Laser surface alloying of an electroless Ni–P coating with Al-356 substrate

Laser surface alloying of an electroless plating Ni–P coatings on an Al-356 aluminium alloy was carried out using a 1-kW pulsed Nd:YAG laser. The microstructure, chemical composition and phase identification of the alloyed layer were determined using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffractometry (XRD), respectively. It was shown that laser surface treatment produced a relatively smooth, crack-free and hard surface layer. The hardness of the surface significantly increased due to the formation of the uniformly distributed fine Ni–Al intermetallic phases. The corrosion behaviour of the surface alloyed specimens in 3.5% NaCl solution at 23 °C was also determined by electrochemical techniques. The laser-alloyed surface showed an improved corrosion and pitting potential compared to the substrate as well as the plated Ni–P coating.     

Effect of welding speed on butt joint quality of Ti–6Al–4V alloy welded using a high-power Nd:YAG laser

Annealed Ti–6Al–4V alloy sheets with 1 and 2 mm thickness are welded using a 4 kW Nd:YAG laser system. The effects of welding speed on surface morphology and shape, welding defects, microstructure, hardness and tensile properties are investigated. Weld joints without or with minor cracks, porosity and shape defects were obtained indicating that high-power Nd:YAG laser welding is a suitable method for Ti–6Al–4V alloy. The fusion zone consists mainly of acicular α′ martensite leading to an increase of approximately 20% in hardness compared with that in the base metal. The heat-affected zone consists of a mixture of α′ martensite and primary α phases. Significant gradients of microstructures and hardness are obtained over the narrow heat-affected zone. The laser welded joints have similar or slightly higher joint strength but there is a significant decrease in ductility. The loss of ductility is related to the presence of micropores and aluminum oxide inclusions.     

Surface Nitridation of Molybdenum by Laser-promoted Reaction

l.IntroductionowingtotheirpromisingproPertiesandPOtentialapplications,transitionmetalni-trideshavedrawngreatattentionandthepreparationandinvestigationofthesecom-poundshavebeenasubjectbothofscientificandoftechnologicalinterest.Transitionmetalnitridescombineadvantagesofexce1lenthardness,highmeltingPOint,goodchemi-calstabilityandhigheIectricalconductivity[11,henceoverlaySofthesecompoundshavefoundwideappIicationsinvariousfie1ds.Molybdenumnitrides,inparticular,havealsoemergedasverypromisingcandi…     

The mechanism of PEO process on Al–Si alloys with the bulk primary silicon

This study focuses on mechanism of ceramic coating on Al–Si alloys with bulk primary Si using plasma electrolytic oxidation (PEO) technology. Al–Si alloys with 27–32%Si in weight were used as substrates. The morphologies, composition and microstructure of PEO coatings were investigated by scanning electron microscopy (SEM) with energy dispersive X-ray system (EDX). Results showed that the PEO process had four different stages. The effect of bulk Si is greatly on the morphology and composition of coatings at first three stages. Anodic oxide films formed on Al and Si phases, respectively. When the voltage exceeded 40 V, glow appeared and concentrated on the localized zone of interface of Al and Si phase. Al–Si–O compounds formed and covered on the dendrite Si phase surface, and the coating on bulk Si, which was silicon oxide, was rougher than that on other phase. If the treatment time was long enough, the coatings with uniform surface morphologies and elements distribution will be obtained but the microstructure of inner layer is looser due to the bulk Si.     

Excimer laser surface treatment of aluminum alloy in nitrogen

The excimer laser nitriding process reported is developed to enhance the mechanical and chemical properties of aluminum alloys. An excimer laser beam is focused onto the alloy surface in a cell containing 1-bar nitrogen gas. A vapor plasma expands from the surface and a shock wave dissociates and ionizes nitrogen. It is assumed that nitrogen from plasma in contact with the surface penetrates to some depth. Thus it is necessary to work with a sufficient laser fluence to create the plasma, but this fluence must be limited to prevent laser-induced surface roughness. The nitrogen-concentration profiles are determined from Rutherford backscattering spectroscopy and scanning electron microscopy coupled to energy-dispersive X-ray analysis. Crystalline quality is evidenced by an X-ray diffraction technique. Transmission electron microscopy gives the in-depth microstructure. Fretting coefficient measurements exhibit a lowering for some experimental conditions. The polycrystalline nitride layer obtained is several micrometers thick and composed of a pure AlN (columnar microstructure) top layer (200–500 nm thick) standing on an AlN (grains) in alloy diffusion layer. From the heat conduction equation calculation it is shown that a 308-nm laser wavelength would be better to increase the nitride thickness, as it corresponds to a weaker reflectance R value for aluminum. Received: 17 October 2000 / Accepted: 19 October 2000 / Published online: 23 May 2001     

