Direct observation of phase transitions by time-resolved pyro/reflectometry of KrF laser-irradiated metal oxides and metals

New experimental results are obtained by coupling both time-resolved reflectivity and rapid infrared pyrometry under a hemispherical reactor. The heating source KrF laser beam (28 ns, 248 nm) is homogenized and as for probing, a CW He-Ne laser beam (10 mW, 633 nm) is used.Using both methods infrared pyrometry with an IR detector cooled with liquid nitrogen and sensitive in the spectral range 1-12 μm, and time-resolved reflectivity with a rapid photodiode, we were able to study complex thermodynamic transitions with nanosecond time resolution. Three different materials are studied by varying the KrF fluence (energy/surface) from 100 to 2000 mJ/cm²: thin films melting (Au/Ni), the threshold of plasma formation (Ti), and complex liquid phase segregation under semi-conductor state (ZnO). The formation of a liquid Zn film induced by temperature gradient is well evidenced by our signals. Also melting of thin films irradiated by low laser fluences (less than 500 mJ/cm²) translates the typical thermodynamic behavior. Finally, wide fluence dynamic (400-2000 mJ/cm²) is analyzed in the case of Ti surface, and results show two distinguished regimes: first one bellow 1000 mJ/cm² corresponding to the early stage plasma initiation, and second one over 1000 mJ/cm² to the dynamics of plasma expansion.     

Time-resolved transmission study of fused silica during laser-induced backside dry etching

Laser-induced backside dry etching (LIBDE) is a promising technique for micro- and nanomachining of transparent materials. Although several experiments have already proved the suitability and effectiveness of the technique, there are several open questions concerning the etching mechanism and the concomitant processes. In this paper time-resolved light transmission investigations of etching process of fused silica are presented. 125 nm thick silver coating was irradiated through the carrying 1 mm thick fused silica plate by single pulses of a nanosecond KrF excimer laser. The applied fluences were 0.38, 0.71 and 1 J/cm². During the etching process the irradiated spots were illuminated by an electronically delayed nitrogen laser pumped dye laser. The delay between the pump and probe pulses was varied in the range of 0 ns and 20 μs. It was found that the transmitted probe beam intensity strongly depends on the applied delays and fluences. Scanning electron microscopy and energy dispersive X-ray spectrometry of the etched surface showed the existence of silver droplets and fragments on the illuminated surfaces and silver atoms built into the treated surface layer influencing the transmission behavior of the studied samples.     

Simulation of dynamics of phase transitions in CdTe by pulsed laser irradiation

Numerical simulation of melting and solidification processes induced in CdTe by nanosecond radiation of ruby laser (λ = 694 nm, τ = 20 and 80 ns) and KrF excimer laser (λ = 248 nm, τ = 20 ns) taking into account components diffusion in melt and their evaporation from the surface has been carried out. Cd atoms evaporation has shown to essentially affect the dynamics of phase transitions in the near-surface region. Thus, in the case of the influence of ruby laser irradiation intensive surface cooling results in the formation of nonmonotone temperature profile with maximum temperature in semiconductor volume at the distance of ∼20 nm from the surface. The melt formed under the surface extends both to the surface and to the semiconductor volume as well. As a result of cadmium telluride components evaporation and diffusion in the melt the near-surface region is enriched with tellurium. The obtained melting threshold value of irradiation energy density is in a reasonable agreement with experimental data.     

Magnetostriction trend of non-oriented 6.5% Si–Fe

Non-oriented electrical steel is produced in strip form typically 0.35–1.0 mm thick and containing 0–3 wt% silicon. It is well-known that non-oriented electrical steel is not quite isotropic but has small anisotropy. In the last decade, NKK produced 0.1 mm thick, non-oriented steel 6.5% Si which has applications such as in high-frequency transformer due to its high electrical resistivity, low core losses, near zero magnetostriction, and high permeability. The magnetostriction of 6.5% silicon steel samples with dimensions 280 mm×30 mm×0.1 mm was measured when magnetised sinusoidally between 0.5 and 1.0 T at frequencies between 0.5 and 6 kHz. Test samples were clamped at one end and the peak-to-peak displacement of the free end was measured with the aid of the single-point laser vibrometer. The average peak–peak magnetostriction was 0.2–0.25 με apart from a sharp rise to 1.2 με at 2 kHz magnetising frequency. This agrees well with the predicted value of 2 kHz for l=0.28 m, d=7430 kg/m³ and E=166 GPa. This shows that although the 6.5% silicon steel is often thought of as having near zero magnetostriction, care is needed to avoid lamination lengths corresponding to resonance points which could induce higher noise in laminated cores.     

