In situ scanning electron microscopy indentation studies on multilayer nitride films: Methodology and deformation mechanisms

Systematic studies of the deformation mechanisms of multilayer transition metal nitride coatings TiN/CrN, TiN/NbN, and NbN/CrN, and corresponding reference coatings of TiN, NbN, and CrN deposited by a direct current (dc) magnetron sputtering process onto silicon 〈100〉 have been performed. Mechanical characterization was conducted using a combination of microindentation and nanoindentation in the load range 30 to 150 mN and 0.5 to 3.5 mN, respectively. For both load ranges, scanning electron microscopy (SEM) in situ indentation was used to observe the indentation process including any pileup, sink-in, and fracture mechanisms specific to each coating. The coatings' microstructure, both before and after indentation, was analyzed using transmission electron microscopy (TEM). It was possible to both correlate the indentation load-displacement response to surface roughness effects and fracture modes (substrate and film cracking) and observe deformation mechanisms within the coating

Effect of Nb doping on structural, optical and photocatalytic properties of flame-made TiO2 nanopowder

TiO2:Nb nanopowders within a dopant concentration in the range of 0.1-15at.% were prepared by one-step flame spray synthesis. Effect of niobium doping on structural, optical and photocatalytic properties of titanium dioxide nanopowders was studied. Morphology and structure were investigated by means of Brunauer-Emmett-Teller isotherm, X-ray diffraction and transmission electron microscopy. Diffuse reflectance and the resulting band gap energy were determined by diffuse reflectance spectroscopy. Photocatalytic activity of the investigated nanopowders was revised for the photodecomposition of methylene blue (MB), methyl orange (MO) and 4-chlorophenol under UVA and VIS light irradiation. Commercial TiO2-P25 nanopowder was used as a reference. The specific surface area of the powders was ranging from 42.9m2/g for TiO2:0.1at.% Nb to 90.0m2/g for TiO2:15at.% Nb. TiO2:Nb particles were nanosized, spherically shaped and polycrystalline. Anatase was the predominant phase in all samples. The anatase-related transition was at 3.31eV and rutile-related one at 3.14eV. TiO2:Nb nanopowders exhibited additional absorption in the visible range. In comparison to TiO2-P25, improved photocatalytic activity of TiO2:Nb was observed for the degradation of MB and MO under both UVA and VIS irradiation, where low doping level (Nb < 1at.%) was the most effective. Niobium doping affected structural, optical and photocatalytic properties of TiO2. Low dopant level enhanced photocatalytic performance under UVA and VIS irradiation. Therefore, TiO2:Nb (Nb < 1at.%) can be proposed as an efficient selective solar light photocatalys

Control of arms of au stars size and its dependent cytotoxicity and photosensitizer effects in photothermal anticancer therapy

Gold nanostars (AuS NPs) are a very attractive nanomaterial, which is characterized by high effective transduction of the electromagnetic radiation into heat energy. Therefore, AuS NPs can be used as photosensitizers in photothermal therapy (PTT). However, understanding the photothermal conversion efficiency in nanostars is very important to select the most appropriate shape and size of AuS NPs. Therefore, in this article, the synthesis of AuS NPs with different lengths of star arms for potential application in PTT was investigated. Moreover, the formation mechanism of these AuS NPs depending on the reducer concentration is proposed. Transmission electron microscopy (TEM) with selected area diffraction (SEAD) and X-ray diffraction (X-Ray) showed that all the obtained AuS NPs are crystalline and have cores with similar values of the diagonal (parameter d), from 140 nm to 146 nm. However, the widths of the star arm edges (parameter c) and the lengths of the arms (parameter a) vary between 3.75 nm and 193 nm for AuS1 NPs to 6.25 nm and 356 nm for AuS4 NPs. Ultraviolet-visible (UV-Vis) spectra revealed that, with increasing edge widths and lengths of the star arms, the surface plasmon resonance (SPR) peak is shifted to the higher wavelengths, from 640 nm for AuS1 NPs to 770 nm for AuS4 NPs. Moreover, the increase of temperature in the AuS NPs solutions as well as the values of calculated photothermal efficiency grew with the elongation of the star arms. The potential application of AuS NPs in the PTT showed that the highest decrease of viability, around 75%, of cells cultured with AuS NPs and irradiated by lasers was noticed for AuS4 NPs with the longest arms, while the smallest changes were visible for gold nanostars with the shortest arms. The present study shows that photothermal properties of AuS NPs depend on edge widths and lengths of the star arms and the values of photothermal efficiency are higher with the increase of the arm lengths, which is correlated with the reducer concentration

