Characteristics of ZrC/ZrN and ZrC/TiN multilayers grown by pulsed laser deposition

ZrC/ZrN and ZrC/TiN multilayers were grown on (1 0 0) Si substrates at 300 °C by the pulsed laser deposition (PLD) technique using a KrF excimer laser. X-ray diffraction investigations showed that films were crystalline, the strain and grain size depending on the nature and pressure of the gas used during deposition. The elemental composition, analyzed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS), showed that films contained a low level of oxygen contamination. Simulations of the X-ray reflectivity (XRR) curves acquired from films indicated a smooth surface morphology, with roughness below 1 nm (rms) and densities very close to bulk values.Nanoindentation results showed that the ZrC/ZrN and ZrC/TiN multilayer samples exhibited hardness values between 30 and 33 GPa, slightly higher than the values of 28-30 GPa measured for pure ZrC, TiN and ZrN films.     

Laser induced mixing in multilayered Ti/Ta thin film structures

The possibility of interlayer mixing in a Ti/Ta multilayer system, induced by laser irradiation, was the main purpose of these experiments. Ti/Ta multilayer system, consisting of ten alternating Ti and Ta thin films and covered by slightly thicker Ti layer, was deposited on Si (100) wafers to a total thickness of 205 nm. Laser irradiation was performed in air by picoseconds Nd:YAG laser pulses in defocused regime with fluences of 0.057 and 0.11 J cm^?2. Laser beam was scanned over the 5?×?5 mm surface area with different steps along y-axes. Structural and compositional characterisation was done by auger electron spectroscopy, X-ray photoelectron spectroscopy, atomic force microscopy, and scanning electron microscopy. Laser processing at lower fluence caused only oxidation of the top Ti layer, despite of the number of applied laser pulses. Interlayer mixing was not observed. Application of laser pulses at fluence of 0.11 J cm^?2 caused partial and/or complete ablation of deposited layers. In partially ablated regions considerable mixing between Ti and Ta films was registered.     

Effects of green laser fluence on the characteristics of graphene nanosheets synthesized by laser ablation method in liquid nitrogen medium

We have studied the effects of laser fluence on the characteristics of graphene nanosheets produced by pulsed laser ablation technique. In this work, The second harmonic of a Q-switched Nd:YAG laser at 532 nm wavelength and 5 Hz repetition rate with different laser fluences in the range of 0.5–1.8 J/cm² was used to irradiate the graphite target in liquid nitrogen medium. The products of ablation were characterized using Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X-ray diffraction pattern, UV–Vis absorption spectroscopy, Raman spectrum and transmission electron microscopy. The Raman spectroscopy indicates that the quality of the graphene nanosheets was decreased while their structure defects were increased as the laser fluence was increased from 0.5 to 1.4 J/cm². Our results suggest that the amount of defects and the number of layers in graphene nanosheets can be changed by adjusting the laser fluence. This study could be a useful guidance for producing of high quality of graphene nanosheets by laser ablation method.     

Optical properties of zinc phthalocyanine thin films prepared by pulsed laser deposition

ZnPc thin films were prepared by pulsed laser deposition (KrF laser, λ = 248 nm, τ = 5 ns, f = 50 Hz) on suprasil substrates in vacuum. Optical properties in UV–Vis spectral region were analyzed as functions of laser fluence from 40 to 100 mJ/cm² by spectrophotometric and spectral ellipsometry measurements. The spectral ellipsometry data were treated using a three-layer model (substrate, film, roughness). The best results of data fitting were obtained when Q band was characterized by two Lorentz oscillators, while two Gaussian oscillators were used for B and C band fitting. We derived the band gap using Tauc plot considering ZnPc a direct band gap semiconductor. The band gap values were found decreasing from 3.13 to 3.09 eV with increasing laser fluence, which might be related with formation of trapping sites at higher fluence.     

Femtosecond laser-induced periodic surface structures on steel and titanium alloy for tribological applications

Laser-induced periodic surface structures (LIPSS, ripples) were generated on stainless steel (100Cr6) and titanium alloy (Ti6Al4V) surfaces upon irradiation with multiple femtosecond laser pulses (pulse duration 30 fs, central wavelength 790 nm). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning geometry for the processing of large surface areas (5 × 5 mm²) covered homogeneously by the nanostructures. The irradiated surface regions were subjected to white light interference microscopy and scanning electron microscopy revealing spatial periods around 600 nm. The tribological performance of the nanostructured surface was characterized by reciprocal sliding against a ball of hardened steel in paraffin oil and in commercial engine oil as lubricants, followed by subsequent inspection of the wear tracks. For specific conditions, on the titanium alloy a significant reduction of the friction coefficient by a factor of more than two was observed on the laser-irradiated (LIPSS-covered) surface when compared to the non-irradiated one, indicating the potential benefit of laser surface structuring for tribological applications.     

