Laser-induced surface oxidation of (Ni/Ti)/Si system with picosecond laser pulses

The surface oxidation of Ni/Ti bilayer, deposited on silicon substrate, affected by picosecond Nd: YAG laser radiation has been investigated. Fluence close to the target ablation threshold and multi-pulse laser irradiation regime were applied. Changes in the chemical composition of the formed surface oxide layer were studied by Elastic Recoil Detection Analysis (ERDA) and X-ray photoelectron spectroscopy (XPS). Morphological features analysis, at the oxide surface layer, was monitored, too. Laser modification as-deposited (Ni/Ti)/Si sample with 10 pulses induces a progressed interaction between Ni and Ti layers with the initial surface oxidation and formation of NiTi alloy phase. Progressed intermixing of components was achieved for the irradiation with 50 and more pulses, when all components were quite uniformly distributed to a depth of about 80 nm. An oxide layer was formed at the surface, with the specific combination of the oxide phases depending on the number of accumulated pulses. Changes in the morphological characteristics are reflected in the increase of the mean surface roughness and the generation of a certain number of cavities. These features are decreased with increasing number of pulses, caused by the surface melting and a pronounced mobility of the materials.     

激光冲击处理对Ti6Al4V力学性能的影响

通过对钛合金Ti6Al4V的激光冲击处理,研究了激光冲击处理工艺对钛合金Ti6Al4V力学性能的影响.实验表明:激光冲击处理能有效提升Ti6Al4V的力学性能,在激光功率密度由1.15GW/cm2增加到2.31GW/cm2过程中,其冲击波峰值压力线性增加,表面最大残余压应力也相应增大,最高达-264MPa,表面硬化层的显微硬度高达510Hv,硬化层深度约为0.25mm,经过激光冲击处理后硬度相对于原始钛板提高了64%,随着激光能量的增加,冲击区域的抗拉强度极大增强,塑性降低.     

Effects of Laser Repetition Rate and Fluence on Micromachining of TiC Ceramic

Micromachining of titanium carbide (TiC) ceramic is very difficult because of its high hardness and brittleness. Femtosecond pulsed laser was employed to process circular rings on the surface of TiC ceramic. The interaction area between femtosecond laser pulses and TiC at different laser repetition rates and fluences was studied. Morphology and composition of irradiated area were analyzed by scanning electron microscope, energy dispersive spectroscopy, and Raman spectrum. The results indicated that the radius of outer circle was close to the intended radius. Laser fluence had obvious effects on the radius and width of circular rings, compared to laser repetition rate. The width of circular rings increased rapidly with increasing laser fluence from 2.55 × 10^?2 to 1.27 × 10^?1 J/mm², and then stabilized at around 40 µm when laser fluence was above 7.64 × 10^?1 J/mm². The surface of circular rings was characterized by ripples at the lower laser fluence. With increasing laser fluence, four kinds of typical morphology were observed, including ripples, cauliflower-like particles, ball-like particles, and deposited oxide layer. Ball-like particles contained high concentration of titanium, which came from melt ball splashing from ablation area. The others came from the different oxidation stages occurred on the surface of TiC sample.     

Synthesis of ultra-thin oxide layer in laser-treated 3× (Al/Fe)/Si multilayer structure

The conditions of ultra-thin oxide films synthesized as the Al/Fe multilayer structures after the surface treatment with femtosecond laser radiation were studied. Thin films composed of three (Al/Fe) bilayers were deposited by DC ion sputtering on (100) Si wafers to the total thickness of 410 nm. Laser irradiations were performed by 40-fs pulses of a Ti:Sapphire laser operating at 800 nm, at fluences slightly higher than the ablation threshold. The samples were characterized by Auger electron spectroscopy, X-ray photoelectron spectroscopy, and scanning electron microscopy. Progressed intermixing of components was achieved for the irradiation with fluence of 0.43 J cm^?2, when intermetallic phase was formed and all components were almost uniformly distributed through the entire multilayer structure. Exception is the subsurface region, to the thickness of 20 nm, where the distribution of constructive components and their oxide is changing with the distance from the surface, and this distribution depends on the applied laser fluences. An ultra-thin oxide layer was formed at the surface, with the specific combination of the oxide phases, Al₂O₃ and Fe₂O₃, depending on the applied fluences. Laser-induced modification was accompanied with the ablation of the material and the creation of parallel periodic structures. These effects of laser-induced morphological features are increased with increasing laser fluences, caused by the pronounced mobility of the materials. The special morphology of the laser-assisted synthesis of mixture of Al₂O₃ and Fe₂O₃ in the form of an ultra-thin oxide layer can improve their characteristics for functional applications, as catalysts and sensors.     

