Austenite modification of AISI 316L SS by pulsed nitrogen ion beams generated in dense plasma focus discharges

We present the results of a surface modification of AISI 316L stainless steel by surface irradiation with high energy, pulsed nitrogen ion beams generated with 0.8 kJ dense plasma focus. The surface characterization was done using GAXRD, Auger electrons spectroscopy, TEM and optical microscopy. After the irradiation, we found a modification of a 1 μm thick surface layer, on which a gradual lattice expansion of the austenite with the number of irradiation pulses, i.e. with the total nitrogen ion fluence, was observed.In addition, ~ 40 nm close to the surface layer, a disordered lattice structure had been observed through TEM analysis. Those results can be explained in terms of the extreme thermal effect induced on the surface through the fast high energy release during the pulsed ion interaction with the steel surface, followed by an also rapid cooling down process which limits the nitrogen diffusion to the bulk.     

Kinetics of picosecond laser treatment of silver nanoparticles on ITO substrate

In this work, the effect of ITO substrate on Ag NP size, morphology and photoinduced absorption depending on the time of 30 ps laser treatment were explicitly studied. Silver nanoparticles with an average diameter of ∼40 nm supported on indium tin oxide (ITO) were irradiated with a tightly focused pulsed laser (doubled frequency beam) at 532 nm. The size transformation of silver nanoparticles induced by a single pulse of Nd:YAG laser (λ = 532 nm, pulse width = 30 ps) was directly observed by an electron scanning microscopy (FE-SEM) on indium tin oxide surface. Simultaneously the change in the absorption and the corresponding derivatives are also presented. These morphological changes are accompanied by a significant change in the optical absorption properties of the array. This study demonstrates that picosecond laser irradiation is an excellent technique to operate and control the properties of nanostructured materials on solid supports.     

Micro-patterning of Si(100) surfaces by ethanol cluster ion beams

The irradiation of Si(100) surfaces by ethanol cluster ion beams exhibited high-rate sputtering and low-damage formation. The sputtered depth increased with increase of the acceleration voltage for ethanol cluster ions, and the sputtering yield was a few hundreds times larger than that by Ar monomer ion beams. Also, the RBS channeling measurement showed that the irradiation damage was much less than that by Ar monomer ion irradiation. Furthermore, the AFM image showed that the surface roughness of the irradiated Si(100) surface was less than 1 nm. As well as the Si(100) surface, the sputtered depth of the photo-resist surface increased with increase of the acceleration voltage for ethanol cluster ions.Based on these results, micro-patterning with various sizes in a range of 3 μm to 100 μm was performed on the Si(100) surfaces by the ethanol cluster ion irradiation. Various kinds of photo-resist mask patterns such as circle, square and line patterns were made on a Si(100) surface by photo-resist technique. The SEM observation showed that micro-patterns were prepared on the Si (100) surface by the ethanol cluster ion irradiation.     

Characterization and comparison of materials produced by Electron Beam Melting (EBM) of two different Ti–6Al–4V powder fractions

Electron Beam Melting (EBM) has been recognized as a revolutionary technique to produce mass-customized parts to near-net-shape from various metallic materials. The technique produces parts with unique geometries from a powder stock material and uses an electron beam to melt the powder layer-by-layer to fully solid structures. In this study we have investigated the use of two different Ti–6Al–4V powders of different size fractions in the EBM process; a larger 45–100 μm powder, and a smaller 25–45 μm powder. We have also investigated the effects of two build layer thicknesses, 70 μm and 50 μm, respectively. We hypothesize that the smaller powder has the potential to improve surface resolution of parts produced in the EBM process. The EBM as-built parts were investigated regarding surface and bulk chemistry, surface oxide thickness, macro- and microstructure, surface appearance and mechanical properties. We conclude from the results that both powders and both build layer thicknesses are feasible to use in the EBM process. The investigated material properties were not significantly affected by powder size or layer thickness within the studied range of process parameters. However, the surface appearance was found to be different for the samples made with the different powder sizes.     