Laser-induced fabrication of randomly distributed nanostructures in fused silica surfaces

The nanostructuring of dielectrics is a big challenge for laser patterning methods. In this study a novel laser structuring method for the fabrication of randomly distributed nanostructures, called laser-induced front side etching using in situ pre-structured metal layers (IPSM-LIFE), is presented. The pulsed laser irradiation of a thin metal film deposited onto a dielectric substrate with fluences below the ablation threshold results in the formation of randomly distributed metal structures by self-assembly processes. Further pulsed laser irradiation of these metal structures with higher or equal laser fluences causes the formation of complex patterns at the surface of the dielectric due to localized ablation and melting processes of the dielectric surface induced by the absorption of the laser energy by the metal structures and the local energy transfer into the dielectric surface. The pattern formation observed in the film and the dielectrics substrate after irradiation of 10 nm chromium layers on fused silica, with laser pulses (Δt _p =25 ns, λ=248 nm), was studied by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Different features with a lateral size down to a few tens of nanometers, like concentric ring patterns, donut-like structures, and bar patterns were observed at the dielectric.     

Synthesis of chromium silicide with laser pulses

Thin chromium films, 60 nm thick, were deposited onto single-crystal silicon wafers. The samples were irradiated with 30 ns single pulses from a Nd: glass laser at fluences ranging from 0.4 to 2.25 J/cm². Rutherford backscattering spectrometry, transmission electron microscopy and electron diffraction measurements evidence the formation of CrSi₂ layers at the Cr/Si interface. The silicide thickness depends on the laser fluence.     

Electrical and optical properties of ITO and ITO/Cr-doped ITO films

In this paper we report on the effects of the insertion of Cr atoms on the electrical and optical properties of indium tin oxide (ITO) films to be used as electrodes in spin-polarized light-emitting devices. ITO films and ITO(80 nm)/Cr-doped ITO(20 nm) bilayers and Cr-doped ITO films with a thickness of 20 nm were grown by pulsed ArF excimer laser deposition. The optical, structural, morphological and electrical properties of ITO films and ITO/Cr-doped structures were characterized by UV–Visible transmission and reflection spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and Hall-effect analysis. For the different investigations, the samples were deposited on different substrates like silica and carbon coated Cu grids. ITO films with a thickness of 100 nm, a resistivity as low as ～4×10^?4 Ω?cm, an energy gap of ～4.3 eV and an atomic scale roughness were deposited at room temperature without any post-deposition process. The insertion of Cr into the ITO matrix in the upper 20 nm of the ITO matrix induced variations in the physical properties of the structure like an increase of average roughness (～0.4–0.5 nm) and resistivity (up to ～8×10^?4 Ω?cm). These variations were correlated to the microstructure of the Cr-doped ITO films with particular attention to the upper 20 nm.     

Laser surface texturing of gray cast iron for improving tribological behavior

Laser surface texturing process involves creation of microfeatures, e.g., tiny dimples, usually distributed in a certain pattern, covering only a fraction of the surface of the material that is being treated. The process offers several advantages for tribological applications, including improved load capacity, wear resistance, lubrication lifetime, and reduced friction coefficient. In the present study, the surface modification of gray cast iron, using millisecond (λ = 1,064 nm), nanosecond (λ = 1,064 nm) and femtosecond (λ = 800 nm) pulse duration laser irradiation, is adopted to establish a particular geometrical pattern with dimple features and dimensions, to improve wear and friction behavior. The effect of various laser processing parameters, including laser pulse energy, pulse duration and processing speed, on the performance characteristics of the laser-treated samples is investigated. The microtextured surfaces were produced on gray cast iron using different millisecond (0.5 ms), nanosecond (40 ns) and femtosecond (120 fs) laser source with the dimple depth between 3 and 15 μm. The coefficient of friction for the untextured surface was ~0.55, millisecond laser textured ~0.31, nanosecond laser textured ~0.02 and femtosecond laser ~0.01, under normal force of 50 N and sliding speed of 63 mm/s. Surface texturing of the gray cast iron surface using femtosecond pulse duration resulted in significant improvement in wear resistance in comparison to the untextured as well as millisecond and nanosecond laser-textured surface.     

Influence of bilayer periods on structural and mechanical properties of ZrC/ZrB2 superlattice coatings

ZrC/ZrB₂ multilayered coatings with bilayer periods ranging from 4.4 to 35.5 nm were synthesized by r.f. magnetron sputtering. X-ray diffraction, scanning electron microscopy and nanoindention were employed to investigate the microstructure and mechanical properties of the nanoscale multilayers. The results indicated that all coatings had the clear multilayered structure with mixed ZrB₂(0 0 1), ZrB₂(0 0 2) and ZrC(1 1 1) preferred orientations. The maximum hardness (41.7 GPa) was observed in the multilayer with 27.5-nm thick period, which is about 25% higher than the rule-of-mixture value of the monolithic ZrC and ZrB₂ coatings. It also exhibited the best adhesion. Its critical load was over 70 mN. While through insert ZrB₂ into ZrC layer periodically, higher residual stress built in ZrC layer can be released.     

