Preparation of lead zirconate titanate nano-powder by electrohydrodynamic atomization

A lead zirconate titanate (PZT) sol was subjected to electrohydrodynamic atomization in the stable cone-jet mode. The droplets generated were sized by laser diffraction before deposition and heating to 600 °C. The droplets were 20–35 m in size and transmission electron microscopy showed that their relics consisted of PZT powder particles, <10 nm in size. Thus, a novel method of preparing nano-powders of functional advanced materials, such as PZT, has been pioneered. PACS 81.20.Ev; 81.20.Rg; 77.84.-s; 81.07.Bc     

Effects of laser fluence on the structural properties of pulsed laser deposited ruthenium thin films

Ruthenium (Ru) has received great interest in recent years for applications in microelectronics. Pulsed laser deposition (PLD) enables the growth of Ru thin films at low temperatures. In this paper, we report for the first time the characterization of pulsed laser deposited Ru thin films. The deposition processes were carried out at room temperature in vacuum environment for different durations with a pulsed Nd:YAG laser of 355-nm laser wavelength, employing various laser fluences ranging from 2 J/cm² to 8 J/cm². The effect of the laser fluence on the structural properties of the deposited Ru films was investigated using surface profilometry, scanning electron microscopy (SEM), and X-ray diffraction (XRD). Ru droplets, some spherical in shape and some flattened into round discs were found on the deposited Ru. The droplets were correlated to ripple formations on the target during the laser-induced ejection from the target. In addition, crystalline Ru with orientations of (100), (101), and (002) was observed in the XRD spectra and their intensities were found to increase with increasing laser fluence and film thickness. Grain sizes ranging from 20 nm to 35 nm were deduced using the Scherrer formula. Optical emission spectroscopy (OES) and energy-dispersive X-ray spectroscopy (EDS) show that the composition of the plume and the deposited Ru film was of high purity.     

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     

Structural and spectral properties of SnO2 nanocrystal prepared by microemulsion technique

Extrafine SnO₂ nanocrystals as small as 2.4 nm were synthesized by the microemulsion method. The grain sizes and crystallization process were measured and investigated by X-ray diffraction. Two growth processes were proposed, and the activation energies of 4.3 and 23 KJ/mol were obtained for respective low-and fast-growth processes. TEM micrographs and the selected-area diffraction recorded their morphology and crystallization, well crystallized at about 773 K. All the IR modes measured by FT-IR spectrometer were assigned. The 616 cm^-1 mode after annealing at 673 K showed fine crystallization. The temperature dependence of the Raman spectra shows that increase in intensity and decrease in linewidth of the 636 cm^-1 mode with the increasing grain size indicate a phonon confinement effect. A new 330 cm^-1 Raman mode originally inactive in bulk, was observed in the SnO₂ nanocrystal by size effect. A low frequency mode at 76 cm^-1 shifts to 38 cm^-1 as the temperature goes up 873 K, which can be characterized to determine the SnO₂ grain sizes. PACS 61.46.+w; 61.10.-i; 78.30.-j; 81.20.-n     

LPE-like growth of YIG ferrimagnetic thin films by pulsed laser ablation with molten droplets

Yttrium iron garnet (YIG) films were grown by pulsed laser ablation (PLA) on (111) Gadolinium Gallium Garnet (GGG) substrates. The second harmonic of YAG laser (532 nm) with a high laser fluence was employed to produce YIG droplets efficiently. It was found that YIG films prepared at RT substrates have a large number of solidified droplets of various sizes. Highly oriented YIG crystals were grown on the (111) GGG substrate heated at 860 °C by PLA using a large number of molten droplets, suggesting an LPE-like growth. This YIG film shows a small ferrimagnetic resonance linewidth of 7.5 Oe. This value is quite small for films prepared by vapor-phase epitaxy techniques.     

Self-assembled nanostructures via electrospraying

A concentrated nanoparticulate-based ethylene glycol suspension was prepared and electrosprayed at optimum and stable cone-jet mode conditions. Using laser spectroscopy, the droplets were measured and found to range within 0.23–3.8 μm. In parallel to spectroscopy-assisted sizing, a volume equivalence route for estimating droplet sizes was carried out by measuring contact angles and diameters of the deposits. The electrosprayed nanosuspension relics were examined using optical and transmission electron microscopy. These deposits were further characterized using energy-dispersive X-rays and selected area electron diffraction. Simultaneously deposits were formed by a controlled route through needle deposition without the presence of an electric field. The structures formed in this non-electric field driven route are compared with those formed with electric fields. Thus, elucidating electrosprays as a competing nanofabrication route for forming self-assemblies with a wide range of nanomaterials in the nanoscale for top-down based bottom-up assembly of structures.     