Submicron-scale depth profiling of residual stress in amorphous materials by incremental focused ion beam slotting

This paper reports a new technique, namely the incremental micro-slotting cutting method, for the investigation of residual stress profiles as a function of depth on a micron scale. The residual-stresses in a peened bulk-metallic glass (BMG) (Zr₅₀Cu₄₀Al₁₀, in atomic per cent) are estimated using finite-element analysis of the surface relaxations, as measured by digital image correlation analysis from field-emission gun scanning electron microscopy images, which occur when a micro-slot is stepwise micro-machined by focused ion beam. The calculation algorithm, which solves this inverse problem of residual-stress estimation, is based on the unit pulses method and is stabilized by a Tikhonov regularization scheme. It is demonstrated on a peened BMG that the new technique allows residual-stress profiles in amorphous materials to be inferred with high spatial definition (∼400 nm). Observations point to the scalability of this method to study residual-stress profiles in volumes as small as 1 × 1 × 0.2 μm³ or less, and is particularly well suited to glasses, but can also be applied to crystalline materials.     

Laser-assisted replication of large-area nanostructures

We proposed and demonstrated a high-throughput fabrication method for large-area nanostructured polymers. The mold used consists of a quartz substrate and a nanostructured diamond-like carbon (DLC) thin film. A laser is irradiated from the back of the mold and only the DLC surface is directly heated. Then the surface of a polymethyl methacrylate (PMMA) film pressed by the mold is melted and the nanostructures are replicated. In this method, replication can be achieved with a low amount of heat and a short cycle time compared with conventional thermal replication. The effects of the laser power density, irradiation time, and environmental temperature on the replication area were experimentally investigated via the spot irradiation of a laser. Furthermore, the temperature distribution around the surfaces of the mold and polymer was investigated by performing numerical simulations. By scanning the laser, we successfully demonstrated the replication of a 500-nm-pitch pattern on a PMMA film with an area of 10 × 10 mm² in about 10 s. This technique is expected to lead to the high-throughput and low-energy fabrication of large-area nanostructured optical films.     

Ion-beam irradiation into biodegradable nanofibers for tissue engineering scaffolds

Tissue engineering scaffolds require cell affinity, biodegradability, and desirable mechanical properties. Poly-_L-lactic acid (PLLA) has been investigated for tissue engineering scaffolds owing to its biodegradability and mechanical strength. Electrospun fibers have large surface area and the fibrous structure provides necessary properties for cell attachment, proliferation, differentiation, and sufficient stiffness. PLLA fibers were irradiated with Kr⁺ at an energy of 50 keV with fluences of 1 × 10¹³, 1 × 10¹⁴, and 1 × 10¹⁵ ions/cm² to improve cell affinity. Morphological change was observed by scanning electron microscopy (SEM). Surface properties were measured by FT-IR-ATR and Raman spectroscopy. L929 cell attachment to Kr⁺-irradiated fibers was evaluated. After the irradiation, the average fiber diameter decreased with high fluence. From the results of the surface analyses, the original chemical bonds were broken and new carbon structures were induced. L929 cell attachment was dramatically improved compared with non-irradiated fibers. Thus, ion-beam irradiated fibers are suitable for tissue engineering scaffolds. This technique is expected to be useful in repairing defects, such as those in nerve, vascular, and liver, in regenerative medicine.     

Cemented carbide surface modifications using laser treatment and its effects on hard coating adhesion

A pulsed HyBrID copper laser (510 nm, 30 ns, 13.8 kHz) was used for the treatment of cemented carbide substrate before deposition of TiCN/Al₂O₃/TiN coating by the MT-CVD process. The influence of the laser treatment on the surface morphology, surface structure and coating adhesion was investigated based on the laser irradiation dynamics used here. The experimental results showed that a large variety of cemented carbide surface textures could be obtained, depending on the laser intensity and number of applied laser pulses. Moreover, this laser process was found to produce some less carbon non-stoichiometric WC phases such as β-WC_1 − x and α-W₂C. Finally, using the Rockwell C adhesion test as output criteria, two sets of laser parameters were identified that produced a surface with adhesion strength comparable to that of commercial tools pretreated by micro-sandblasting.     

Polyacrylic acid as a corrosion inhibitor for aluminium in weakly alkaline solutions. Part I: Weight loss, polarization, impedance EFM and EDX studies

This part is devoted to study the influence of three selected polyacrylic acids (PAAs) with different molecular weights (PAA1 = 1800, PAA2 = 11,000 and PAA3 = 14,000 g mol⁻¹) on the corrosion inhibition of Al in weakly alkaline solutions (pH 8 and 10) at 30 °C. Measurements were conducted under different experimental conditions using chemical (weight loss) and electrochemical (potentiodynamic polarization and impedance) techniques, complemented with ex situ energy dispersive X-ray (EDX) examinations of the electrode surface. Electrochemical frequency modulation (EFM), a non-destructive corrosion measurement technique that can directly give values of corrosion current without prior knowledge of Tafel constants, is also presented here. The results demonstrated that these polymers inhibit the alkaline corrosion of Al. The inhibition effect of these polymers is due to their adsorption on Al surface. The isoelectric point (IEP) of aluminium oxide (pH 9) seems to be an important factor controlling corrosion inhibition and adsorption of the three polymers. The three polymers inhibit the corrosion reaction of aluminium excellently at pH 8, but less effectively at pH 10. Polarization measurements showed that the three polymers act as mixed-type inhibitors. The inhibition efficiencies of these polymers increase with increasing concentration, molecular weight and immersion time. Results obtained from the chemical and electrochemical measurements are in good agreements.     