Effect of carbon content on the microstructure and the cracking susceptibility of Fe-based laser-clad layer

The laser cladding of Fe-based alloys on a medium carbon steel substrate was performed using a CO₂ laser and Ar shielding gas that was blown into a molten pool. The microstructure and cracking susceptibility of the laser-clad layers were studied in terms of carbon additions. Results show that the small change of the carbon content in the alloy powders can obviously change the microstructure and properties of the layers. When the carbon content is in the range of 0.3–0.4 wt.%, the decrease of the carbon content in alloy powders will increase the hardness and toughness of the layers simultaneously under the same process parameters. As a result, crack-free coatings with high hardness can be obtained. As the carbon content increases from 0.2 wt.% to 0.4 wt.%, the segregation ratio of chromium increases, while the segregation ratios of nickel, manganese, and silicon first decrease and then increase. At the same time, a new designing principle concerning the composition and microstructure has been put forward, and the principal mechanisms of strengthening and toughening of the layers are fine-grain strengthening and low carbon martensitic phase transformation strengthening.     

Laser/sol–gel synthesis: a novel method for depositing nanostructured TiN coatings in non-vacuum conditions

In this work results of experiments on the in situ production of titanium nitride by the reaction of titania sol–gel with a nitrogenous admixture under laser irradiation are reported. A diode laser beam at different powers and traverse speeds was applied to the mixture placed on EN43 mild steel and 316L stainless steel substrates. Composite coatings of titanium nitride and titanium oxide with a hardness of 17–21 GPa have been achieved by this new method. Surface morphology and microstructure of the deposited coatings and substrate surface layers were examined using optical microscopy, scanning electron microscopy, and field-emission gun scanning electron microscopy. Chemical composition was determined by energy-dispersive X-ray analysis. The phases were identified by X-ray diffraction. Results of microhardness and nanohardness at the top surface were evaluated. PACS 81.15.Fg; 81.20.Fw; 81.05.-t     

Surface hardening of titanium by pulsed Nd:YAG laser irradiation at 1064- and 532-nm wavelengths in nitrogen atmosphere

The surface hardness of titanium modified by laser irradiation at different wavelengths in nitrogen atmosphere was investigated. Further, surface characteristics such as morphology, chemical state, and chemical composition in the depth direction were also studied. The size and depth of the craters observed in the laser-irradiated spots increased monotonically with an increase in the laser power. Furthermore, the crater formed by the 532-nm laser was deeper than that formed by the 1064-nm laser for the same laser power. Laser power beyond a certain threshold value was required to obtain a titanium nitride layer. When the laser power exceeds the threshold value, a titanium nitride layer of a few tens of nanometers in thickness was formed on the substrate, whereas a titanium oxide layer containing small amounts of nitrogen was formed when the laser power is below the threshold value. Thus, it was shown that laser irradiation using appropriate laser parameters can successfully harden a titanium substrate, and the actual hardness of the titanium nitride layer, measured by nanoindentation, was approximately five times that of an untreated titanium surface.     

Microstructure and wear properties of TiCN/Ti coatings on titanium alloy by laser cladding

Titanium carbide nitride (TiCN) reinforced Ti coating was fabricated on the surface of Ti–6Al–4V alloy by laser cladding method. Microstructure and wear properties at the surface of the coating in atmosphere were investigated. Three zones can be distinguished of the coating: the clad zone (CZ), the heat affected zone (HAZ) and the substrate. The clad zone is composed of TiCN dendrites, TiO₂ and Ti. A metallurgical bonding between the coating and the substrate was obtained. The microhardness and wear resistance of the TiCN/Ti coating are significantly improved. The average hardness of the coating is about 3 to 6 times of that of the substrate. The friction coefficients of the substrate and the coating are 0.48 and 0.34 respectively. The friction coefficient of the Ti–6Al–4V substrate was insensitive to the normal load, while that of the cladded TiCN/Ti coating was very sensitive to the normal load. The wear mass losses of the cladded samples are much lower than that of the substrate whatever the normal load is.     

