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.     

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.     

Mechanism of surface modification of a porous-coated Ti-6Al-4V implant fabricated by electrical resistance sintering

A porous-coated Ti-6Al-4V implant was fabricated by electrical resistance sintering, using 480 F capacitance and 1.5 kJ input energy. X-ray photoelectron spectroscopy (XPS) was used to study the surface characteristics of the implant material before and after sintering. There were substantial differences in the content of O and N between as-received atomized Ti-6Al-4V powders and the sintered prototype implant, which indicates that electrical resistance sintering alters the surface composition of Ti-6Al-4V. Whereas the surface of atomized Ti-6Al-4V powders was primarily TiO₂, the surface of the implant consisted of a complex of titanium oxides as well as small amounts of titanium carbide and nitride. It is proposed that the electrical resistance sintering process consists of five stages: stage I – electronic breakdown of oxide film and heat accumulation at the metal-oxide interface; stage II – physical breakdown of oxide film; stage III – neck formation and neck growth; stage IV – oxidation, nitriding, and carburizing; and stage V – heat dissipation. The fourth stage, during which the alloy repassivates, is responsible for the altered surface composition of the implant.     

Development of a β-type Ti–12Mo–5Ta alloy for biomedical applications: cytocompatibility and metallurgical aspects

Ti-based biocompatible alloys are especially used for replacing failed hard tissue. Some of the most actively investigated materials for medical implants are the beta-Ti alloys, as they have a low elastic modulus (to inhibit bone resorption). They are alloyed with elements such as Nb, Ta, Zr, Mo, and Fe. We have prepared a new beta-Ti alloy that combines Ti with the non-toxic elements Ta and Mo using a vacuum arc-melting furnace and then annealed at 950 degrees C for one hour. The alloy was finally quenched in water at room temperature. The Ti-12Mo-5Ta alloy was characterised by X-ray diffraction, optical microscopy, SEM and EDS and found to have a body-centred-cubic structure (beta-type). It had a lower Young's modulus (about 74 GPa) than the classical alpha/beta Ti-6Al-4V alloy (120 GPa), while its Vickers hardness remained very high (about 303 HV). This makes it a good compromise for a use as a bone substitute. The cytocompatibility of samples of Ti-12Mo-5Ta and Ti-6Al-4V titanium alloys with various surface roughnesses was assessed in vitro using organotypic cultures of bone tissue and quantitative analyses of cell migration, proliferation and adhesion. Mechanically polished surfaces were prepared to produce unorientated residual polished grooves and cells grew to a particularly high density on the smoother Ti-12Mo-5Ta surface tested.     

Laser boronising of Ti–6Al–4V as a result of laser alloying with pre-placed BN

This paper discusses the effect of CO₂ laser alloying of pre-placed BN coating with Ti–6Al–4V alloy. The formation of titanium boride and titanium nitride investigated using energy dispersive X-ray diffraction (EDXRD) result were related to the microhardness and microstructure. The nitrogen and boron diffusion during the laser boronising process identified using secondary ion mass spectrometry (SIMS) and X-ray photoelectron spectrometry (XPS) analysis was compared with the EDXRD results. The surface hardness HV1500–1700 observed at the boronised layer was five to six times higher than that of untreated Ti–6Al–4V alloy. This was compared with needle platelet and dendrite type microstructures. Theoretically estimated surface temperature values were used to interpret the compound formation in the laser alloyed layer.     

选区激光熔化工艺参数对Ti-6Al-4V成形质量的影响

选区激光熔化是一种利用高能束选择性熔化金属粉末进而直接制造复杂几何形状产品的增材制造技术。采用选区激光熔化成形Ti-6Al-4V样品,分析影响选区激光熔化成形质量的主要因素,采用体式显微镜、金相显微镜、扫描电子显微镜(SEM)、显微硬度计系统研究了不同工艺参数对Ti-6Al-4V合金选区激光熔化成形样品的表面形貌、致密度、组织、显微硬度的影响规律。研究得出Ti-6Al-4V合金选区激光熔化成形的优选工艺参数为:扫描功率450W,扫描速度2 500mm/s,扫描间距0.07mm,该工艺参数下打印出的样品具有较为优良的成形质量,致密度高达97.8%,显微硬度平均值为446HV。     

钛合金激光表面处理研究

本文采用5KWTEACO_2激光器,对 Ti—6Al—4V 钛合金进行表面合金化处理,实验结果表明,经激光辐照后,材料表层及次表层组织结构产生变化,与基体组织大不相同,其硬度有很大提高,由 Hv250提高到 Hv800～900。磨损试验表明,经激光处理的试件,其耐磨性提高2～3倍。扫描电镜分析表明:处理区域由精细枝晶区,等轴细晶区和马氏体区组成,表层硬度的提高及耐磨性的改善与表层组织形态、晶粒细化及硬质点的弥散分布有关。     

