Experimental investigation and metallographic characterization of fiber laser beam welding of Ti-6Al-4V alloy using response surface method

In the present study, experimental investigations of fiber-laser-beam-welding of 5 mm thick Ti-6Al-4V alloy are carried out based on statistical design of experiments. The relationship between the process parameters such as welding power, welding speed, and defocused position of the laser beam with the output responses such as width of the fusion zone, size of the heat affected zone, and fusion zone area are established in terms of regression models. Also, the most significant process parameters and their optimum ranges are identified and their percentage contributions on output responses are calculated. It is observed that welding power and speed plays the major role for full penetration welding. Also, welding power shows direct effect whereas welding speed shows the inverse effect on the output responses. The bead geometry is influenced by the defocused position of the laser beam due to the change in power density on the workpiece surface. However, overall fusion zone area is unaffected. Mechanical characterization of the welded samples such as microstructural analysis, hardness, and tensile tests are conducted. It is noticed that the hardness value of the FZ is higher than the HAZ and BM zone due to the difference in cooling rate during welding which promotes the formation of α′ martensitic phase in the FZ. Also, an average hardness value in the FZ is compared for two different defocusing positions (i.e. 1 and 2 mm). It is found that hardness value is higher for 1 mm defocused position than 2 mm due the decrement in grain size below a critical range at 2 mm defocused position. The ultimate tensile strength and % elongation of the welded samples are degraded as compared to BM which can be further improved by post heat treatment.     

Hydrogen peroxide treatment on Ti-6Al-4V alloy: A promising surface modification technique for orthopaedic application

Ti-6Al-4V alloy was treated with various concentrations (5 wt.%, 15 wt.% and 25 wt.%) of hydrogen peroxide (H₂O₂) and then heat treated to produce an anatase titania layer. The surface modified substrates were immersed in simulated body fluid (SBF) solution for the growth of an apatite layer on the surface and the formed apatite layer was characterized using various surface characterization techniques. The results revealed that titania layer with anatase nature was observed for all H₂O₂ treated Ti-6Al-4V alloy, irrespective of the H₂O₂ concentrations. Ti-6Al-4V alloy treated with 15 wt.% and 25 wt.% of H₂O₂ induced apatite formation, however 5 wt.% of H₂O₂ treated Ti-6Al-4V failed to form apatite layer on the surface. The electrochemical behaviour of H₂O₂ treated specimens in SBF solution was studied using potentiodynamic polarization and electrochemical impedance spectroscopy. Ti-6Al-4V alloy treated with 25 wt.% of H₂O₂ solution exhibited low current density and high charge transfer resistance values compared to specimens treated with other concentrations of H₂O₂ and untreated Ti-6Al-4V alloy.     

CO2 laser gas assisted nitriding of Ti-6Al-4V alloy

Laser gas assisted nitriding of Ti-6Al-4V alloy is carried out and nitride compounds formed and their concentration in the surface vicinity are examined. SEM, XRD and XPS are accommodated to examine the nitride layer characteristics. Microhardness across the nitride layer is measured. Temperature field and nitrogen distribution due to laser irradiation pulse is predicted. It is found that the nitride layer appears like golden color; however, it becomes dark gold color once the laser power irradiation is increased. The δ-TiN and ?-TiN are dominant phases in the surface vicinity. The needle like dendrite structure replace with the feathery like structure in the surface region due to high nitrogen concentration. No porous or microcracks are observed in the nitrided layer, except at high power irradiation, in this case, elongated cracks are observed in the surface region where the nitrogen concentration is considerably high.     

Investigation of the voltage and time effects on the formation of hydroxyapatite-containing titania prepared by plasma electrolytic oxidation on Ti-6Al-4V alloy and its corrosion behavior

Producing titania and hydroxyapatite (HA) bioceramic coating on titanium alloys increases corrosion resistance and biocompatibility of these alloys. Plasma electrolytic oxidation (PEO) is one of the effective techniques for producing this type of coating. This method produces coatings with enough thickness and appropriate adhesion. In this study, titania and HA were directly produced on Ti-6Al-4V by applying PEO process in a Ca- and P-containing electrolyte by changing voltage and time parameters. Morphology and cross section, chemical composition and elements of coatings were investigated by scanning electron microscope, X-ray diffraction and energy dispersive spectroscopy, respectively. Corrosion behavior of the samples was also examined by potentiodynamic polarization and electrochemical impedance spectroscopy. The results indicated that the formation of HA phase with titania needs a minimum voltage below which HA is not formed. By increasing the operation time, the amount of the formed HA increased. Also, the sample coated at 500 V and 15 min showed the best corrosion behavior in Ringer's solution.     

