ti or their combinations to the DLC films has been found to increase the adhesion strength substantially. In our study, grade 316L stainless steel and grade 5 titanium alloy (Ti-6Al-4V) were used as biomaterial substrates. They were coated with DLC films containing boron additives at various levels using various Si interfacial layer thicknesses. The best film adhesion was achieved at 8% and 20% on DLC coated Ti-6Al-4V and grade 316L substrates, respectively. It has been demonstrated that doping the DLC with boron increases their adhesion strength to both substrates even without silicon interfacial layer and increases it substantially with optimum silicon layer thickness. The adhesion strength is also correlated with the hydrogen contents in the B-DLC films. It is found to reach its maximum value of 700 kg/cm² and 390 kg/cm² at 2/7 and 3/6 for CH₄/Ar partial pressures (in mTorr ratio) for Ti-6Al-4V and 316L substrates, respectively.     

Microstructural characterisation of nanocomposite nc-MeC/a-C coatings on oxygen hardened Ti-6Al-4V alloy

Nanocomposite coatings are novel, important systems composed of two or more nanocrystalline, or nanocrystalline and amorphous, phases. Such coatings offer a possibility of tailoring the coating microstructure and achieving new improved properties of coated materials. In this work a duplex surface treatment, consisting of an oxygen diffusion treatment and deposition of low friction nanocomposite nc-MeC/a-C (Me = transition metal, Ti, W or Cr) coatings, was applied for improvement of the Ti-6Al-4V alloy properties. The coatings composed of nanocrystallites of transition metal carbides (TiC or Cr_xC_y or WC) embedded in hydrogen-free amorphous carbon (a-C) matrix were deposited onto the surface of an oxygen hardened Ti-6Al-4 V alloy substrate by means of a simple DC magnetron sputtering. A nano/microstructure of the substrate material and coatings has been examined by scanning- and transmission electron microscopy complemented with the results of X-ray diffraction analyses.It was found that the nanocomposite coatings are composed of different carbide nanocrystals (with sizes of a few nanometres) embedded in an amorphous carbon matrix. The results of qualitative and quantitative analyses of the nanocrystalline phase in the coatings with use of high-resolution transmission electron microscopy combined with image analysis are given in the paper.An effect of the nano/microstructure parameters of the coated alloy onto its micro-mechanical (nanohardness and Young's modulus) and tribological properties (wear resistance and friction coefficient) is discussed in the paper.     

Saddle field fast atom beam source: A new low pressure plasma nitriding method for a alloy Ti-6Al-4V

Ti and its alloys (Ti-6Al-4V) have been used in different engineering applications due to their several outstanding properties. Nevertheless, their use in practical applications is limited in many cases due to their poor tribological property. Researches are ongoing on surface modification of Ti based materials by different plasma and ion based techniques to overcome this problem. However, the conventional plasma nitriding techniques have several problems such as formation of an arc, increased possibility of surface contamination due to a comparatively higher operating pressure, production of a very thin nitrided layer after a long processing time, etc. In this present work, the possibility of a new low-pressure plasma nitriding process using a Plasma Enhanced Chemical Vapor Deposition (PECVD) based saddle field fast atom beam source on a Ti-6Al-4V alloy sample is investigated. Plasma nitriding was carried out at 900 °C and at a pressure 0.1 Pa for 8 h by using a beam current 0.5 A. Optical Microscopy investigation of the cross-section of the nitrided sample revealed a compound nitrided layer (thickness approximately 16 μm) followed by a diffusion layer. X-Ray Diffraction (XRD) analysis confirmed the presence of a TiN phase in the nitrided layers. A roughly three fold higher hardness value (1578 HV_0.015) in the top nitriding layer was observed by Vickers microhardness testing compared to hardness value of untreated sample (568 HV_0.015),with a gradually decreasing hardness in the core material. The results show that this is a promising method for low pressure plasma nitriding of Ti alloy within a short processing time compared to the conventional nitriding process.     

Evaluation of the effects of plasma nitriding temperature and time on the characterisation of Ti 6Al 4V alloy

The effects of plasma nitriding (PN) temperature and time on the structural and tribological characterisation of Ti 6Al 4V alloy were investigated. PN processes under gas mixture of N₂/H₂ = 4 were performed at temperatures of 700, 750, 800 and 850 °C for duration of 2, 5 and 10 h. Cross section and surface characterisation were evaluated by means of SEM, AFM, XRD and microhardness test techniques. Dry wear tests were performed using a pin on disc machine. Mass loss and coefficient of friction were measured during the wear tests. Three distinguished structures including of a compound layer (constituted of δ-TiN and ɛ-Ti₂N), an aluminium-rich region and a diffusion zone (interstitial solid solution of nitrogen in titanium) were detected at the surface of plasma nitrided Ti 6Al 4V alloy. These structures increased surface hardness of Ti 6Al 4V alloy significantly and gradually distributed the hardness from the surface to the substrate. The "surface hardness", "surface roughness", "wear resistance" and "coefficient of friction" of the alloy were increased due to plasma nitriding process. Moreover, rising both process temperature and time led to increasing of "layers thicknesses", "surface hardness", "surface roughness", "dynamic load-ability" and "wear resistance" of Ti 6Al 4V alloy.     