Fabrication of nano-structured gold films by electrohydrodynamic atomisation

A monodisperse alcosol containing 0.1 wt. % 15 nm gold particles was subjected to controlled flow through a metal capillary exposed to an electric field at the ambient temperature to generate an electrohydrodynamic jet, which subsequently disintegrated into droplets. A silicon substrate was used to collect the droplets and prepare gold films. By varying the deposition time, we have prepared gold films in the thickness range of ∼500–∼ 2000 nm in a maximum spray time of 450 s. This is a significant achievement considering the initial concentration of gold and the spray time involved. The characteristics of the jet, droplets and films prepared were evaluated using advanced analytical techniques. PACS 81.15.Rs; 81.15.-z; 81.07.-b; 81.20.-n; 68.55.jd     

Generation of debris in the femtosecond laser machining of a silicon substrate

A mechanism of debris accumulation around the hole created on a silicon substrate with a femtosecond laser is experimentally studied. The hole created by the laser pulses has an edge consisting of pillared structures. However, no solid or liquid materials with similar dimensions as the pillared structures were ejected from the hole as the laser machining was performed in vacuum or in the presence of various gases. When the target was placed in a gas under 100 Torr, a thick layer of cotton-like material formed around the hole. Laser irradiation of a vertically placed target resulted in re-solidified material that formed after dripping from the hole edge, showing that substrate was partially melted. The surface morphology features suggest that the debris was formed as a result of aggregation of small particles such as atoms or atomic clusters on the substrate surface instead of large-scale droplets or fragments, which are commonly observed with nanosecond lasers. PACS 78.67.Bf; 81.15.Fg; 81.16.Mk; 81.20.Wk; 81.65.Cf     

Modeling of Multiple Scattering Effects in Fraunhofer Diffraction Particle Size Analysis

A model for the direct problem of calculating the forward scattering signature of a multiple scattering medium is presented. The new formulation is optimized for integration into schemes for reconstructing the particle size distribution from laser diffraction (forward scattering) signatures obtained from optically thick media. The analysis is valid for media where the particle sizes and interparticle spacings are large (relative to the wavelength and the particle size, respectively) such that Fraunhofer diffraction theory adequately describes the properties of the forward scattered light from individual scattering events. The simulated performance of laser diffraction particle sizing instruments was then studied using predictions of the scattered light signatures which would be measured by laser diffraction instrument under multiple scattering conditions. The results were compared with experimental data and theoretical calculations based on other models.     

Planar dropsizing by elastic and fluorescence scattering in sprays too dense for phase Doppler measurement

An attempt was made to measure, non-intrusively, average droplet sizes in a dense cooling spray of water. The small droplet size and high number density presented severe problems to conventional nonintrusive measurement methodology with phase Doppler anemometry (PDA). A recently developed optical technique, with more promise for measurements in dense sprays, laser sheet dropsizing (LSD), was tried with more success. Sources of error were considered and the uncertainty of the drop sizes measured by LSD was estimated at ±7%, neglecting multiple scattering, dropsize distribution effects and the contributions of droplets at the edge of the laser beam. The greatest of the known contributions to uncertainty is the calibration of the technique against PDA. The greatest of the unknown contributions is likely to be multiple scattering in such dense sprays. Received: 1 March 2000 / Revised version: 25 May 2000 / Published online: 20 September 2000     

A new NLO Material: L-Asparagine thiocyanate (LATC) for opto-electronic applications

L-asparagine monohydrade thiocyanate (LATC), which is potentially a non-linear optical crystal, was grown by the conventional slow evaporation solution technique (SEST) using doubly de-ionized water at room temperature. The lattice parameters were found by using single crystal X-ray diffraction analysis. Perfection of the grown crystal was confirmed by powder X-ray diffraction. The various functional groups were identified from FT-IR analysis. The optical parameters, such as the optical absorption, the band gap, photoluminescence and second harmonic generation (SHG), were analyzed on the grown crystal. The induced surface laser damage threshold was measured using a Q-switched Nd:YAG laser. The thermal behavior and stability of the grown crystal was analyzed by TG/DTA analysis. The dielectric constant (ε_r) and dielectric loss (tanδ) as a function of frequency has been investigated at different temperatures. The mechanical property of the grown crystal was studied using the Vickers micro hardness method.     

Novel forming of single and multiple ceramic micro-channels

This paper reports a cost-effective processing route for forming micrometre-size channels containing multiple exits/entries. An alumina suspension was electrosprayed in the stable cone-jet mode and the fine ceramic droplets generated were deposited on an organic fibre, which was pre-shaped to the architecture of the micro-channel(s) required. The coated structure was heated to 1400 °C to pyrolyse the fibre and create the ceramic micro-channel(s). PACS 81.20.Rg; 81.05.Je; 07.10.Cm     

Deep drilling on a silicon plate with a femtosecond laser: experiment and model analysis

The ablation rate when drilling fine holes having large aspect ratios in silicon substrates with femtosecond laser pulses was estimated from mechanically ground cross sections of the ablated holes. The ablation rate shows a dramatic change at the depth at which the laser pulse reaches a certain fluence, which is nearly constant when the initial laser fluence was varied from 14.5 to 59.4 J/cm². The ablation rate, threshold fluence, in three fluence domains, and the transition fluences at which the ablation rate shows a dramatic change, were derived. However, when a pulse energy of 200 μJ was used a much greater ablation rate was obtained, suggesting that another fluence domain for larger ablation rates exists. The experimentally obtained hole depths as a function of shot numbers were reproduced by a theoretical model, which incorporates laser pulse attenuation in the holes that is the same as that in waveguides for some attenuation coefficient and ablation rates for three fluence domains. PACS 42.62.-b; 42.65.Re; 78.40.Fy; 78.47.+p; 81.20.Wk     