Thermophysical Properties of Solid and Liquid Ti-6Al-4V (TA6V) Alloy

Ti-6Al-4V (TA6V) titanium alloy is widely used in industrial applications such as aeronautic and aerospace due to its good mechanical properties at high temperatures. Experiments on two different resistive pulse heating devices (CEA Valduc and TU-Graz) have been carried out in order to study thermophysical properties (such as electrical resistivity, volume expansion, heat of fusion, heat capacity, normal spectral emissivity, thermal diffusivity, and thermal conductivity) of both solid and liquid Ti-6Al-4V. Fast time-resolved measurements of current, voltage, and surface radiation and shadowgraphs of the volume have been undertaken. At TU-Graz, a fast laser polarimeter has been used for determining the emissivity of liquid Ti-6Al-4V at 684.5 nm and a differential scanning calorimeter (DSC) for measuring the heat capacity of solid Ti-6Al-4V. This study deals with the specific behavior of the different solid phase transitions (effect of heating rate) and the melting region, and emphasizes the liquid state (T > 2000 K).     

Measurement of the heat of fusion of titanium and a titanium alloy (90Ti-6Al-4V) by a microsecond-resolution transient technique

A microsecond-resolution pulse heating technique was used for the measurement of the heat of fusion of titanium and a titanium alloy (90Ti-6Al-4V). The method is based on rapid (50- to 100-s) resistive self-heating of the specimen by a high-current pulse from a capacitor discharge system and measuring, as functions of time, current through the specimen, voltage across the specimen, and radiance of the specimen. Melting of the specimen is manifested by a plateau in the measured radiance. The time integral of the net power absorbed by the specimen during melting yields the heat of fusion. The values obtained for heat of fusion were 272 J · g^–1 (13.0 kJ · mol^–1) for titanium and 286 J · g^–1 for the alloy 90Ti-6Al-4V, with an estimated maximum uncertainty of ±6% in each value.Paper presented at the Second Workshop on Subsecond Thermophysics, September 20–21, 1990, Torino, Italy.     

Influences of processing parameters and heat treatment on microstructure and mechanical behavior of Ti-6Al-4V fabricated using selective laser melting

Selective laser melting (SLM) has provided an alternative to the conventional fabrication techniques for Ti-6Al-4V alloy parts because of its flexibility and ease in creating complex features. Therefore, this study investigated the effects of the process parameters and heat treatment on the microstructure and mechanical properties of Ti-6Al-4V fabricated using SLM. The influences of various process parameters on the relative density, tensile properties, impact toughness, and hardness of Ti-6Al-4V alloy parts were studied. By employing parameter optimization, a high-density high-strength Ti-6Al-4V alloy was fabricated by SLM. A relative density of 99.45%, a tensile strength of 1 188 MPa, and an elongation to failure of 9.5% were achieved for the SLM-fabricated Ti-6Al-4V alloy with optimized parameters. The effects of annealing and solution aging heat treatment on the mechanical properties, phase composition, and microstructure of the SLM-fabricated Ti-6Al-4V alloy were also studied. The ductility of the heat-treated Ti-6Al-4V alloy was improved. By applying a heat treatment at 850 ℃ for 2 h, followed by furnace cooling, the elongation to failure and impact toughness were found to be increased from 9.5% to 12.5%, and from 24.13 J/cm² to 47.51 J/cm², respectively.The full text can be downloaded at https://link.springer.com/article/10.1007/s40436-022-00389-y     

Microstructure and notched tensile fracture of Ti–6Al–4V to Ti–4.5Al–3V–2Fe–2Mo dissimilar welds

Dissimilar welding of Ti–6Al–4V (Ti-6-4) to Ti–4.5A1–3V–2Fe–2Mo (SP-700) alloys was performed using a CO₂ laser. The microstructure and notched tensile strength (NTS) of the dissimilar welds were investigated in the as-welded and post-weld heat treatment (PWHT) conditions. Moreover, the results were compared with homogeneous laser welds with the same PWHT. The dilution of SP-700 with the Ti-6-4 alloy caused the formation of fine needle-like α + β structures, resulting in the exhibition of a moderately high fusion zone (FZ) hardness of HV 398. The high FZ hardness (HV 438) for the weld with the PWHT at 482 °C was associated with low NTS or high notch brittleness. The fracture appearance of the notched tensile specimen was related to its inherent microstructure. With increasing the PWHT temperature, the thickness of grain boundary α increased, which promoted an intergranular dimple fracture. By contrast, fine shallow dimples were present in the peak-aged weld, which was induced by the refined α + β microstructures in the basket-weave form.     