Laser surface coating of Mo–WC metal matrix composite on Ti6Al4V alloy

Laser surface alloying of Mo, WC and Mo–WC powders on the surface of Ti6Al4V alloys using a 2 kW Nd-YAG laser was performed. The dilution effect upon the microstructure, microhardness and wear resistance of the surface metal matrix composite (MMC) coating was investigated. With a constant thickness of pre-placed powder, the dilution levels of the alloyed layers were found to increase with the incident laser power. The fabricated surface MMC layer was metallurgically bonded to the Ti6Al4V substrate. The microhardness of the fabricated surface layer was found to be inversely proportional to the dilution level. The EDAX and XRD spectra results show that new intermetallic compounds and alloy phases were formed in the MMC layer. With the existence of Mo content in the pre-placed powder, the β-phase of Ti in the MMC coating can be retained at the quenching process. With increasing weight percentage content of WC particles in the Mo–WC pre-pasted powder, the microhardness and sliding wear resistance of the laser surface coating were increased by 87% and 150 times, respectively, as compared with the Ti6Al4V alloy. The surface friction of the laser-fabricated MMC coatings was also decreased as compared with the worn Ti6Al4V substrate.     

Surface characterization and biocompatibility of titanium alloys implanted with nitrogen by Hardion+ technology

In this study, the new Hardion+ micro-implanter technology was used to modify surface properties of biomedical pure titanium (CP-Ti) and Ti?C6Al?C4V ELI alloy by implantation of nitrogen ions. This process is based on the use of an electron cyclotron resonance ion source to produce a multienergetic ion beam from multicharged ions. After implantation, surface analysis methods revealed the formation of titanium nitride (TiN) on the substrate surfaces. An increase in superficial hardness and a significant reduction of friction coefficient were observed for both materials when compared to non-implanted samples. Better corrosion resistance and a significant decrease in ion release rates were observed for N-implanted biomaterials due to the formation of the protective TiN layer on their surfaces. In vitro tests performed on human fetal osteoblasts indicated that the cytocompatibility of N-implanted CP-Ti and Ti?C6Al?C4V alloy was enhanced in comparison to that of the corresponding non treated samples. Consequently, Hardion+ implantation technique can provide titanium alloys with better qualities in terms of corrosion resistance, cell proliferation, adhesion and viability.     

Functionally gradient titanium-aluminide composites produced by laser cladding

The laser surface cladding of Ti-Al/TiB₂ composites was investigated as a means of producing a functionally gradient material on a commercially pure Ti substrate. Single and double layers were produced. The processing parameters were: 1.7 kW laser power, 3 mm beam diameter, 3–22 mms^–1 traverse speeds, 2.2–6.2 g min^–1 powder flow rates. The results showed that functionally gradient Ti-Al/TiB₂ systems 2 mm thick, with a progressive increase in the Al content from 0 to 35 wt% Al (50 at % Al) could be produced by vertically overlapping two clad layers using powder mixtures of selected compositions. Microstructural and compositional characterization were performed on single-layer and two-layer clads. Preliminary wear testing carried out on a laser surface Ti-Al/TiB₂ single-clad layer and on commercial-purity titanium demonstrated the beneficial effect of laser cladding on the wear resistance.     

Laser surface processing of Ti6Al4V in gaseous nitrogen: corrosion performance in physiological solution

Laser surface processing was carried out in gaseous nitrogen atmosphere at ambient temperature. The laser scan speed was varied (50–150 cm/min) at constant power of 1500 watts and resulting changes such as microstructural evolution, hardness, and electrochemical response of modified surface in Ringer’s physiological solution at varying pH were studied. Increase in laser scanning speed was found to reduce the thickness of alloyed zone from 258 to 87 μm. The microstructure of laser-modified surface contains dendrites grown perpendicular to the laser traverse direction, beneath which basket weave structure of acicular α (martensite) was prevalent. Hardness at the top surface of laser-processed at 50 cm/min was ∼1137 kg/mm² that reduced with increase in the laser scan speed (577 kg/mm² at 150 cm/min). Laser surface processing shifted the corrosion potential of Ti6Al4V towards noble side as compared to untreated alloy; the maximum shift by ∼494 mV was recorded in pH ∼ 9 solution. Passivation after laser surface modification was improved as currents were at least 1/3 of the untreated Ti6Al4V in passive region. While the pitting potential of untreated material was found to increase from 1.84 V for 4.0 pH to >2.5 V for 9.0 pH, the pitting potential after laser treatment was observed to drop from maximum of 74% for 4.0 pH (at 100 cm/min) to maximum of 42% for 9.0 pH (at 150 cm/min).     