Diffusion of silicon in titanium nitride films. Efficiency of TiN barrier layers

Two kinds of reactively evaporated titanium nitride films with columnar (B ₀ films) and fine-grained film structure (B ₊ films) have been examined as diffusion barriers, preventing the silicon diffusion in silicon devices. The silicon diffusion profiles have been investigated by 2 MeV ⁴He⁺ Rutherford backscattering spectrometry (RBS) after annealing at temperatures up to 900° C, in view of application of high-temperature processes. The diffusivity from 400 to 900° C: D (m² s^–1)=2.5×10^–18 exp[–31 kJ/mol/(RT)] in B ₀ layers and D (m² s^–1)=3×10^–19 exp[–26 kJ/mol/(RT) in B ₊ TiN layers. The diffusivities determined correspond to grain boundary diffusion, the difference being due to the different microstructure. The very low diffusivity of silicon in B ₊ TiN layer makes it an excellent high-temperature barrier preventing silicon diffusion.     

Measurement of the electro-optic coefficient of polymer thin films with better spatial resolution

A method for measuring the electro-optic coefficient of polymer films on the basis of an asymmetry Fabry–Perot cavity is introduced. The sample layer is located between two aluminium layers, which are deposited on glass substrates by thermal evaporation. This layer structure is objected to a laser beam, and a variable voltage is applied to the aluminium films resulting in a modulation of the transmitted laser power. The electro-optic coefficient γ₁₃ of the poled polymer film can be calculated by evaluating the Fabry–Perot equation. The spatial resolution is tested with a polymer film that was poled by a needle corona discharge in air through a metal grating with a period of 120 μm. By scanning the sample plate in the direction perpendicular to the grating lines, the spatial resolution is also demonstrated according to the spacing of the poled structure.     

Surface treatment of titanium by Nd:YAG laser irradiation in the presence of nitrogen

This work presents the surface treatment of commercial titanium alloy by means of a Nd:YAG (1.064 7m) laser in the presence of nitrogen. The treated surface was characterised by using scanning electron microscopy, atomic force microscopy, X-ray diffraction, secondary ion mass spectrometry, UV-visible spectrophotometry and microindentation. Experimental results show the formation of a nitrogen-rich layer, 500 nm thick, with a surface morphology characterised by the presence of polygonal structures which suggest that melting occurred under the action of the laser. The ' phase of titanium nitride was identified, in addition to a nitrogen in !-titanium solid solution. The reflectance spectrum of the yellow-golden sample is similar to that of deposited titanium nitride thin films. The hardness of the treated surface was measured by microindentation and found to be 14 GPa, a value three times higher than that of the titanium alloy. In scratch tests the nitrided layer detached at a load of 0.9 N.     

Fabrication of Zr and Zr-N surface alloying layers and hardness improvement of Ti-6Al-4V alloy by plasma surface alloying technique

Titanium alloys are very attractive materials because they have high specific strength, excellent corrosion and erosion resistance in many active environments. However, their low hardness values and poor tribological properties require improvement of their surface properties. The present study is concerned with the fabrication of Zr and Zr-N alloying layers in the surfaces of Ti-6Al-4V substrates by plasma surface alloying technique. The microstructure, chemical composition and hardness of the surface alloying layers were analyzed to understand the mechanisms of surface alloying and hardness improvement. The Zr and Zr-N surface alloying layers formed were homogeneous and compact, in which the surface alloying elements all displayed gradient distributions. The Zr and Zr-N surface alloying layers all enhanced the surface hardness of Ti-6Al-4V alloy. Zr-N surface alloying resulted in greater improvement in hardness and the maximum microhardness of (1.37 ± 0.04) × 10³ HK was obtained at the subsurface, which was much higher than that of the untreated Ti-6Al-4V alloy. The Zr-N surface alloying layer consisted of an outer nitride layer and an inner diffusion zone of Zr and N, and its very high hardness owed to the formation of the nitride layer. The mechanism of hardness improvement of Zr surface alloyed Ti-6Al-4V alloy was solid solution strengthening.     