Reflection of high-intensity nanosecond Nd:YAG laser pulses by metals

Total reflectivity of silver and molybdenum samples irradiated by high-intensity nanosecond Nd:YAG laser pulses in air of atmospheric pressure is experimentally studied as a function of laser fluence in the range of 0.1–100 J/cm². The study shows that at laser fluences below the plasma formation threshold the total reflectivity of both silver and molybdenum remains virtually equal to the table room-temperature reflectivity values. The total reflectivity of these metals begins to decrease at a laser fluence of the plasma formation threshold. As the laser fluence increases above the plasma formation threshold, the reflectivity sharply drops to a low value and then remains unchanged with further increasing laser fluence. Calculation of the surface temperature at the plasma formation threshold fluence shows that the surface temperature value is substantially below the melting point that indicates an important role of the surface nanostructural defects in the plasma formation on a real sample due to their enhanced heating caused by both plasmonic absorption and plasmonic nanofocusing.     

A comparative study of gadolinium gallium garnet growth by femtosecond and nanosecond pulsed laser deposition

The growth of epitaxial Nd:Gd₃Ga₅O₁₂ (GGG) on Y₃Al₅O₁₂ (YAG) by femtosecond pulsed laser deposition is reported. We have used a Ti:sapphire laser at a wavelength of 800 nm and pulse length of 130 fs, operating at a repetition rate of 1 kHz. The film properties have been studied systematically as a function of the deposition parameters of laser fluence, spot-size, oxygen pressure, target-substrate distance and temperature. Scanning electron microscopy, atomic force microscopy and X-ray diffractometry were used to characterise the surface structure and crystallinity of the films. X-ray diffraction analysis shows that epitaxial growth has occurred. A comparison between the ion velocities produced by nanosecond and femtosecond laser ablation of the GGG target material has been investigated by the Langmuir probe technique. The results indicate a large difference in the plasma characteristics between femtosecond and nanosecond ablation, with ion velocities up to eight times faster observed in the femtosecond case.     

Ceramic components manufacturing by selective laser sintering

In the present paper, technology of selective laser sintering/melting is applied to manufacture net shaped objects from pure yttria-zirconia powders. Experiments are carried out on Phenix Systems PM100 machine with 50 W fibre laser. Powder is spread by a roller over the surface of 100 mm diameter alumina cylinder. Design of experiments is applied to identify influent process parameters (powder characteristics, powder layering and laser manufacturing strategy) to obtain high-quality ceramic components (density and micro-structure).The influence of the yttria-zirconia particle size and morphology onto powder layering process is analysed. The influence of the powder layer thickness on laser sintering/melting is studied for different laser beam velocity V (V = 1250-2000 mm/s), defocalisation (−6 to 12 mm), distance between two neighbour melted lines (so-called “vectors”) (20-40 μm), vector length and temperature in the furnace. The powder bed density before laser sintering/melting also has significant influence on the manufactured samples density.Different manufacturing strategies are applied and compared: (a) different laser beam scanning paths to fill the sliced surfaces of the manufactured object, (b) variation of vector length (c) different strategies of powder layering, (d) temperature in the furnace and (e) post heat treatment in conventional furnace. Performance and limitations of different strategies are analysed applying the following criteria: geometrical accuracy of the manufactured samples, porosity. The process stability is proved by fabrication of 1 cm³ volume cube.     