Improving the wear resistance of AA 6061 by laser surface alloying with NiTi

To improve the wear resistance of a popular aluminum alloy AA 6061, a 1.5 mm thick hard surface layer consisting of Ni–Al and Ti–Al intermetallic compounds was synthesized on the alloy by laser surface alloying technique. NiTi powder was preplaced on the aluminum alloy substrate and irradiated with a high-power CW Nd:YAG laser in an argon atmosphere. With optimized processing parameters, a modified surface layer free of cracks and pores was formed by reaction synthesis of Al with Ni and Ti. X-ray diffractometry (XRD) confirmed the main phases in the layer to be TiAl₃ and Ni₃Al. The surface hardness increased from below 100 HV for untreated AA 6061 to more than 350 HV for the laser-treated sample. Accompanying the increase in hardness, the wear resistance of the modified layer reached about 5.5 times that of the substrate.     

Influence of laser power on the corrosive behavior of laser metal deposited Ti6Al4V+Cu in artificially prepared sea water

Titanium alloy is an excellent corrosion resistance material due to its greater affinity with oxygen when exposed to an aggressive medium such as sea water. The protection against attack is due to the oxidizing fume formed into its surface. This paper reports the effect of laser power on the corrosive behavior of laser metal deposited Ti6Al4V alloy with 5 weight percent (wt. %) copper in freshly prepared artificial sea water. The open circuit potential, potentiodynamic polarization curves, and the scanning electron microscope (SEM) morphologies of the entire Ti6Al4V+5 Cu alloy samples had been investigated and reported. From the results obtained, it can be deduced that the laser power is inversely proportional to the corrosion rate. Sample PL3 deposited with a laser power of 1600 W exhibited the best corrosion rate of 0.0123 mm/year when exposed to sea water under aerated condition. The morphologies of the entire laser deposited samples of the scanning electron microscope (SEM) unveiled typical passivity due to the strong inter-atomic bonds between the α/β phases formed with the copper inclusion within the lattices of the titanium alloy.     

Fe+注入增强Ti6Al4V表面喷丸强化层的生物摩擦学性能

为改善Ti6A14V表面喷丸强化层的生物摩擦学性能,把不同参数Fe+注入到直径4 mm喷丸的强化层中.用Nano IndenterⅡ型纳米显微力学探针测定试样改性层的纳米硬度,在MRTR多功能摩擦磨损试验机上以ZrO2球/改性层为摩擦副进行人工唾液和透明质酸钠溶液润滑下的生物摩擦学试验,使用S-3000N扫描电子显微镜分析改性层组织形貌和生物摩擦学试验后的磨痕形貌.结果表明:Fe+注入Ti6A14V表面喷丸强化层的形成相为Fe2Ti.随着注入能量和剂量增加,Fe2Ti含量从3.7％增至4.7％;Fe+注入改性层的纳米硬度从8.46 GPa增至10.29 GPa,都远高于单一喷丸强化层的5.59 GPa;在人工唾液和透明质酸钠溶液润滑下的摩擦因数分别从0.53降至0.38和从0.49降至0.28,都低于单一喷丸强化层的0.62和0.59,磨损呈现不同程度的减轻.Fe+注入能显著提高Ti6AI4V表面单一喷丸强化层的减摩抗磨性能.     

Development of cBN reinforced Ti6Al4V MMCs through laser sintering and process optimization

In this work, a systematic study and optimization on direct metal laser sintering (DMLS) of a cBN reinforced Ti6Al4V metal matrix composite (MMC) has been carried out using the response surface methodology (RSM). Variable process parameters such as volume % of cBN (5–15%), laser power (50–60?W), scanning speed (3500–4500?mm/min), and constant parameters such as laser spot diameter (0.2?mm), hatching gap (0.2?mm), and layer thickness (0.4) were considered for the experiments. The RSM was employed to establish a regression equation to predict different output parameters of the sintered samples such as the wear rate, relative density, and microhardness. Based on the developed model, the influence of process parameters on the wear rate, density, and microhardness were accomplished with optimized results. Hence, the result, thus, obtained showed the maximum hardness and density of 519 HV_0.2 and 4.23?g/cm³, respectively, and the minimum wear of 26.49?µm in a testing time duration of 10 minutes. X-Ray Diffraction (XRD) analysis of the fabricated MMC confirms the presence of different phases such as cBN, AlN, TiN, TiB₂, and TiO₂ as a consequence of a series of chemical reactions among cBN and different elements of Ti6Al4V in an argon atmosphere.     