Effect of pulsed laser parameters on in-situ TiC synthesis in laser surface treatment

Commercial titanium sheets pre-coated with 300-μm thick graphite layer were treated by employing a pulsed Nd:YAG laser in order to enhance surface properties such as wear and erosion resistance. Laser in-situ alloying method produced a composite layer by melting the titanium substrate and dissolution of graphite in the melt pool. Correlations between pulsed laser parameters, microstructure and microhardness of the synthesized composite coatings were investigated. Effects of pulse duration and overlapping factor on the microstructure and hardness of the alloyed layer were deduced from Vickers micro-indentation tests, XRD, SEM and metallographic analyses of cross sections of the generated layer. Results show that the composite cladding layer was constituted with TiC intermetallic phase between the titanium matrix in particle and dendrite forms. The dendritic morphology of composite layer was changed to cellular grain structure by increasing laser pulse duration and irradiated energy. High values of the measured hardness indicate that deposited titanium carbide increases in the conditions with more pulse duration and low process speed. This occurs due to more dissolution of carbon into liquid Ti by heat input increasing and positive influence of the Marangoni flow in the melted zone.     

Experimental studies on the microstructure and hardness of laser-treated steel specimens

An experimental investigation with 5 kW CW CO₂ laser system was carried out to study the effects of different laser and process parameters on the microstructure and hardness of carbon steel specimen with varying carbon percentage. The laser beam is allowed to scan on the surface of the work piece varying the power (1.1–2.5 kW) and traverse speed (6–15 mm/s) at two different spot sizes using TEM_01* mode laser beam. The most hardenable microstructure achieved in case of three grades of carbon steel and the most influencing parameter on the value of hardness are reported. Besides the above study, some multipass operations are also carried out to recommend an appropriate gap between consecutive passes.     

X-ray photoelectron spectroscopic study on surface reaction on titanium by laser irradiation in nitrogen atmosphere

The surface reaction on titanium due to pulsed Nd:YAG laser irradiation in a nitrogen atmosphere was investigated using X-ray photoelectron spectroscopy (XPS). The laser, with a wavelength of 532 nm (SHG mode), was irradiated on a titanium substrate in an atmosphere-controlled chamber, and then the substrate was transported to an XPS analysis chamber without exposure to air. This in situ XPS technique makes it possible to clearly observe the intrinsic surface reaction. The characteristics of the surface layer strongly depend on the nitrogen gas pressure. When the pressure is 133 kPa, an oxynitride and a stoichiometric titanium nitride form the topmost and lower surface layers on the titanium substrate, respectively. However, only a nonstoichiometric titanium oxide layer containing a small amount of nitrogen is formed when the pressure is lower than 13.3 kPa. Repetition of laser shots promotes the formation of the oxide layer, but the formation is completed within a few laser shots. After the initial structure is formed, the chemical state of the surface layer is less influenced by the repetition of laser shots.     

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.     

光纤激光气体氮化钛合金发射光谱及等离子体研究

激光气体氮化工艺可在钛合金表面快速生成氮化层,提高钛合金表面硬度和耐磨性,促进钛合金应用.采用光纤激光气体氮化Ti-6Al-4V合金,为了明确氮化过程光谱发射区是否形成等离子体,采用探针法检测了光谱发射区导电性;为了研究工艺参数对光谱特性、光谱发射区温度及等离子数量的影响,采用光谱仪采集了氮化过程发射光谱,并采用高速摄...     

Gate voltage-dependent Aharanov–Bohm experiment in the presence of Rashba spin–orbit interaction

We measured gate voltage-dependent Aharonov–Bohm oscillations in an InGaAs-based two-dimensional electron gas ring with a gate on top of one of the branches. After ensemble averaging, the h/e oscillation spectrum showed smooth oscillatory behavior as a function of the gate voltage. This could be a manifestation of the spin–orbit interaction induced interference.     

Simultaneous formation of contacts and diffusion barriers for VLSI by rapid thermal silicidation of TiW

The formation of (Ti_xW_1–x)Si₂/(Ti_xW_1–x)N, by rapid thermal processing of Ti_xW_1–x on Si in an N₂ ambient is investigated. An activation energy of 1.7 eV is obtained for silicide formation. A distinct snow-ploughing of As atoms is observed during silicide formation whereas the interfacial B concentration decreases with increasing silicide formation temperature. The diffusion barrier properties of the (Ti_xW_1–x)Si₂/(Ti_xWi_1–x)N stack in contact with Al is investigated upon post-metal annealing. No interaction between the layers is found for temperatures as high as 475°C after 60 min. The improved thermal stability of the (Ti_xW_1–x)N layer in contact with Al is attributed to nitrogen blocking of the grain boundaries.