Features of laser radiation interaction with metals having cryogenic temperature

In this paper we determine the features of the thermophysical processes involved in the interaction of laser radiation with metals that have cryogenic temperature. To do so, we use a one-dimensional model that involves heating a semi-infinite solid by a point thermal source with a constant flux density. Temperature fields, heating and cooling rates in the laser-irradiated zone for iron and titanium at the ambient temperatures of 77 (liquid nitrogen), 293 and 573 K were calculated. The intensity of the laser irradiation enabled the melting temperatures of 1933 K and 1812 K on the Ti and Fe surface, respectively, to be reached. The duration of the laser pulse was 4.5 ms. We show that a drop in ambient temperature from 573 to 77 K leads to a rise in cooling rate from 3.25 × 10³ and 6.4 × 10⁶ K/s to 4.25 × 10³ and 1.3 × 10⁷ K/s in the Ti and Fe targets, respectively. Agreement was good between the calculated depths of melting and phase transformation isotherms and the experimental depths of the interfaces of melting and heat-affected zones.     

Accumulation morphology on the surface of stainless steel irradiated by a nanosecond Nd:YAG pulsed laser

In this study, results in the irradiation of stainless steel AISI 304 in air with nanosecond laser pulses at laser irradiation power density 4×10⁷ W/cm² are reported. Laser processing parameters, such as wavelengths 532 and 1064 nm, pulse duration 20 ns and repetition rate 10 Hz were used. It is shown that the surface morphology of the stainless steel is related to the number of pulses applied to the same spot. The following surface morphological changes were observed: (i) occurrence of the micro-grains microstructures at wavelengths 532 and 1064 nm after 10 000 pulses irradiation and (ii) occurrence of vermiform-like microstructures at wavelength 1064 nm after 1000 pulses irradiation. Generally, it is concluded that irradiation due to several consecutive pulses caused significant damage and enhanced the stainless steel surface roughness.     

Solitary surface acoustic waves and bulk solitons in nanosecond and picosecond laser ultrasonics

Recent achievements of nonlinear acoustics concerning the realization of solitons and solitary waves in crystals and their surfaces attained by nanosecond and picosecond laser ultrasonics are discussed and compared. The corresponding pump-probe setups are described, which allow an all-optical contact-free excitation and detection of short strain pulses in the broad frequency range between 10 MHz and about 300 GHz. The formation of solitons in the propagating longitudinal strain pulses is investigated for nonlinear media with intrinsic lattice-based dispersion. The excitation of solitary surface acoustic waves is realized by a geometric film-based dispersion effect. Future developments and potential applications of nonlinear nanosecond and picosecond ultrasonics are discussed.     

Mechanism of phase conjugation via stimulated Brillouin scattering in narrow band gap semiconductors

We develop a theoretical model to study optical phase conjugation via stimulated Brillouin scattering (OPC-SBS) in narrow band gap transversely magnetized semiconductors. Threshold value of pump electric field and reflectivity of the image radiation for the onset of OPC-SBS are estimated. The analysis is applied to both cases viz. centrosymmetric (CS) and non-centrosymmetric (NCS) crystals. Numerical estimates made for n-type InSb crystal at liquid nitrogen temperature duly irradiated by nanosecond pulsed 10.6 μm CO₂ laser shows that high OPC-SBS reflectivity (90%) can be achieved in NCS crystals at moderate pump electric fields if the crystal is used as an optical waveguide with relatively large interaction length (L = 5 mm) which proves its potential in practical applications such as fabrication of phase conjugate mirrors.     

Reflectivity modification of polymethylmethacrylate by silicon ion implantation

The effect of silicon ion implantation on the optical reflection of bulk polymethylmethacrylate (PMMA) was examined in the visible and near UV. A low-energy (30 and 50 keV) Si⁺ beam at fluences in the range from 10¹³ to 10¹⁷ cm⁻² was used for ion implantation of PMMA. The results show that a significant enhancement of the reflectivity from Si⁺-implanted PMMA occurs at appropriate implantation energy and fluence. The structural modifications of PMMA by the silicon ion implantation were characterized by means of photoluminescence and Raman spectroscopy. Formation of hydrogenated amorphous carbon (HAC) layer beneath the surface of the samples was established and the corresponding HAC domain size was estimated.     