Surface characteristics of self-assembled microporous Ti-6Al-4V compacts fabricated by electro-discharge-sintering in air

A single electro-discharge-sintering (EDS) pulse (1.0 kJ/0.7 g), from a 300 (F capacitor, was applied to atomized spherical Ti-6Al-4V powder in air to produce microporous compact. A solid core surrounded by a porous layer was self-assembled by a discharge in the middle of the compact. X-ray photoelectron spectroscopy was used to study the surface characteristics of the compact material. C, N, O and Ti were the main constituents, with smaller amounts of Al and V. The surface was lightly oxidized and was primarily in the form of TiO₂. A lightly etched EDS sample showed the surface form of metallic Ti, indicating that EDS breaks down the oxide film of the as-received Ti-6Al-4V powder during the discharge process. The EDS Ti-6Al-4V compact surface also contained small amounts of TiN in addition to TiO₂, resulting in the reaction between nitrogen in air and the Ti substrate in times as short as 125 μs.     

Microstructure and tribological behaviors of Ti6Al4V alloy treated by plasma Ni alloying

Ni modified layer was prepared on surface of the Ti6Al4V substrate by plasma surface alloying technique. Surface morphology, micro-structure, composition distribution, phase structure, and microhardness of the Ni modified layer were analyzed. Tribological performance of the Ni modified layer and Ti6Al4V substrate was investigated by using pin-on-disc tribometer. The results indicate that roughness of the Ni modified layer was increased due to formation of the micro-convex on the modified surface. The concentration of Ni gradually decreased from the surface to interior. The maximum content of Ni atoms was nearly 90%. The modified layer was composed of TiNi, Ti2Ni and Ti phases. The maximum microhardness of the Ni modified layer was about 677 HV_0.025 which was increased about two-fold of microhardness of the control Ti6Al4V substrate. Wear resistance of the Ni modified layer was improved obviously, and showed micro-abrasion wearing. The strengthened mechanism of the as-treated Ti6Al4V alloy is discussed.     

Combination of laser keyhole and conduction welding: Dissimilar laser welding of niobium and Ti-6Al-4V

Pulsed Nd:YAG laser welding of pure niobium plate to titanium alloy Ti-6Al-4V sheet in butt joint is studied regarding the laser/metal interaction modes. To obtain the optimized process parameters in dissimilar welding of Ti-6Al-4V/Nb, the melting ratio of laser beam energy for each weld counterpart is evaluated experimentally. Different laser welding modes of keyhole and conduction are predicted regarding the absorbed energy from the similar laser pulses on each weld counterpart. Laser keyhole and conduction welding were observed simultaneously through direct visualization of laser interaction with dissimilar metals using High Speed Imaging (HSI) system.     

TC_4合金TiN激光表面合金化层的组织和硬度研究

通过采用CO_2激光对TC_4合金进行TiN表面合金化处理,探讨了激光功率对合金化层组织和硬度的影响。结果表明,激光合金化试样存在组织不同的三个区域,分别为TiN合金化层,基底熔凝层和淬火层。TiN合金化层由钛合金基体和TiN组成,其中TiN呈现颗粒和树枝晶两种形态。基底熔凝层为定向生长的柱状晶,基底淬火层为针状马氏体。TiN激光合金化层的硬度在700～1100HV之间,约为TC_4合金的2～4倍。     

Growth characteristics of plasma electrolytic oxidation ceramic coatings on Ti-6Al-4V alloy

The aim of this work is to discuss the growth characteristics of the ceramic coatings on Ti alloy by plasma electrolytic oxidation (PEO) technique. Ceramic coatings were prepared on Ti alloy by plasma electrolytic oxidation in different electrolyte solutions under different pulse modes. The composition and the structure of the coatings were investigated by X-ray diffraction and scanning electron microscopy (SEM), respectively. The amount of the dissolved titanium into the electrolytes during PEO process was measured by inductively coupled plasma-atomic emission spectrometer (ICP-AES). The structure and the composition of the coatings were related to the mode of the spark discharge during PEO process. (a) Under the pulsed single-polar mode: In Na₃PO₄ solution, the spark discharge was mainly due to the breakdown of the oxide film, and the coatings prepared were porous and mainly structured by the Ti from the substrate. In K₄ZrF₆-H₃PO₄ and NaAlO₂-Na₃PO₄ solutions, the main mode of the spark discharge was the breakdown of the oxide film at the initial stage, and then changed into the breakdown of the vapor envelope, and the coatings were rough and thick, and mainly structured by the elements from the electrolyte. (b) Under the pulsed bi-polar mode in NaAlO₂-Na₃PO₄ solution, the spark discharge may be mainly due to the breakdown of the oxide film, the coatings prepared were dense in inner layer and loose in outer layer, and structured by the elements from both the substrate and the electrolyte. Besides, the ICP-AES analyses showed that the amount of the dissolved titanium in the electrolyte during PEO process was more under the breakdown of the oxide film than under the breakdown of the vapor envelope, which was consistent with the changes of the structure of the coatings. Cathode pulse in the pulsed bi-polar mode increased the amount of the dissolved titanium in the electrolyte, compared with the pulsed single-polar one.     