金属钛激光气体氮化层组织及表面特征

采用连续波Nd-YAG激光在氮气环境中对金属钛进行激光气体氮化处理.利用SEM,XRD,XPS研究氮化层的显微组织、表面成分、结构.结果表明:通过激光气体氮化可以在金属钛表面得到表面相对平滑、无裂纹的氮化层;氮化层与基体材料之间为冶金结合.氮化层主要由枝晶状TiN组成,同时有TiNxOy,TiO2及TiC存在,外表面有C,O污染或吸附;TiN枝晶密度由表面沿深度方向下降.     

Using hybrid ionized physical vapor deposition to control interface reaction during titanium deposition onto aluminum under-layer

For via structures landed on aluminum (Al) lines, ionized metal plasma (IMP) titanium (Ti) liner deposition can induce high via resistance as a result of the reaction between high energy Ti ions and the Al under-layer. The scale of the interface reaction is a function of the energy of the incoming Ti ions. A method to minimize the Ti/Al interface reaction is to introduce a thin protection layer over the Al under-layer prior to IMP Ti liner deposition. A convenient way to implement this method is to use a hybrid process, in which a Ti protection layer is first deposited in non-ionized mode prior to IMP Ti deposition. Hybrid ionized physical vapor deposition has been confirmed to be effective in minimizing the Ti/Al interface reaction during titanium deposition onto the aluminum under-layer.     

钛合金表面加弧辉光离子渗镍铬及其性能研究

采用加弧辉光离子渗金属新技术处理钛合金Ti5Al2.5Sn表面,研究了渗层的相组成特点,成分分布情况,评价了改性层的磨擦摩损性能,及与钛合金基体间的接触腐蚀相容性等。结果表明加弧辉光离子渗技术可以快速地在钛合金表面获得NiCr镀渗复合层。渗层由Ni3Ti等金属间化合物组成,其硬度、耐磨性能均高于离子注氮层,具有较高的抗含Cl^-1水溶液腐蚀性能,在含Cl^-1腐蚀环境中与钛合金基体接触相容。     

Self-assembled right handed helical ribbons of the bone mineral hydroxyapatite

Osteointegration of titanium or its alloy with bone can be greatly improved by calcium phosphate coatings, and further enhanced by an extracellular matrix protein layer such as collagen. In this study, an octacalcium phosphate (OCP)/collagen composite coating layer on Ti6Al4V substrate was prepared using electrolytic deposition method. A layer of OCP mineral consisting of flake-like crystals was first formed on the Ti6Al4V substrate. Subsequently, mineralized collagen fibrils were deposited on the former OCP layer. These collagen fibrils were interconnected and well adhered on the OCP layer so that they were immobilized. The microstructure of the composite coating varied with collagen concentration in the electrolyte. This study could offer a possibility of fabricating a desired surface matrix on orthopedic implants to enhance bone formation and fixation of implants.     

High temperature stability of multicomponent TiAlSiN and CrAlSiN coatings

The high temperature oxidation behavior of TiAlSiN and CrAlSiN coatings was studied. These coatings were deposited on silicon substrates by using a cathodic-arc deposition system with lateral rotating arc cathodes. Titanium, chromium and Al88Si12 cathodes were used for the deposition of TiAlSiN and CrAlSiN coatings. All the deposited Ti(0.49)Al(0.44)Si(0.07)N, Ti(0.41)Al(0.51)Si(0.08)N and Cr(0.50)Al(0.440Si(0.06)N coatings showed B1-NaCl crystal structure and possessed nano-grain sizes of 6-8 nm. For the high temperature oxidation test, the coated samples were annealed at 900 degrees C in air for 2 hours. The Ti(0.41)Al(0.51)Si(0.08)N with higher Al and Si contents possessed lower oxidation rate than that of Ti(0.49)Al(0.44)Si(0.07)N. The oxide layer formed on the Ti(0.49)Al(0.44)Si(0.07)N coatings consisted of large TiO2 and TiAlSiN grains at the oxide-coating interface, followed by a layer of Al2O3 in the near-surface region. The oxidation rate of the Cr(0.50)Al(0.44)Si(0.06)N coated sample was much lower than that of the Ti(0.49)Al(0.44)Si(0.07)N and Ti(0.41)Al(0.51)Si(0.08)N. The dense Al2O3 with amorphous top layer at the oxide-coating interface retarded the diffusion of oxygen into the Cr(0.50)Al(0.44)Si(0.06)N. The deposited Cr(0.50)Al(0.44)Si(0.06)N showed a high temperature performance superior to those of the Ti(0.49)Al(0.44)Si(0.07)N and Ti(0.41)Al(0.51)Si(0.08)N.     