Evolution of femtosecond laser-induced damage in doped GaN thin films

Mg- and Si-doped GaN layers deposited by metalorganic chemical vapor deposition method were irradiated with femtosecond pulse duration laser of three different wavelengths 1,030, 515 and 343 nm. Both single and multiple shot laser induced damage thresholds of doped GaN layers were evaluated and discussed. The scanning electron microscopy employed with electron beam induced current and energy dispersive X-ray techniques were used to study laser damage morphology. It was observed that ablated area and laser-induced damage increased with irradiation fluence. The mechanism of damage generation by Gaussian beam profile laser was considered.     

Study of optical properties and biocompatibility of DLC films characterized by sp3 bonds

Optical and biomedical properties of diamond-like carbon (DLC) films of various sp², sp³ bonds were studied. The layers were prepared by pulsed laser deposition (PLD) for laser energy densities from 4 J?cm^?2 to 14 J?cm^?2. The percentage of sp² and sp³ bonds was calculated using X-ray photoelectron spectroscopy (XPS). In dependence on density the films contained up to 70 % of sp³ bonds. Optical properties were measured using spectroscopic ellipsometry in region from 250 nm to 1000 nm (n=2.6–2.7; k=0.07–0.25) and by transmission measurement (from 200 nm to 1100 nm). The adhesion and growth of human fibroblasts and keratinocytes of DLC films were tested in vitro.     

Biocompatible film deposition by using Nd:YAG pulsed laser

A Nd:YAG laser operating at the fundamental wavelength (1064 nm) and at the second harmonic (532 nm), with 9 ns pulse duration, 100–900 mJ pulse energy, and 30 Hz repetition rate mode, was employed to ablate in vacuum (10^?6 mbar) biomaterial targets and to deposit thin films on substrate backings. Titanium target was ablated at the fundamental frequency and deposited on near-Si substrates. The ablation yield increases with the laser fluence and at 40 J/cm ² the ablation yield for titanium is 1.2×10¹⁶ atoms/pulse. Thin film of titanium was deposited on silicon substrates placed at different distance and angles with respect to the target and analysed with different surface techniques (optical microscopy, scanning electron spectrosopy (SEM), and surface profile).

Hydroxyapatite (HA) target was ablated to the second harmonic and thin films were deposited on Ti and Si substrates. The ablation yield at a laser fluence of 10 J/cm ² is about 5×10¹⁴ HA molecules/pulse. Thin film of HA, deposited on silicon substrates placed at different distance and angles with respect to the target, was analysed with different surface techniques (optical microscopy, SEM, and Raman spectroscopy).

Metallic films show high uniformity and absence of grains, whereas the bio-ceramic film shows a large grain size distribution. Both films found special application in the field of biomaterial coverage.     

Excimer laser crystallization of amorphous silicon on metallic substrate

An attempt has been made to achieve the crystallization of silicon thin film on metallic foils by long pulse duration excimer laser processing. Amorphous silicon thin films (100 nm) were deposited by radiofrequency magnetron sputtering on a commercial metallic alloy (N42-FeNi made of 41 % of Ni) coated by a tantalum nitride (TaN) layer. The TaN coating acts as a barrier layer, preventing the diffusion of metallic impurities in the silicon thin film during the laser annealing. An energy density threshold of 0.3 J?cm^?2, necessary for surface melting and crystallization of the amorphous silicon, was predicted by a numerical simulation of laser-induced phase transitions and witnessed by Raman analysis. Beyond this fluence, the melt depth increases with the intensification of energy density. A complete crystallization of the layer is achieved for an energy density of 0.9 J?cm^?2. Scanning electron microscopy unveils the nanostructuring of the silicon after laser irradiation, while cross-sectional transmission electron microscopy reveals the crystallites’ columnar growth.     

Biocompatible and bioactive nanostructured glass coatings synthesized by pulsed laser deposition: In vitro biological tests

We report on the synthesis by pulsed laser deposition with a KrF* excimer laser source (λ = 248 nm, τ = 25 ns) of bioglass thin films of 6P57 and 6P61 types. Physiology, viability, and proliferation of human osteoblast cells were determined by quantitative in vitro tests performed by flow cytometry on primary osteoblasts cultured on pulsed laser deposited bioglasses. Both types of glass films proved to be appropriate mediums for cell survival and proliferation. In a parallel investigation, cell morphology and adhesion to the surface was studied by fluorescence microscopy and scanning electron microscopy. Strong bonds between the materials and cells were found in both cases, as osteoblast pseudopodes penetrated deep into the material. According to our observations, the 6P57 glass films were superior with respect to viability and proliferation performances.     