Laser Surface Nitriding of Ti-6A1-4V Titanium Alloy

Titanium and its alloys are known for their high specific strength as well as fatigue and corrosion resistance. However, they suffer from poor wear and friction resistance, limiting their use in tribological applications. Nitriding of these materials may be carried out favourably to harden them and thus to improve both wear and friction resistance. The laser nitriding process involves using the intense energy of the laser to melt the surface in a nitrogen comprising atmosphere. This results in creation of a very hard layer consisting of dendritic structures of nitride. But the non-uniformity of the melt pool and cracks in the nitrided layers have been generally observed. Our study deals with the results of Ti-6Al-4V laser surface nitriding and with the effects of a sample preheating on the cracks generation.     

Fabrication of TiC/TiB/Ti3AlC2 phases reinforced coatings on Ti-6Al-4V substrate

Intermetallic matrix composite coatings reinforced by TiC, TiB₂, and Ti₃AlC₂ were fabricated by laser cladding the mixed power Ti, Al, and B₄C on the Ti-6Al-4V alloy. X-ray diffraction, scanning electron microscope, and energy dispersive spectroscopy were chosen to investigate the structures and morphologies of the coatings. Results showed that the coatings mainly consisted of the reinforcements of TiC, TiB₂, and Ti₃AlC₂ and the matrix of Ti₃Al, TiAl, TiAl₃, and α-Ti. The hardness and wear-resisting property of the prepared specimens of Ti-45Al-10B₄C and Ti-45Al-20B₄C were studied contrastively. It was found that the coating was metallurgical bonded to the Ti-6Al-4V substrate. The micro-hardness and dry sliding wear-resisting properties of the specimen of Ti-45Al-20B₄C were enhanced further. And the micro-hardness of Ti-45Al-20B₄C was from 900 HV_0.2 to 1225 HV_0.2. The wear-resisting property of Ti-45Al-20B₄C was four times as large as that of the Ti-6Al-4V alloys.     

Wear resistant and anti-corrosive treatment for TI-6AL-4V using metal vapor vacuum arc source in comparison with plasma immersion ion implantation

This study utilizes two ion-implantation methods, plasma immersion ion implantation (PIII) and metal vapor vacuum arc (MeVVA), to prepare Ti-N phases on the surface of Ti-6Al-4V. By the nitrogen PIII method, both nitrogen and minor oxygen species are simultaneously attracted by the negatively charged substrate. The penetration of N and O interstitial elements to an extensible depth is possible owing to the effect from the negatively charged target. The nitrogen PIII treatment does not produce a novel Ti-N phase. As a result, the modified surface does not behave anticorrosive. The H_n and the E determined by nanoindentation also remain unchanged. It is still potential to apply this non-directional treatment by increasing bias voltage of the target, coating pure titanium on Ti-6Al-4V, and adjusting the regeneration process of nitrogen ions. The MeVVA treatment creates a novel αTiN_0.3 (011) phase on Ti-6Al-4V in present study. It signifies that the interactions between kinetic Ti ions of varied energies and minor nitrogen molecules, with minor participation of oxygen, are highly feasible. The novel ion-implanted Ti-N phase is corrosion resistant, which is capable to reduce passivation current density by forming a passive film. Moreover, the MeVVA-treated surface is surface-hardened; the E is simultaneously increased. The increase of nano mechanical properties can be visualized by 3D images using Nano Vision and determined by analyzing the tip/surface impact structure on the indentation site.     