Design and modelling of a passive wireless pressure sensor

This investigation is concerned with the design and modelling of a passive wireless pressure sensor to detect blood pressure inside an abdominal aortic aneurysm sac after endovascular repair of the aneurysm. The sensor consists of a coil and a capacitor to form an inductor-capacitor (LC) resonant circuit which oscillates electrically at its resonant frequency. This miniature sensor has a size of 6 mm × 6 mm × 1 mm and can be fabricated by microelectromechanical system (MEMS) technology. By activating the sensor with an electromagnetic field, aneurysm sac pressure information can be acquired. The properties and behaviour of this sensor based on computer simulation are also presented in this paper.     

Part II. Large scale applications of NixMn0.8−xMg0.2Fe2O4; 0.1 ≤ x ≤ 0.35 using laser irradiation

Ni_xMn_0.8−xMg_0.2Fe₂O₄; 0.1 ≤ x ≤ 0.35 was prepared by standard ceramic technique at sintering temperature 1200 °C using heating / cooling rate 4 °C/min. The samples were irradiated by Nd YAG pulsed laser with energy of the pulse 250 mJ. X-ray diffractograms reveal cubic spinel structure for all the samples before and after laser irradiation. After laser irradiation, better crystallinity was obtained in a form of an increase in the calculated crystal size. This increase was discussed as due to the change in the valence of some ions like Fe³⁺, Ni²⁺ and Mn²⁺. The conductivity of all the investigated samples decreases after laser irradiation and becomes temperature independent for a wider range than that before irradiation. This was ascribed to electron rearrangement after laser irradiation. Accordingly, these ferrites are recommended to be useful in electronic devices.     

Influence of oxygen ion irradiation on the corrosion aspects of Ti-5%Ta-2%Nb alloy and oxide coated titanium

The corrosion resistance of Ti-5%Ta-2%Nb alloy and DOCTOR (double oxide coating on titanium for reconditioning) coated titanium by O⁵⁺ ion irradiation were compared and investigated for their corrosion behaviour. O⁵⁺ ion irradiations were carried out at a dose rate of 1 × 10¹⁷, 1 × 10¹⁸ and 1 × 10¹⁹ ions/m² at 116 MeV. The surface properties and corrosion resistance were evaluated by using scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray (EDX), glancing-angle X-ray diffraction (GXRD) and electrochemical testing methods. The results of electrochemical investigations in 11.5 N HNO₃ indicated that the open circuit potential (OCP) of DOCTOR coated titanium is nobler than Ti-5%Ta-2%Nb alloy. The potentiodynamic polarization study of Ti-5%Ta-2%Nb alloy and DOCTOR coated specimen indicated decrease in passive current density with increase in ion doses (1 × 10¹⁷ to 1 × 10¹⁹ ions/m²) indicating decrease in anodic dissolution. Nyquist arc behaviour in the electrochemical impedance study substantiated the enhancement in oxide layer stability by O⁵⁺ ion irradiation. AFM results revealed that the DOCTOR coated Ti surface was dense without gross voids, and the surface roughness decreased by O⁵⁺ ion irradiation, but increased after corrosion test. EDX and GXRD patterns of DOCTOR coated Ti sample indicated that the coating was mainly composed of rutile TiO₂. Based on the above results, the O⁵⁺ ion irradiation effect on corrosion behavior of Ti-5%Ta-2%Nb alloy and DOCTOR coated titanium are discussed in this paper.     