X-ray properties and interface study of B4C/Mo and B4C/Mo2C periodic multilayers

We present a comparative study of B₄C/Mo and B₄C/Mo₂C periodic multilayer structures deposited by magnetron sputtering. The characterization was performed by grazing incidence X-ray reflectometry at two different energies and high resolution transmission electron microscopy. The experimental results indicate the existence of an interdiffusion layer at the B₄C-on-Mo interface in the B₄C/Mo system. Thus, the B₄C/Mo multilayers were modeled by an asymmetric structure with three layers in each period. The thickness of B₄C-on-Mo interfacial layer was estimated about 1.1 nm. The B₄C/Mo₂C multilayers present less interdiffusion and are well modeled by a symmetric structure without interfacial layers. This study shows that B₄C/Mo₂C structure is an interesting alternative to B₄C/Mo multilayer for X-ray optic applications.     

Pulsed laser deposition of PbTe films on glass substrates

PbTe thin films were prepared by pulsed laser deposition from a Nd:YAG laser (532 nm). The films were deposited on glass substrates. The influence of deposition temperature (80-160 °C), fluence (5-13 J/cm²) and nominal composition of the target on the chemical composition of the films was studied. It was found that the tellurium content of the film is strongly dependent on both the laser fluence and the deposition temperature. Highly textured stoichiometric films can be obtained with suitable conditions.     

Deposition and properties of high-carbon iron films

Thin high-carbon iron films were deposited by pulsed laser deposition onto grids for transmission electron microscopy using pre-combined carbon/iron targets with equal area ratio. The deposited films of about 20 nm in thickness were directly characterized by transmission electron microscopy. The films showed a variety of phases, surprisingly also including the NaCl-type FeC phase, which was theoretically predicted in the literature. For comparison, thin high-carbon stainless-steel films were deposited onto oxidized Si wafers with different carbon ratios in the targets (10, 20, 40 and 50 at.%). These films were characterized by means of Mössbauer Spectroscopy, the magneto-optical Kerr-effect, grazing incidence X-ray diffraction and Rutherford backscattering spectrometry. With these methods clearly defined multilayer-structures were observed which could lead to interesting magneto-resistance phenomena if the thickness of the multilayers can be controlled by the processing parameters.     

Stabilization of high spin FCC Fe in (Fe/Pd)n multilayers

Polycrystalline (Fe/Pd)_n multilayers are grown onto sapphire substrates at room temperature in a UHV system. The number of periods n=40 and the thickness of Pd layers of t_Pd=4 nm are kept constant, whereas the thickness of the Fe layers is varied from 1.5 to 5 nm. Structural properties are studied by in situ reflection high energy diffraction (RHEED), scanning tunnelling microscopy (STM) and ex situ by X-ray diffraction at small angles and large angles. Analyzing the experimental data using the program SUPREX we obtain interplanar distances of d_Fe=2.03±0.01 Å for an Fe layer thickness larger than about 2.5 nm as expected for (1 1 0) planes of BCC Fe. For Fe layers with thicknesses less than about 2.5 nm the interplanar distance is d_Fe=2.1±0.01 Å, which is close to the distance between (1 1 1) planes of FCC Fe with a lattice parameter of a=3.64 Å. Magnetic susceptibility measurements at temperatures between 1.5 and 300 K for (Fe/Pd)_n multilayers with FCC Fe yield a magnetic moment per Fe atom of μ=2.7±0.1 μ_B, which is about 20% larger compared to μ=2.2 μ_B for BCC Fe. We show that the occurrence of the large magnetic moment originates from FCC Fe being in the high spin (HS) state rather than from polarization effects of Pd at Fe/Pd interfaces.     

Sub-100-nm laser-induced periodic surface structures upon irradiation of titanium by Ti:sapphire femtosecond laser pulses in air

The formation of laser-induced periodic surface structures (LIPSS) on titanium upon irradiation with linearly polarized femtosecond (fs) laser pulses (τ=30 fs, λ=790 nm) in an air environment is studied experimentally and theoretically. In the experiments, the dependence on the laser fluence and the number of laser pulses per irradiation spot has been analyzed. For a moderate number of laser pulses (N<1000) and at fluences between ～0.09 and ～0.35 J/cm², predominantly low-spatial-frequency-LIPSS with periods between 400 nm and 800 nm are observed perpendicular to the polarization. In a narrow fluence range between 0.05 and 0.09 J/cm², high-spatial-frequency-LIPSS with sub-100-nm spatial periods (～λ/10) can be generated with an orientation parallel to the polarization (N=50). These experimental results are complemented by calculations based on a theoretical LIPSS model and compared to the present literature.