Surface modifications of AISI 1045 steel created by high intensity 1064 and 532 nm picosecond Nd:YAG laser pulses

Interaction of Nd:YAG laser, operating at 1064 or 532 nm wavelength and a pulse duration of 40 ps, with AISI 1045 steel was studied. Surface damage thresholds were estimated to be 0.30 and 0.16 J/cm² at the wavelengths of 1064 and 532 nm, respectively. The steel surface modification was studied at the laser energy density of 10.3 J/cm² (at 1064 nm) and 5.4 J/cm² (at 532 nm). The energy absorbed from Nd:YAG laser beam is partially converted to thermal energy, which generates a series of effects, such as melting, vaporization of the molten material, shock waves, etc. The following AISI 1045 steel surface morphological changes and processes were observed: (i) both laser wavelengths cause damage of the steel in the central zone of irradiated area; (ii) appearance of a hydrodynamic feature in the form of resolidified droplets of the material in the surrounding outer zone with 1064 nm laser wavelength; (iii) appearance of periodic surface structures, at micro- and nano-level, with the 532 nm wavelength and, (iv) development of plasma in front of the target. Generally, interaction of laser beam with the AISI 1045 steel (at 1064 and 532 nm) results in a near-instantaneous creation of damage, meaning that large steel surfaces can be processed in short time.     

Experimental study on reflection of high-intensity nanosecond Nd:YAG laser pulses in ablation of metals

The total reflectivity of tin and magnesium in ablation by nanosecond Nd:YAG laser pulses in air is studied. It was found that the high initial reflectivity of the studied metals undergoes a significant drop to values of 0.11 for Sn and 0.16 for Mg within a laser fluence range between about 0.8 and 11 J/cm². These reduced reflectivity values remain virtually unchanged with further increasing laser fluence. This study shows that a significant reflectivity decrease of the studied metals is caused by plasma formation in front of the irradiated surface. Below the plasma formation threshold, the reflectivity of the studied metals is observed to be virtually independent of laser fluence, indicating a small role of Drude׳s temperature effect on the reflectivity of the studied samples.     

High level compressive residual stresses produced in aluminum alloys by laser shock processing

Laser shock processing (LSP) has been proposed as a competitive alternative technology to classical treatments for improving fatigue and wear resistance of metals. We present a configuration and results for metal surface treatments in underwater laser irradiation at 1064 nm. A convergent lens is used to deliver 1.2 J/cm² in a 8 ns laser FWHM pulse produced by 10 Hz Q-switched Nd:YAG, two laser spot diameters were used: 0.8 and 1.5 mm.Results using pulse densities of 2500 pulses/cm² in 6061-T6 aluminum samples and 5000 pulses/cm² in 2024 aluminum samples are presented. High level of compressive residual stresses are produced −1600 MPa for 6061-T6 Al alloy, and −1400 MPa for 2024 Al alloy. It has been shown that surface residual stress level is higher than that achieved by conventional shot peening and with greater depths. This method can be applied to surface treatment of final metal products.     

Modifications of AISI 1045 steel by picosecond Nd:YAG laser at 266 nm; comparison with 532 and 1064 nm pulses

Interaction of Nd:YAG laser, operating at 266 nm wavelength and a pulse duration of 40 ps, with AISI 1045 steel was studied. Surface damage threshold was estimated to be 0.14 J/cm². The steel surface modification was studied at the laser fluence of ∼1.0 J/cm². The energy absorbed from Nd:YAG laser beam is partially converted to thermal energy, which generates a series of effects, such as melting, vaporization of the molten material, shock waves, etc. The following AISI 1045 steel surface morphological changes and processes were observed: (i) intensive damage of the target in the central zone of irradiated area; (ii) appearance of periodic surface structures at nano-level, with periodicity in agreement with the used wavelength; (iii) reduction of oxygen concentration in irradiated area; and (iv) development of plasma in front of the target. Generally, interaction of laser beam with AISI 1045 steel (at 266 nm) results in a near-instantaneous creation of damage, meaning that large steel surfaces can be modified in short times.     

