Starting from solid-solutions (SS) of AlCoCrFeNix high-entropy alloys (HEAs) that have been produced with high purity constituent elements by vacuum arc remelting (VAR) method varying the nickel molar ratio x from 0.2 to 2.0, we investigated the synthesis of protective thin films of HEAs and high-entropy nitrides (HENs) with the aid of the pulsed laser deposition (PLD) system. The structure of all ten available bulk targets have been examined by means of X-Ray Diffraction (XRD), as well as their elemental composition by means of energy dispersion X-ray spectroscopy (EDS). Three targets with nickel molar composition x = 0.4, 1.2 and 2.0 corresponding to BCC, mixed BCC and FCC, and finally FCC structures were used for thin film depositions using a KrF excimer laser. The depositions were performed in residual low vacuum (10−7 mbar) and under N2 (10−4 mbar) at room temperature (RT~25 °C) on Si and glass substrates. The deposited films’ structure was investigated using grazing incidence XRD, their surface morphology, thickness and elemental composition by scanning electron microscopy (SEM), EDS and X-ray photoelectron spectroscopy (XPS), respectively. A homemade four-point probe (4PP) set-up was applied to determine layers electrical resistance. Besides, a Nanoindentation (NI) was employed to test films’ mechanical properties. XRD results showed that all deposited films, regardless of the initial structure of targets, were a mixture of FCC and BCC structures. Additionally, the quantitative and qualitative EDS and XPS results showed that the elemental composition of films was rather close to that of the targets. The depositions under an N2 atmosphere resulted in the inclusion of several percentage nitrogen atoms in a metallic nitride type compound into films, which may explain their higher electrical resistivity. The Young’s modulus, nanohardness and friction coefficient values showed that the deposited films present good mechanical properties and could be used as protective coatings to prevent damage in harsh environments.
Carbon thin films of 50–100 nm thickness were synthesized by Pulsed Laser Deposition in vacuum at different laser fluences from 2 to 6 J/cm2. The deposited films were characterized by Raman spectroscopy for compositional assessment, scanning electron microscopy for morphology/thickness evaluations, and X-ray reflectivity for density, thickness, and roughness determinations. The films were ~100 nm thin, smooth, droplet-free, made of a-C:H type of diamond-like carbon. The mechanical properties of synthesized films were studied by nanoindentation and adhesion tests. The films that were obtained at low laser fluences (2, 3 J/cm2) had better mechanical properties as compared to those synthesized at higher fluences. The mean values of hardness were around 20 GPa, while the friction coefficient was 0.06. The deposition conditions of carbon thin films that displayed the best mechanical properties were further used to coat commercial drills. Both uncoated and coated drills were tested on plates that were made of three types of steel: Stainless steel 304, general use AISI 572 Gr 65 steel (OL60), and AISI D3 tool steel (C120). All of the drill edges and tips were studied by optical and scanning electron microscopes. The coated samples were clearly found to be more resistant, and displayed less morphological defects than their uncoated counterparts when drilling stainless steel and OL60 plates. In the case of C120 steel, carbon coatings failed because of the high friction between drill and the metal plate resulting in tip edges blunting that occurred during processing.
15 August 2016 in Journal of Vacuum Science & Technology A
LaB6 thin films were deposited at a temperature of 500 °C under vacuum or Ar atmosphere by the pulsed laser deposition technique on (100) Si substrates using a KrF laser. Grazing incidence x-ray diffraction investigations found that films were nanocrystalline, with grain size dimensions from 86 to 102 nm and exhibited microstrain values around 1.1%. Simulations of the x-ray reflectivity curves acquired from the deposited films showed that films had a density around 4.55 g/cm3, and were very smooth, with a surface roughness root-mean-square of 1.5 nm, which was also confirmed by scanning electron and atomic force microscopy measurements. All films were covered by a ∼2 nm thick contamination layer that formed when samples were exposed to the ambient. Auger electron spectroscopy investigations found very low oxygen impurity levels below 1.5 at. % once the contamination surface layer was removed by Ar ion sputtering. Four point probe measurements showed that films were conductive, with a resistivity value around 200 μΩ cm for those deposited under Ar atmosphere and slightly higher for those deposited under vacuum. Nanoindentation and scratch investigations showed that films were rather hard, H ∼ 16 GPa, E ∼ 165 GPa, and adherent to the substrate. Thermionic emission measurements indicated a work function value of 2.66 eV, very similar to other reported values for LaB6.
In this study, we report the performance improvement of wound dressings by covering them with magnetite-based nanostructured coatings. The magnetite nanoparticles (Fe3O4 NPs) were functionalized with Nigella sativa (N. sativa) powder/essential oil and dicloxacillin and were synthesized as coatings by matrix assisted pulsed laser evaporation (MAPLE). The expected effects of this combination of materials are: (i) to reduce microbial contamination, and (ii) to promote rapid wound healing. The crystalline nature of core/shell Fe3O4 NPs and coatings was determined by X-ray diffraction (XRD). Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) have been coupled to investigate the stability and thermal degradation of core/shell nanoparticle components. The coatings’ morphology was examined by scanning electron microscopy (SEM). The distribution of chemical elements and functional groups in the resulting coatings was evidenced by Fourier transform infrared (FTIR) spectrometry. In order to simulate the interaction between wound dressings and epithelial tissues and to evaluate the drug release in time, the samples were immersed in simulated body fluid (SBF) and investigated after different durations of time. The antimicrobial effect was evaluated in planktonic (free-floating) and attached (biofilms) bacteria models. The biocompatibility and regenerative properties of the nanostructured coatings were evaluated in vitro, at cellular, biochemical, and the molecular level. The obtained results show that magnetite-based nanostructured coatings functionalized with N. sativa and dicloxacillin are biocompatible and show an enhanced antimicrobial effect against Gram positive and Gram negative opportunistic bacteria.
A new method for the synthesis and deposition of tungsten oxide nanopowders directly on the surface of a carbon-fiber-reinforced polymer composite (CFRP) is presented. The CFRP was chosen because this material has very good thermal and mechanical properties and chemical resistance. Also, CFRPs have low melting points and are transparent under ionized radiation. The synthesis is based on the direct interaction between high-power-density microwaves and metallic wires to generate a high-temperature plasma in an oxygen-containing atmosphere, which afterward condenses as metallic oxide nanoparticles on the CFRP. During microwave discharge, the value of the electronic temperature of the plasma, estimated from Boltzmann plots, reached up to 4 eV, and tungsten oxide crystals with a size between 5 nm and 100 nm were obtained. Transmission electron microscopy (TEM) analysis of the tungsten oxide nanoparticles showed they were single crystals without any extended defects. Scanning electron microscopy (SEM) analysis showed that the surface of the CFRP sample does not degrade during microwave plasma deposition. The X-ray attenuation of CFRP samples covered with tungsten oxide nanopowder layers of 2 µm and 21 µm thickness was measured. The X-ray attenuation analysis indicated that the thin film with 2 µm thickness attenuated 10% of the photon flux with 20 to 29 KeV of energy, while the sample with 21 µm thickness attenuated 60% of the photon flux.