The effects of loading waveform and microstructure on the fatigue response of titanium aero-engine compressor disk alloys

Microstructural variations produced from manufacturing processes and their influence on fatigue crack growth in titanium disks were investigated. Charpy‐tests on titanium disk material were performed and materials with fracture energy values in the range of 3.8–19.1 J/cm² were selected for tests under cyclic loads. Results of Charpy‐tests were compared with fractographic features related to fatigue crack growth in Ti?6Al?3Mo?0.4Si and Ti?6Al?3Mo?2Cr alloys with a two‐phase (α + β) lamellar structure under various cyclic waveforms using specimens made from compressor disks. The material sensitivity to cyclic load waveform can be seen for in‐service disks using a criteria based on fracture energy values determined in Charpy‐tests. A difference in fatigue crack growth periods of 2.5 times was discovered for specimens made from the disk with a filament type microstructure and the mainly globular two‐phase structure of the Ti?6Al?3Mo?0.4Si alloy. The shorter crack growth period correlated with the mainly facetted pattern formation with local zones of fatigue striations when fatigue crack growth is along the planes of the filaments. Fatigue striations are the major fracture surface relief when crack growth occurs in the perpendicular direction to the plane of the filaments. A quantitative fractographic method for estimating the crack growth period for in‐service failed disks was performed for the case of crack development along planes of such microstructural filaments created during the manufacturing process. Specimen tests involving a hold‐time in the cyclic loads are recommended for in‐service accepted titanium disks using a criteria based on the fracture energy value. Selection of disks based on these criteria can indicate a material sensitivity to cyclic load waveforms.     

Treating orthopedic prosthesis with diamond-like carbon: minimizing debris in Ti6Al4V

Prostheses are subject to various forms of failing mechanisms, including wear from ordinary patient motion. Superficial treatments can improve tribological properties of the contact pair, minimizing wear and increasing prostheses lifetime. One possibility is the diamond-like carbon (DLC) coating, where Carbon is deposited with variable ratio of sp²/sp³ structures, leading to an increase in surface hardness. So in this research Ti6Al4V samples were coated with DLC using sputtering process to evaluate the debris release. The Ti6Al4V and Ti6Al4V plus DLC coating surfaces were analyzed using Raman spectroscopy and instrumented indentation (hardness). The wear behavior was tested using a reciprocating linear tribometer. The wear rate was smaller in the coated samples, producing less debris than the untreated Ti6Al4V alloy. Debris morphology was also evaluated, using scanning electronic microscopy, and it was observed that debris size from the coated samples were bigger than those observed from the uncoated Ti6Al4V alloy, above the size that generally triggers biological response from the host.     

Controlling of the morphology of Co–Ti LDH

It is known that Mg–Al layer double hydroxide (Mg–Al LDH) possesses plate-like morphology if carefully crystallized. This work focuses on the preparation of Co–Ti LDH having fibrous morphology or mixture of plate-like and fibrous morphologies. The Co–Ti LDH obtained by precipitation for relatively short aging time showed plate-like morphology. By increasing aging time, the plate-like morphology was transformed into fibrous morphology. The percentage of titanium also played an important role to determine the morphology of Co–Ti LDH. The samples having low percentage of titanium 20% and 17% showed plate-like morphology with a small amount of fibrous morphology if prepared from cobalt nitrate. However, the sample having high percentage of titanium 27% showed a large amount of fibrous morphology with a small amount of plate-like morphology. In the sample having 24% of titanium, SEM images showed needles morphology. Furthermore, in the sample prepared from cobalt chloride with low percentage of titanium 17%, the SEM images show the production of a large amount of fibrous morphology.