Ti-6Al-4V合金表面超声振动滚压强化研究

采用超声振动滚压加工技术对Ti-6Al-4V合金表面进行处理,探究该项技术对Ti-6Al-4V合金表面质量的影响。通过对该工艺加工前后的Ti-6Al-4V合金进行表面粗糙度参数、XRD图谱、截面微观形貌、表层残余应力及显微硬度的对比分析,结果表明:经该工艺处理后的合金表面各项粗糙度参数皆有明显降低;加工后的合金表面XRD图谱的衍射峰减弱且宽化,衍射角向高角度方向偏移;加工后的合金表层β相组织相较加工前明显细化,且随着深度增加β相组织逐渐增大;在距离表面约50μm位置的残余应力值最大可达到-967 MPa;加工后的合金表面显微硬度可达到421HV,且在0~140μm的深度范围内,显微硬度随着深度的增加逐渐减小至与基体硬度一致。经超声振动滚压加工后的Ti-6Al-4V合金表面质量显著提高,有利于提高其零部件的使用性能。     

Ti-12Mo-6Zr-2Fe钛合金的纳米压入特征

利用纳米压入测量仪测试了Ti-12Mo-6Zr-2Fe钛合金的硬度和模量.测试表明,Ti-12Mo-6Zr-2Fe钛合金的硬度比Ti-6Al-4V ELI高,而模量比后者低,与常规方法得到的规律一致,表明该方法能很好地表征钛合金的力学特性.对测试过程的分析表明这种方法得到的结果不能与传统方法得到的结果互换,表面状态对测量结果有一定影响.     

High-temperature thermal barrier coating formation by laser alloying of CP-Ti with pre-placed Ni-SiC coating

High-temperature thermal barrier coating was created on CP-Ti using a pre-placed Ni-SiC layer by laser alloying technique. The coating was developed using 80% Ni + 20% SiC, 50% Ni + 50% SiC and 60% Ni + 40% SiC, and the latter two compositions are found to be efficient in producing a uniform layer. The 100% SiC pre-placement was also used. A flaw-less coating of 0.4–0.6 mm thickness was produced at a lower power density of 1.3 to 1.9 × 10⁵ W cm^–2. Very high power density of 2.5–3.0 × 10⁵ W cm^–2 is inefficient to produce uniform coating. The laser alloyed coating consists of dendrites and intermetallic precipitates. The degree of dendrite population depends upon the coating composition and laser processing conditions. The coating hardness was 600–1200 HV, which is three to six times higher than the base titanium. Uniform hardness was obtained for the coatings produced at a laser power density of 1.3 × 10⁵ W cm^–2. The titanium silicide (TiNiSi, Ti₅Si₃, TiSi) and nickelide (NiTi₂) phases formed on the laser-alloyed coating surface was confirmed by X-ray analysis. These intermetallic phases can improve high-temperature properties of titanium and its alloys. The effect of laser power density and coating composition on the alloying depth alloying width, hardness and microstructure are discussed. The present work investigated the microstructure evolution, hardness and compound phases by means of optical and scanning electron microscopy, Vickers hardness testing, EDXRD and SIMS analysis. A 5 kW CW CO₂ laser was used for laser alloying experiments.     

Characterization and tribological evaluation of duplex treatment by depositing carbon nitride films on plasma nitrided Ti-6Al-4V

Carbon nitride (CN_X) films (with N/C ratio of 0.5) were deposited on both untreated and plasma nitrided Ti-6Al-4V substrates by D.C. magnetron sputtering using a graphite target in nitrogen plasma. TEM and XPS analysis revealed the formation of both amorphous CN_X structure and crystalline -C₃N₄ phases in the deposited coatings. Nano-indentation tests showed that the film hardness was about 18.36 GPa. Both the scratch tests and indentation tests showed that compared with CN_X film deposited directly on Ti-6Al-4V, the load bearing capacity of CN_X film deposited on plasma nitrided Ti-6Al-4V was improved dramatically. Ball-on-disk wear tests under both dry sliding and lubricated conditions (with simulated body fluids) were performed to evaluate the friction and wear characteristics of the deposited coatings. Results showed that under both dry and lubricated conditions, the duplex treated system (i.e., with CN_X film deposited on plasma nitrided Ti-6Al-4V substrate) was more effective in maintaining a favorable low and stable coefficient of friction and improving wear resistance than both individual plasma nitriding and CN_X films on Ti-6Al-4V substrate. Under dry sliding conditions, the generated wear debris of spalled films were accumulated on the wear track, mechanically alloyed and graphitized, thus significantly reducing the coefficient of friction and preventing wear of the substrate. However, under lubricated conditions, due to the flowing of the fluids, the lubricating wear debris was taken away by the fluids, and therefore, the direct contact of two original surfaces resulted in high coefficient of friction and extensive abrasive wear of the substrate for CN_X films deposited on Ti-6Al-4V substrate. Also when there was some small-area spallation of CN_X films, the fluids could seep into the interface between the film and substrate, thus degrading the interfacial adhesion and resulting in a large area spallation.     