Wettability modification of electrospun poly(?-caprolactone) fibers by femtosecond laser irradiation in different gas atmospheres

The effect of femtosecond laser irradiation in air and in O₂ and CF₄ gas flows on the wettability of electrospun poly(?-caprolactone) fiber tissue scaffolds was studied. Laser power, focus spot size, raster scan spacing and gas atmosphere were varied in experiments. SEM imaging showed the average fiber diameter and surface porosity sizes were both altered by ablation. The micro-scale surface roughness measured by scanning laser profilometry was found to have a non-monotonic relationship to the surface wettability measured by the contact angle of sessile water droplets. In contrast, surface water contact angle continuously decreased with increased oxygen atomic percentage and oxygen-containing group fraction as measured by XPS. Further, the oxygen content was larger for more extensively ablated fiber surfaces, regardless of whether the increased ablation was caused by high laser power, smaller scanning space or smaller defocusing distance. Of the three gas atmospheres, O₂ gas flow was the most favorable environment for increasing surface oxidization, resulting in the largest water contact angle decrease for given laser power. For CF₄ gas flow, the least oxidization occurred, and the magnitude of water contact angle decrease was smallest for treatment at a given laser power.     

An analysis of the grain growth kinetics in Mn2O3 nanocrystals

The isothermal grain growth of Mn₂O₃ nanocrystals, prepared by the chemical liquid-phase homogeneous precipitation route, was investigated at various temperatures between 200 and 500 °C for different annealing times. X-ray diffraction patterns and transmission electron micrographs show that the average grain sizes are in the range of 4–50 nm. The grain growth data were analyzed using two different models. The first model, assuming normal grain growth as that in conventional polycrystalline materials, yields large grain growth exponent (n) and extremely low activation energy (Q). Although it can describe the evolution of grain sizes, it fails to give satisfactory physical interpretation of n and Q, both beyond the theoretical predictions. The second model is based on the structural relaxation of the interface component in nanocrystalline materials. In this case, the ordering of distorted interfaces by structural relaxation proceeds with grain growth. This structure relaxation model not only describes the evolutions of grain growth well, but also makes reasonable attribution of the low activation energy to the short-range rearrangement of atoms in the interface region as well. PACS 63.50.+x; 78.30.-j; 81.20.-n     

Probing particle-particle interactions in flocculated oil-in-water emulsions using ultrasonic attenuation spectrometry

The flocculation of silicone oil-in-water emulsions ( φ = 0.1) containing quasi-monodisperse droplets was studied by ultrasound. The ultrasonic attenuation spectra of emulsions with different particle sizes (200-1600 nm) were measured between 0.5 and 10 MHz using an interferometer. Flocculation was induced by adding excess sodium dodecyl sulphate micelles to the emulsions to increase the attractive forces between the droplets. Droplet flocculation decreased the ultrasonic attenuation at low frequencies because of overlap of the thermal waves caused by the close proximity of the droplets within the flocs. A mean-field model which takes into account this effect was used to determine the droplet volume fraction within the flocs and thus to estimate the distance between the droplets. Received 17 July 2000     

Modelling of the thermal processes that occur during laser sintering of reacting powder compositions

A two-dimensional mathematical model has been developed to describe simultaneous self-propagating high-temperature synthesis (SHS) and selective laser sintering (SLS) of powder compositions. The models applicability is limited by the magnitude of laser irradiation. It allows a comparison to be made between product geometry and the velocity of the laser irradiation spot. PACS 81.20.ka; 81.05.bx; 81.05.Zx     

Striation-free fibre laser cutting of mild steel sheets

High-power laser cutting is extensively used in many industrial applications. An important weakness of this process is the formation of striations, i.e. regular lines on the cut surface, which lowers the quality of the surfaces produced. The elimination of striation formation is thus of considerable importance, since it could open a variety of novel high-precision applications. This study presents the initial results of a laser cutting study using a 1 kW single-mode fibre laser, a relative newcomer in the field of laser metal cutting. Striation-free laser cuts are demonstrated when cutting 1 mm thick mild steel sheets. PACS 42.62.Cf; 81.05.Bx; 81.20.Wk; 42.55.Wd; 89.20.Bb     

Optical laue diffraction on photonic structures designed by laser lithography

Two-dimensional photonic crystals with square symmetry C_4v were obtained using the laser lithography method. The structure of these samples was studied by scanning electron microscopy. Optical Laue diffraction for monochromatic light was studied experimentally depending on the incidence angle of laser beam and lattice constant. Interpretation of the observed diffraction patterns is given in the framework of the Laue diffraction mechanism for an one-dimensional chain of scattering elements. Red thresholds for different diffraction orders were determined experimentally and theoretically. The results of calculations are in an excellent agreement with experiment.