Influence of process duration on structure and chemistry of borided low carbon steel

In this study, we employed an ultra-fast boriding technique to grow hard boride layers on low carbon steel substrates using an induction furnace at 900 °C. The technique utilizes an electrochemical cell in which it is possible to achieve very thick (i.e., about 90 μm thick) boride layers in about 30 min. The effects of process duration on boride layer thickness, composition, and structural morphology were investigated using microscopic and X-ray diffraction (XRD) methods. We also developed an empirical equation for the growth rate of boride layers. XRD results revealed two principal boride phases: FeB and Fe₂B thickness of which was very dependent on the process duration. For example, Fe₂B phase was more dominant during shorter boriding times (i.e., up to 15 min.) but FeB became much more pronounced at much longer durations. The growth rate of total boride layer was nearly linear up to 30 min of treatment. However during much longer process duration, the growth rate assumed a somewhat parabolic character that could be expressed as d = 1.4904 (t)^0.5 + 11.712), where d (in μm) is the growth rate, t (in s) is duration. The mechanical characterization of the borided surfaces in plane and in cross-sections has confirmed hardness values as high 19 GPa at or near the borided surface (where FeB phase is present). However, the hardness gradually decreased to 14 to 16 GPa levels in the region where Fe₂B phase was found.     

Biocompatibility control of recombinant collagen by ion beam modification

Collagen, which is widely used as a biomaterial because of its excellent tissue compatibility, is generally extracted from animal tissues. The animal-derived biomaterials have the potential for viral or infectious agent contamination risks and allergic reaction problems. Therefore, this study focused on a recombinant human collagen which was pure and homogeneous, compared to the collagen derived from animals. Recombinant human type I collagen was modified by using an ion beam to control the biocompatibility for the substrates of medical devices. He⁺ ion beam irradiation of the recombinant collagen was performed at an energy of 150 keV with fluences of 1 × 10¹³, 1 × 10¹⁴ and 1 × 10¹⁵ ions/cm². To investigate anti-thrombogenicity, Ca²⁺-replenished platelet-rich plasma (PRP) was placed in contact with the surfaces for 5 min. Platelet response was significantly inhibited at a fluence of 1 × 10¹⁴ ions/cm², although the surfaces of the non-modification and other fluences promoted this response. Endothelial cells were cultured on the surfaces for 4 days to evaluate the cellular response. The cell-adhesive property of the recombinant collagen still remained at the fluences of 1 × 10¹⁴ ions/cm² or less; however, the surface modified with a fluence of 1 × 10¹⁵ ions/cm² dramatically inhibited the cell adhesion. These results suggest that platelet and cell adhesion onto the recombinant collagen surface can be individually controlled by the fluence of 150 keV He⁺ ion beam modification. It is concluded that the recombinant collagen surface modified with a fluence of 1 × 10¹⁴ ions/cm² not only retains cell-adhesive property but also possesses anti-thrombogenicity.     

Glass biochip fabrication by laser micromachining and glass-molding process

Due to their low cost, small size, and high-speed performance, biochips are often used in various bio-experiments. Compared with polymer-based biochips, glass-based substrates are less sensitive to heat and organic environments. This study presents a hybrid processing approach that uses laser micromachining (LMM) and precision glass molding (PGM) techniques to mass-produce glass-based biochips. A silicon carbide (SiC) mold with an outside diameter of 20 mm was used to hot emboss biochip channels measuring 200 μm wide and 185 μm deep. This study also identifies the optimal conditions for glass molding when processing soda-lime glass for biochip applications, and discusses the influence of the major processing parameters on biochip channel depth. This study uses the Taguchi method to assess the effects of several molding parameters on larger-the-better performance characteristics. The experiments in this study consider the effects of several molding parameters, such as molding temperature, pressing force, moving speed, temperature holding time, and vacuum environment, to achieve optimum characteristics for biochip channels. Orthogonal array analysis indicates that the optimal process parameters includes a 620 °C molding temperature, 1 kN pressing force, 5 mm/min moving speed, 60 s temperature holding time, and a vacuum-free environment. This study also investigates the surface roughness of glass biochip channels.     

Corrosion inhibition study of pure Al and some of its alloys in 1.0 M HCl solution by impedance technique

This paper describes the use of the potentiodynamic polarization and electrochemical impedance spectroscopy technique (EIS) in order to study the corrosion inhibition process of pure Al, (Al + 6%Cu) and (Al + 6%Si) alloys in 1.0 M HCl solution at the open circuit potential (OCP) in the temperature range 10-60 °C. Dodecyl phenol ethoxidate as a non-ionic surfactant (NS) inhibitor has been examined. The Nyquist diagrams consisted of a capacitive semicircle at high frequencies followed by a well defined inductive loop at low frequency values. The impedance measurements were interpreted according to a suitable equivalent circuit. The results obtained showed that the addition of the surfactant inhibits the hydrochloric acid corrosion of the three Al samples. The inhibition occurs through adsorption of the surfactant on the metal surface without modifying the mechanism of corrosion process. Potentiodynamic polarization measurements showed that the surfactant acts predominately as anodic inhibitor. The inhibition efficiency increases with an increase in the surfactant concentration, but decreases with an increase in temperature. Maximum inhibition is observed around its critical micelle concentration (CMC). The inhibition efficiency for the three Al samples decreases in the order: (Al + 6%Si) > (Al + 6%Cu) > Al. Kinetic-model and Frumkin adsorption isotherm fit well the experimental data. Thermodynamic functions for both dissolution and adsorption processes were determined.     