Lattice dynamics in two-photon-excited CdS studied by picosecond time-resolved X-ray diffraction

Lattice dynamics and radiative processes in single-crystal cadmium sulfide induced by two-photon excitation with a femtosecond laser are investigated. The development of lattice expansion is directly observed by picosecond time-resolved X-ray diffraction. The obtained lattice dynamics are explained on the basis of a thermally induced impulsive-strain model. The model calculation indicates that two- and more-photon absorption processes occur and that reflectivity rapidly increases under laser irradiation. In photoluminescence spectroscopy, the spectra for TW cm⁻² excitation are shifted to lower energy and show an additional shoulder at 2.35 eV. Furthermore, emission due to Fabry-Perot laser modes with self-formed cavities was observed under 11 TW cm⁻² excitation. The discrepancy between carrier densities deduced from the lattice expansion and the PL spectra indicates that the predominant process at a higher carrier density is not radiative recombination, but Auger recombination followed by lattice heating.     

Microstructure and corrosion behavior of austenitic stainless steel treated with laser

Surface modification of AISI316 stainless steel by laser melting was investigated experimentally using 2 and 4 kW laser power emitted from a continuous wave CO₂ laser at different specimen scanning speeds ranged from 300 to 1500 mm/min. Also, an investigation is reported of the introduction of carbon into the same material by means of laser surface alloying, which involves pre-coating the specimen surfaces with graphite powder followed by laser melting. The aim of these treatments is to enhance corrosion resistance by the rapid solidification associated with laser melting and also to increase surface hardness without affecting the bulk properties by increasing the carbon concentration near the surface. Different metallurgical techniques such as optical microscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD) were used to characterize the microstructure of the treated zone. The microstructures of the laser melted zones exhibited a dendritic morphology with a very fine scale with a slight increase in hardness from 200 to 230 Hv. However, the laser alloyed samples with carbon showed microstructure consisting of γ dendrite surrounded by a network of eutectic structures (γ+carbide). A significant increase in hardness from 200 to 500 Hv is obtained. Corrosion resistance was improved after laser melting, especially in the samples processed at high laser power (4 kW). There was shift in I_corr and E_corr toward more noble values and a lower passive current density than that of the untreated materials. These improvements in corrosion resistance were attributed to the fine and homogeneous dendritic structure, which was found throughout the melted zones. The corrosion resistance of the carburized sample was lower than the laser melted sample.     

Two-color laser desorption of nanostructured MgO thin films

Neutral magnesium atom emission from nanostructured MgO thin films is induced using two-color nanosecond laser excitation. We find that combined vis/UV excitation, for single-color pulse energies below the desorption threshold, induces neutral Mg-atom emission with hyperthermal kinetic energies in the range of 0.1-0.2 eV. The observed metal atom emission is consistent with a mechanism involving rapid electron transfer to three-coordinated Mg surface sites. The two-color Mg-atom signal is significant only for parallel laser polarizations and temporally overlapped laser pulses indicating that intermediate excited states are short-lived compared to the 5 ns laser pulse duration.     

Effect of an absorbent overlay on the residual stress field induced by laser shock processing on aluminum samples

Laser shock processing (LSP) or laser shock peening is a new technique for strengthening metals. This process induces a compressive residual stress field, which increases fatigue crack initiation life and reduces fatigue crack growth rate. Specimens of 6061-T6 aluminum alloy are used in this investigation. A convergent lens is used to deliver 2.5 J, 8 ns laser pulses by a Q-switch Nd:YAG laser, operating at 10 Hz. The pulses are focused to a diameter of 1.5 mm onto aluminum samples. Density of 2500 pulses/cm² with infrared (1064 nm) radiation was used. The effect of an absorbent overlay on the residual stress field using this LSP setup and this energy level is evaluated. Residual stress distribution as a function of depth is assessed by the hole drilling method. It is observed that the overlay makes the compressive residual stress profile move to the surface. This effect is explained on the basis of the vaporization of the coat layer suppressing thermal effects on the metallic substrate. The effect of coating the specimen surface before LSP treatment may have advantages on improving wear and contact fatigue properties of this aluminum alloy.