Laser diffusion nitriding of Ti-6Al-4V for improving hardness and wear resistance

Owing to poor tribological properties, titanium (Ti) alloys are usually surface-treated to enhance their surface properties. Laser surface nitriding, among others, is a common method employed to increase hardness and wear resistance for Ti alloys. Conventional laser nitriding involves surface melting of Ti alloys in a nitrogen atmosphere. This inevitably results in a roughened surface and post-treatment might be required. The present study aims at laser diffusion nitriding Ti alloys without surface melting via carefully selecting the laser processing parameters. The nitrided surface was characterized by X-ray diffractometry (XRD), optical microscopy (OM), scanning-electron microscopy (SEM), and profilometry. The nitride layer formed was about 1.62 μm upon repeated passes. The change in surface roughness resulting from laser diffusion nitriding was only minimal. Nanoindentation measurements revealed that the hardness of the nitride layer was around 11.3 GPa, being about 2.3 times that of Ti-6Al-4V. Ball-on-slab sliding wear test recorded a reduction in wear volume by about 8 times. The results of the present work thus demonstrate the feasibility of diffusion nitriding of Ti-6Al-4V by laser treatment for enhancing its surface properties and performance.     

Structural characterization of titanium oxide layers prepared by plasma based ion implantation with oxygen on Ti6Al4V alloy

Ti6Al4V alloy was implanted with oxygen by using plasma based ion implantation (PBII) at pulsed voltage ranging from −10 to −50 kV with a frequency of 100 Hz. In order to maintain a lower implantation temperature, an oil cooling working table was employed. The structure of the modified layers was characterized by X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. The results show that the thickness of the titanium oxide layer increases significantly with the increase of implanted voltage. The structure of the modified layer changes along depth. It is found that the surface layer consists of TiO₂, and the subsurface layer is a mixing structure of TiO_2, Ti₂O₃ and TiO. There is crystalline rutile phase existing in the modified layer of sample implanted at high implanted voltage. In addition, in the outmost modified surface, aluminum present as oxidized state, and vanadium could not be detected.     

Structure and tribological performance by nitrogen and oxygen plasma based ion implantation on Ti6Al4V alloy

Ti6Al4V alloy was implanted with nitrogen-oxygen mixture by using plasma based ion implantation (PBII) at pulsed voltage −10, −30 and −50 kV. The implantation was up to 6 × 10¹⁷ ions/cm² fluence. The changes in chemical composition, structure and hardness of the modified surfaces were studied by XPS and nanoindentation measurements. According to XPS, it was found that the modified layer was predominantly TiO₂, but contained small amounts of TiO, Ti₂O₃, TiN and Al₂O₃ between the outmost layer and metallic substrate. Surface hardness and wear resistance of the samples increased significantly after PBII treatment, the wear rate of the sample implanted N₂-O₂ mixture at −50 kV decreased eight times than the untreated one. The sample implanted N₂-O₂ mixture showed better wear resistance than that of the sample only implanted oxygen at − 50 kV. The wear mechanism of untreated sample was abrasive-dominated and adhesive, and the wear scar of the sample implanted at −50 kV was characterized by abrasive wear-type ploughing.     

Laser gas-assisted processing of carbon coated and TiC embedded Ti-6Al-4V alloy surface

Laser gas-assisted treatment of Ti-6Al-4V alloy surface is carried out. The alloy surface is initially coated by a carbon layer, in which the TiC particles are embedded prior to laser processing of the surface. The carbon coating with the presence of TiC particles on the workpiece surface is expected to result in carbonitride compound in the surface vicinity after the laser treatment process. Optical and scanning electron microscopes are used to examine the morphological and the metallurgical changes in the laser treated layer. The residual stress formed in the surface region after the laser treatment process is critical for the practical applications of the resulting surface. Therefore, the residual stress formed in the laser treated region is predicted from the analytically equation. The X-ray diffraction technique is incorporated to obtain the residual stress formed in the surface region. It is found that the residual stress predicted agrees with the X-ray diffraction data. The dense structures consisting of TiC_xN_1−x, TiN_x, Ti₂N, and TiC compounds are formed in the surface region of the treated layer. This, in turn, significantly increases the microhardness at the surface.     