Generalized fatigue-failure diagrams for titanium alloys

Summary The effects of various factors have been examined for the cyclic cracking resistance in titanium alloys. Basic fatigue failure diagrams have been constructed for Ti-6Al-4V and Ti-6Al-6V-2Sn in air, distilled water, and 3.5% NaCl. A study has been made on the relationship between the cyclic cracking resistance characteristics and the yield point.Karpenko Physicomechanical Institute, Ukrainian Academy of Sciences, L'vov. Translated from Fiziko-Khimicheskaya Mekhanika Materialov, No. 1, pp. 21–35, January–February, 1993.     

增材制造Ti-6Al-4V合金组织调控研究现状

增材制造技术可实现复杂钛合金零件的快速成形,制造的Ti-6Al-4V合金具有较高的强度以及优异的高温性能,被广泛应用于航空、医疗等各大领域。综述了金属增材制造的典型工艺,分析了Ti-6Al-4V合金的相变特征,总结了选区激光熔化制造Ti-6Al-4V的力学性能和组织调控方法,着重分析了热处理温度、冷却速率、变质处理以及超声冲击等对合金组织的影响;展望了增材制造Ti-6Al-4V合金的主要发展方向。     

Microtwin formation in the α phase of duplex titanium alloys affected by strain rate

The effect of tensile strain rate on deformation microstructure was investigated in Ti-6-4 (Ti-6Al-4V) and SP700 (Ti-4.5Al-3V-2Mo-2Fe) of the duplex titanium alloys. Below a strain rate of 10⁻² s⁻¹, Ti-6-4 alloy had a higher ultimate tensile strength than SP700 alloy. However, the yield strength of SP700 was consistently greater than Ti-6-4 at different strain rates. The ductility of SP700 alloy associated with twin formation (especially at the slow strain rate of 10⁻⁴ s⁻¹), always exceeded that of Ti-6-4 alloy at different strain rates. It is caused by a large quantity of deformation twins took place in the α phase of SP700 due to the lower stacking fault energy by the β stabilizer of molybdenum alloying. In addition, the local deformation more was imposed on the α grains from the surrounding β-rich grains by redistributing strain as the strain rate decreased in SP700 duplex alloy.     

Gas Tungsten Arc Surface Alloying of T1-6A1-4V with Carbon

Ti-6A1-4V was surface alloyed with carbon using gas tungsten arc. Microstructural studies on scanning electron microscope showed that in the alloyed layer a cellular/dendritic phase was distributed in the matrix having an acicular structure. Analysis of the alloyed layer showed an average overall increase of 1.45 wt% in the carbon content. X-ray diffraction studies confirmed the presence of TiC in the alloyed zone. Electron probe microanalysis revealed that the cellular/dendritic phase was rich in carbon and had about 15 wt% carbon, whereas the matrix was depleted in carbon. We concluded from the detailed studies that the alloyed zone matrix was supersaturated with carbon in which TiC was distributed. As a result of this surface treatment, the alloyed layer hardness increased from 350 to 640 HV.     

Nanostructured glass–ceramic coatings for orthopaedic applications

Glass–ceramics have attracted much attention in the biomedical field, as they provide great possibilities to manipulate their properties by post-treatments, including strength, degradation rate and coefficient of thermal expansion. In this work, hardystonite (HT; Ca₂ZnSi₂O₇) and sphene (SP; CaTiSiO₅) glass–ceramic coatings with nanostructures were prepared by a plasma spray technique using conventional powders. The bonding strength and Vickers hardness for HT and SP coatings are higher than the reported values for plasma-sprayed hydroxyapatite coatings. Both types of coatings release bioactive calcium (Ca) and silicon (Si) ions into the surrounding environment. Mineralization test in cell-free culture medium showed that many mushroom-like Ca and phosphorus compounds formed on the HT coatings after 5 h, suggesting its high acellular mineralization ability. Primary human osteoblasts attach, spread and proliferate well on both types of coatings. Higher proliferation rate was observed on the HT coatings compared with the SP coatings and uncoated Ti-6Al-4V alloy, probably due to the zinc ions released from the HT coatings. Higher expression levels of Runx2, osteopontin and type I collagen were observed on both types of coatings compared with Ti-6Al-4V alloy, possibly due to the Ca and Si released from the coatings. Results of this study point to the potential use of HT and SP coatings for orthopaedic applications.