Electromagnetic reduction of a pre-formed radius on AA 5754 sheet

Electromagnetic (EM) forming is a high-speed forming process that uses the forces induced on a conductive workpiece by a transient high frequency current to form the workpiece into a desired shape. This paper presents the results of an experimental and numerical study carried out to determine whether EM forming techniques could be used to obtain sharper radii in aluminum alloy AA 5754 compared to that attained using conventional stamping process alone. AA 5754 1 mm sheet was formed into a v-shape with a 20 mm outer radius and then the radius was reduced or “sharpened” to 5 mm using EM forming. This “hybrid” process was modeled numerically to gain insight into the process and the challenges involved in the numerical simulation of the physical phenomena that are present in this process. As with any novel process, there are limitations and issues that must be addressed if this technique is to be implemented commercially; however; the research indicates that features that are not achievable using traditional stamping techniques can be obtained using EM forming.     

Improvement of surface flatness in face milling based on 3-D holographic laser metrology

This paper presents two approaches to improve the flatness of face milled surface based on 3-D holographic laser measurement. The first approach, cutting depth compensation method, generates a compensation cutting profile that is ideally a mirror image of the surface profile from a straight cutting path. The surface profile describes the machined surface along the feed direction and is extracted using surface decomposition technique developed in this study. Issues of back-cutting and gouging, which limit the applicability of this approach, are also addressed. The second prescribed approach is the feed rate optimization method. In this technique, the tool feed rate is altered to match the axial force on the cutter with the local compliance of the workpiece. This is performed with the aim of reducing force-induced distortion. Experiments using aluminum workpieces and 50.8 mm diameter face mill demonstrate that the surface flatness can be reduced from 32 to 7 μm with the cutting depth compensation method. With the optimized feed rate, the flatness can be reduced by 19 μm with the same cycle time as that of the original constant feed rate.     

The influence of polymerization time and dopant concentration on the absorption of microwave radiation in conducting polypyrrole coated textiles

Temperature changes in conducting polypyrrole/para-toluene-2-sulphonic acid (PPy/pTSA) coated nylon textiles due to microwave absorption in the 8–9 GHz and 15–16 GHz frequency ranges were obtained by a thermography station during simultaneous irradiation of the samples. The temperature values are compared and related to the amounts of reflection, transmission and absorption obtained with a non-contact free space transmission technique, indicating a relationship between microwave absorption and temperature increase. Non-conductive samples showed no temperature increase upon irradiation irrespective of frequency range. The maximum temperature difference of around 4 °C in the conducting fabrics relative to ambient temperature was observed in samples having 48% absorption and 26.5 ± 4% reflection. Samples polymerized for 60 or 120 min with a dopant concentration of 0.018 mol/l or polymerized for 180 min with a dopant concentration of 0.009 mol/l yielded optimum absorption levels. As the surface resistivity decreased and the reflection levels increased, the temperature increase upon irradiation reduced.     

Ion-assisted vapor deposition of acryl polymer thin films

Polymer thin films were prepared by an ion-assisted vapor deposition polymerization method that involves physical vapor deposition of monomer combined with low-energy ion irradiation. In a high vacuum environment, zinc diacrylate monomer was evaporated at a rate of 0.8 nm/min on gold-coated glass substrates under simultaneous irradiation by nitrogen ions of 20 nA/cm² at ion energy ranging from 500 to 2000 eV. The ion irradiation remarkably reduced the surface roughness of the deposited films. Infrared spectroscopy showed that the absorption bands of the vinyl group diminish with increasing ion energy. Formation of polymer molecules was confirmed by gel permeation chromatograph. Moreover, the film became insoluble to organic solvents when the ion energy was increased. These results indicate that polymer thin films can be prepared by vapor deposition of monomers under ion irradiation. The ion-assisted vapor deposition polymerization was also possible on insulating substrates.