INFLUENCE OF DOUBLE SOLUTION TREATMENT ON HARDNESS IN 17-4 PH STEEL

The investigated material is a corrosion-resistant, Cu precipitation hardened steel 17-4PH, which undergoes a macroscopic contraction, as a result of applying the following heat treatment: double solution treatment at 1028°C for 1 h (condition A), ageing at 540°C for 4 h (condition H1025). The second solution treatment at 1028°C was found to eliminate the retained austenite, being the evidence of a completely finished martensitic transformation.Indeed, the only phase identified in all samples was fcc lath martensite exhibiting a parallel striped structure. Unfortunately, this additional heat-treatment operation leads likewise to significant and irregular grain growth, which consequently causes a drop in material hardness. Moreover, the second solution annealing, caused a shift in the XRD peaks to higher 2θ angles, resulting from a lattice parameter decrease by0,25%. The two subsequent heat-treatment procedures bring the lattice parameter back to its initial value. This seemingly reversible process of decrease and increase of the lattice parameter was observed for samples subjected to all the heat treatment operations, strongly suggesting the existence of a relation between the microstructural changes and the macroscopic contraction of the steel material. In addition to the martensitic phase, in the unaged samples, a δ- ferrite phase could be identified by TEM and electron diffraction, which is favorable for ductility and toughness of the material. In all samples, non-coherent fcc-NbC precipitates identified by electron diffraction and EDX mapping having sizes up to 70 nm were found

INFLUENCE OF DOUBLE SOLUTION TREATMENT ON HARDNESS IN 17-4 PH STEEL

The investigated material is a corrosion-resistant, Cu precipitation hardened steel 17-4PH, which undergoes a macroscopic contraction, as a result of applying the following heat treatment: double solution treatment at 1028°C for 1 h (condition A), ageing at 540°C for 4 h (condition H1025). The second solution treatment at 1028°C was found to eliminate the retained austenite, being the evidence of a completely finished martensitic transformation.Indeed, the only phase identified in all samples was fcc lath martensite exhibiting a parallel striped structure. Unfortunately, this additional heat-treatment operation leads likewise to significant and irregular grain growth, which consequently causes a drop in material hardness. Moreover, the second solution annealing, caused a shift in the XRD peaks to higher 2θ angles, resulting from a lattice parameter decrease by0,25%. The two subsequent heat-treatment procedures bring the lattice parameter back to its initial value. This seemingly reversible process of decrease and increase of the lattice parameter was observed for samples subjected to all the heat treatment operations, strongly suggesting the existence of a relation between the microstructural changes and the macroscopic contraction of the steel material. In addition to the martensitic phase, in the unaged samples, a δ- ferrite phase could be identified by TEM and electron diffraction, which is favorable for ductility and toughness of the material. In all samples, non-coherent fcc-NbC precipitates identified by electron diffraction and EDX mapping having sizes up to 70 nm were found

Raising the COx Methanation Activity of a Ru/γ-Al2O3 Catalyst by Activated Modification of Metal–Support Interactions

Ru/Al2O3 is a highly stable, but less active catalyst for methanation reactions. Herein we report an effective approach to significantly improve its performance in the methanation of CO2/H2 mixtures. Highly active and stable Ru/γ-Al2O3 catalysts were prepared by high-temperature treatment in the reductive reaction gas. Operando/in situ spectroscopy and STEM imaging reveals that the strongly improved activity, by factors of 5 and 14 for CO and CO2 methanation, is accompanied by a flattening of the Ru nanoparticles and the formation of highly basic hydroxylated alumina sites. We propose a modification of the metal–support interactions (MSIs) as the origin of the increased activity, caused by modification of the Al2O3 surface in the reductive atmosphere and an increased thermal mobility of the Ru nanoparticles, allowing their transfer to modified surface sites

Fe3O4@SiO2@Au nanoparticles for MRI-guidedchemo/NIR photothermal therapy of cancer cells

Novel functionalized (biofunctionalization followed by cisplatin immobilization) Fe3O4@SiO2@Au nanoparticles (NPs) were designed. The encapsulation of Fe3O4 cores inside continuous SiO2 shells preserves their initial structure and strong magnetic properties, while the shell surface can be decorated by small Au NPs, and then cisplatin (cPt) can be successfully immobilized on their surface. The fabricated NPs exhibit very strong T2 contrasting properties for magnetic resonance imaging (MRI). The functionalized Fe3O4@SiO2@Au NPs are tested for a potential application in photothermal cancer therapy, which is simulated by irradiation of two colon cancer cell lines (SW480 and SW620) with a laser (λ = 808 nm, W = 100 mW cm−2). It is found that the functionalized NPs possess low toxicity towards cancer cells (∼10–15%), which however could be drastically increased by laser irradiation, leading to a mortality of the cells of ∼43–50%. This increase of the cytotoxic properties of the Fe3O4@SiO2@Au NPs, due to the synergic effect between the presence of cPt plus Au NPs and laser irradiation, makes these NPs perspective agents for potential (MRI)-guided stimulated chemo-photothermal treatment of cancer