Electrical discharge machining of titanium alloy (Ti-6Al-4V)

In this study, the electrical discharge machining (EDM) of titanium alloy (Ti-6Al-4V) with different electrode materials namely, graphite, electrolytic copper and aluminium and process parameters such as, pulse current and pulse duration were performed to explore the influence of EDM parameters on various aspects of the surface integrity of Ti6Al4V. Scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectrograph (EDS) and hardness analysis were performed. The experimental results reveal that the value of material removal rate, surface roughness, electrode wear and average white layer thickness are tendency of increase with increasing current density and pulse duration. However, extremely long-pulse durations such as 200 μs led to decrease MRR and surface roughness. Furthermore, the surface hardness is increasing due to the Ti₂₄C₁₅ carbides formed on the surface and obvious cracks are always evident in re-solidified layer when machining copper electrode. The surface crack densities and critical crack lines were determined for the tested material. The graphite electrode is beneficial on material removal rate, electrode wear and surface crack density but relatively poorer surface finish.     

Microstructure and wear resistance of composite layers on a ductile iron with multicarbide by laser surface alloying

Multicarbide reinforced metal matrix composite (MMC) layers on a ductile iron (QT600-3) were fabricated by laser surface alloying (LSA) using two types of laser: a 5 kW continuous wave (CW) CO₂ laser and a 400 W pulsed Nd:YAG laser, respectively. The research indicated that LSA of the ductile iron with multicarbide reinforced MMC layers demonstrates sound alloying layers free of cracks and porosities. The microstructure, phase structure and wear properties of MMC layers were investigated by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD), as well as dry sliding wear testing. The microstructure of the alloyed layer is composed of pre-eutectic austenite, ledeburite, spherical TiC, Cr₇C₃ and Cr₂₃C₆ with various morphologies. TiC particles are dispersed uniformly in the upper region of MMC layers. The average hardness of LSA layers by CO₂ laser and pulsed Nd:YAG laser is 859 HV_0.2 and 727 HV_0.2, respectively. The dry sliding wear testing shows the wear resistance of ductile iron is significantly improved after LSA with multicarbide.     

Laser surface micro-texturing of Ti-6Al-4V substrates for improved cell integration

Biological behaviour of an implant, such as osseointegration, depends on both the chemical composition and the morphology of the surface of the implant. This paper reports the surface modification of Ti-6Al-4V - which is widely used in implantation - by Nd:YAG (λ = 1064 nm, τ = 100 ns) laser irradiation in order to enhance biointegration. Surface parameters are evaluated in terms contact angle measurement and surface roughness. Biocompatibility of the samples is investigated in vitro by monitoring 2T3 osteoblast cell growth on the samples through MTT assay.     

Study on the microstructure and wear resistance of the composite coatings fabricated on Ti-6Al-4V under different processing conditions

Composite coatings mainly containing titanium carbides and borides were produced by laser surface alloying of Ti-6Al-4V with graphite and boron mixed powders. The test results show that the coatings have higher hardness (1600-1700 HV_0.1) and are more resistant to wear than the as-received sample. Laser scanning speed and the content of alloying elements (weight ratio of graphite to boron) have an effect on both the microstructure and the wear resistance of the coatings. TEM results show that strip titanium carbides and borides grow alternately and thus restrain the formation of coarse needle-like TiB and dendritic TiC crystals produced by laser alloying of titanium alloys with boron and graphite separately.     

Influence of slight microstructural gradients on the surface properties of Ti6Al4V irradiated by UV

Ti6Al4V alloy is one of the most widely used materials for biomedical implants. Among its properties, it is remarkable the photoactivity displayed by its passive layer, which is mainly composed by titanium dioxide. However, variations in the processing conditions may yield to differences in the microstructure which can be reflected on the surface properties of the machined product. From contact angle measurements taken on different zones of samples removed from a commercial bar of Ti6Al4V, it has been shown that the modifications of the surface Gibbs energy suffered by the alloy under UV irradiation have a radial dependence. This behaviour is related to slight microstructural changes of the alloy, particularly with an increase in the volume fraction of the β-phase when moving to the interior of the sample, which alters the composition and/or microstructure of the passive layer along its radius. This study shows that gradients in the microstructure and physical properties are sample size dependent and are likely related to thermal gradients during processing.