The microstructural observation and wettability study of brazing Ti-6Al-4V and 304 stainless steel using three braze alloys

Both Ti-6Al-4V and 304 stainless steels (304SS) are good engineering alloys and widely used in industry due to their excellent mechanical properties as well as corrosion resistance. Well-developed joining process can not only promote the application of these alloys, but also can provide designers versatile choices of alloys. Brazing is one of the most popular methods in joining dissimilar alloys. In this study, three-selected silver base filler alloys, including Braze 580, BAg-8 and Ticusil®, are used in vacuum brazing of 304SS and Ti-6Al-4V. Based upon dynamic sessile drop test, Braze 580 has the lowest brazing temperature of 840°C, in contrast to 870°C for BAg-8 and 900°C for Ticusil® braze alloy. No phase separation is observed for all brazes on 304SS substrate. However, phase separation is observed for all specimens brazed above 860°C on Ti-6Al-4V substrate. The continuous reaction layer between Braze 580 and 304SS is mainly comprised of Ti, Fe and Cu. The thickness of reaction layer at Braze 580/Ti-6Al-4V interface is much larger than that at Braze 580/304SS interface. Meanwhile, a continuous Cu-Sn-Ti ternary intermetallic compound is found at the Braze 580/Ti-6Al-4V interface. Both Ticusil® and BAg-8 brazed joint have similar interfacial microstructures. Different from the Braze 580 specimen, there is a thick Cu-Ti-Fe reaction layer in both BAg-8/304SS and Ticusil®/304SS interfaces. The formation of Cu-Ti-Fe interfacial layer can prohibit wetting of BAg-8 and Ticusil® molten brazes on 304SS substrate. Meanwhile, continuous Ti₂Cu and TiCu layers are observed in Ti-6Al-4V/BAg-8 and Ti-6Al-4V/Ticusil® interfaces.     

Effect of Nb coating on the sulphidation/oxidation behaviour of Ti and Ti-6Al-4V alloy

The environmental response of Nb-coated Ti and Ti-6Al-4V alloy was studied at 750 °C in an atmosphere of pS₂ ∼ 10⁻¹ Pa and pO₂ ∼ 10 ⁻¹⁸ Pa. By acting as a diffusion barrier and through the formation of a Nb_1−xS scale the Nb coating deposited enhanced the corrosion resistance of both Ti and Ti-6Al-4V alloy. The corrosion products generated on uncoated titanium in the same environment and temperature were characterized by a double layered oxide scale of TiO₂ beneath which a TiS₂ layer was formed. For the Ti-6Al-4V alloy, α-Al₂O₃ was precipitated in the external portion of the outer-layer of TiO₂ whilst a layer containing Al₂S₃, TiS₂ and vanadium sulphide (possibly V₂S₃) was idenitified underlying the inner TiO₂ layer. After prolonged exposure (168 h), the Nb coating deposited on Ti and Ti-6Al-4V alloy was consumed. A scale following the sequence of TiO₂/TiO₂+NbO₂+Nb₂O₅/Nb_1−xS/TiO₂/ TiS₂/(substrate) was observed on the surface of the Nb-coated Ti, whilst a scale with sequence of TiO₂/V₂S₃/TiO₂+NbO₂+Nb₂O₅/Nb_1−xS/TiO₂/Al₂S₃+TiS₂/(substrate) characterized the corrosion products formed on the Nb-coated Ti-6Al-4V alloy.     

Investigating the wear characteristics of engineered surfaces: low-temperature plasma nitriding and TiN + MoS x hard-solid lubricant coating

Significant progress has been made in the past decade in plasma nitriding with a majority of the research work focusing on improving hardness and wear resistance of the nitrided surface through the reduction of nitriding temperature, pressure or time. Hard-solid lubricating coatings have also been extensively studied for lowering the wear rate and coefficient of friction of traditional hard coatings such as TiN by the combined effect of hardness and solid lubrication. In this study, the wear characteristics of low-temperature plasma-nitrided steel substrate performed using a Saddle-field fast atom beam source and TiN + MoS _x hard-solid lubricant coating deposited by a closed-field magnetron-sputtering technique have been investigated. The thin hard layer in plasma-nitrided substrates exhibited much higher hardness and lower wear compared to the untreated substrate in pin-on-disc wear testing. In addition, the study of the wear track morphology of the nitrided samples evidenced significant reduction of deeper ploughing and plastic deformation due to higher hardness and load supporting of the nitrided layer. On the other hand, due to the incorporation of MoS₂ in TiN coating, the wear resistance and coefficient of friction were greatly improved in TiN + MoS _x coating compared to pure TiN coating. In contrast to TiN coating, a relatively smoother wear track with less abrasive wear also supported the beneficial effects of adding MoS₂ in TiN coating.     

Structural and mechanical properties of titanium oxide thin films for biomedical application

Titanium oxide thin films were deposited by radiofrequency reactive sputtering in Ar-O₂ atmosphere on silicon (100) wafers and titanium alloy plates (Ti-6Al-4V). Thin films structural characterization was carried out by grazing incidence X-ray diffraction, atomic force microscopy, scanning and transmission electron microscopies. Chemical composition was checked by X-ray wavelength dispersive spectroscopy. Mechanical assessment was achieved by nano-indentation and nano-scratch measurements. The films deposited on silicon substrates are over-stoechiometric in oxygen, with an oxygen to titanium ratio of about 2.2. The growth of anatase and rutile phases was promoted by ranging the total and oxygen partial pressures between 0.17-1.47 Pa and 35-85%. The growth rate of films, determined by grazing incidence X-ray reflectivity, was ranging from 35 to 55 nm/h. The rutile single-phased films possess a hardness of about 2.5 times higher and a lower friction coefficient than the anatase films. The films which contain anatase possess a high surface root-mean-square roughness and a reduced elastic modulus of around 120 GPa close to reduced elastic moduli of hydroxyapatite bioceramic and titanium alloy. So the anatase film could be the best candidate as a titanium oxide intermediate layer between hydroxyapatite and titanium alloy in the field of biomedical implants.     

Surface characteristics of a porous-surfaced Ti-6Al-4V implant fabricated by electro-discharge-compaction

Electro-discharge-compaction (EDC) is a unique method for producing porous-surfaced metallic implants. The objective of the present studies was to examine the surface characteristics of the Ti-6Al-4V implants formed by EDC. Porous-surfaced Ti-6Al-4V implants were produced by employing EDC using 480 F capacitance and 1.5 kJ input energy. X-ray photoelectron spectroscopy was used to study the surface characteristics of the implant materials. C, O, and Ti were the main constituents, with smaller amounts of Al and V. EDC Ti-6Al-4V also contained N. Titanium was present mainly in the forms of mixed oxides and small amounts of nitride and carbide were observed. Al was present in the form of aluminum oxide, while V in the implant surface did not contribute to the formation of the surface oxide film. The surface of conventionally prepared Ti-6Al-4V primarily consists of TiO₂, whereas, the surface of the EDC-fabricated Ti-6Al-4V consists of complex Ti and Al oxides as well as small amounts of titanium carbide and nitride components. However, preliminary studies indicated that the implant was biocompatible and supports rapid osseointegration.     

Si3N4和52100钢对磨副材料对CrN薄膜干摩擦学行为的影响

利用阴极电弧离子镀技术在316L不锈钢基体上制备了CrN薄膜。采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、纳米压痕仪对CrN薄膜的形貌、成分和力学性能进行了表征。为了研究Si_3N_4和52100钢对磨副材料对CrN薄膜和316L不锈钢干摩擦行为的影响,在2N、5N、8N三种载荷下,将CrN薄膜和316L不锈钢基体与Si_3N_4陶瓷球和52100钢球分别进行了往复式滑动干摩擦实验。采用扫描电子显微镜观察了磨痕的微观形貌,并对CrN薄膜和316L不锈钢基体的磨损机制进行了分析。结果表明:CrN薄膜表面平整,缺陷较少;CrN薄膜的纳米硬度约为28GPa,弹性模量约为350GPa;与Si_3N_4陶瓷球相比,CrN薄膜与52100钢球摩擦时摩擦因数相对较小(保持在0.7左右)且更加稳定;316L不锈钢的摩擦因数远大于CrN薄膜且波动较大;对磨球为Si_3N_4陶瓷球时,CrN薄膜的主要磨损机制为磨粒磨损,伴有少量的氧化和黏着磨损,316L不锈钢的磨损机制主要为磨粒磨损和塑性变形,伴有少量的氧化和黏着磨损;对磨球为52100钢球时,CrN薄膜的主要磨损机制为黏着磨损,伴有少量的氧化,316L不锈钢的磨损机制主要为黏着磨损,伴有少量的氧化和磨粒磨损。CrN薄膜与两种对磨球的磨损量均小于316L不锈钢基体的磨损量,说明CrN薄膜有效提高了基体的耐磨性。     

基于RFPECVD方法不锈钢上沉积类金刚石薄膜的机械与摩擦特性

讨论用射频等离子体增强化学气相沉积(RFPECVD)工艺,在室温下实现在1Cr18Ni9Ti不锈钢基底上镀类金刚石(DLC)膜.为提高DLC膜的结合力,首先在不锈钢基底上沉积Ti/TiN/TiC功能梯度膜.借助所设计的界面过渡层,成功地在不锈钢基底上沉积了一定厚度的DLC膜.通过优化沉积参数,所沉积的DLC膜在与100Cr6钢球对磨时摩擦系数低于0.020.在摩擦过程中DLC膜的磨损机制借助SEM、Raman分析进行了研究.