Synthesis, thermal evolution and magnetic investigations of SBA-15 silica functionalized with anchored iron phosphonate molecules.

In the current work, we report on the synthesizing of a series of novel nanocomposite materials obtained by functionalizing the SBA-15 silica matrix with anchored iron phosphonate molecules and the following thermal treatment. The obtained results reveal the formation of a unique amorphic layer of Fe-based compounds on the surface of silica walls of SBA-15 channels as a result of the organic groups' decomposition after moderate thermal treatment. Due to their unique structure, represented in an active Fe-containing amorphous coating spread over a large surface area, these materials are of great interest for their potential applications in fields such as catalysis, adsorption, and non-linear optics. The obtained materials remain amorphous, preserving the SBA-15 mesoporous structure up to temperatures of approximately 800 °C, after which the partial melting of the silica backbone is observed with the simultaneous formation of nanocrystals inside the newly-formed glassy mass. All obtained materials were characterized using such techniques as thermogravimetry, transmission and scanning electron microscopy combined with energy dispersive x-ray spectroscopy mapping, Raman spectroscopy, N2sorption analysis, x-ray diffraction, x-ray photoelectron spectroscopy, Mössbauer spectroscopy, and SQUID measurements.

Mechanical Properties and Microstructure of Inconel 718 Lattice Structures Produced by Selective Laser Melting Process.

This article presents the results of an analysis regarding the microstructure, mechanical strength, and microhardness of two kinds of samples built through selective laser melting with Inconel 718, the most frequently used alloy in metal additive manufacturing due to its excellent mechanical properties. The sample geometry was made up of two types of lattice structures with spherical and hyperbolical stiffness elements. The goals of these studies are to determine how homogenization heat treatment influences the microhardness and the mechanical properties of the specimens and to identify the structure with the best mechanical properties. The analysis showed that heat treatment was beneficial because the regular dendritic structure disappears, the δ phase precipitates at the grain boundaries, and both the γ and γ″ phases dissolve. It has also been shown that the structures with hyperbolical stiffness elements have better compressive strength than the structures with the elliptical structures, with a 47.6% increase for the as-fabricated structures and an approximate 50% increase for the heat-treated structure.

Tuning Electrochemical Performance by Microstructural Optimization of the Nanocrystalline Functional Oxygen Electrode Layer for Solid Oxide Cells.

Further development of solid oxide fuel cell (SOFC) oxygen electrodes can be achieved through improvements in oxygen electrode design by microstructure miniaturization alongside nanomaterial implementation. In this work, improved electrochemical performance of an La0.6Sr0.4Co0.2Fe0.8O3-d (LSCF) cathode was achieved by the controlled modification of the La0.6Sr0.4CoO3-d (LSC) nanocrystalline interlayer introduced between a porous oxygen electrode and dense electrolyte. The evaluation was carried out for various LSC layer thicknesses, annealing temperatures, oxygen partial pressures, and temperatures as well as subjected to long-term stability tests and evaluated in typical operating conditions in an intermediate temperature SOFC. Electrochemical impedance spectroscopy and a distribution of relaxation times analysis were performed to reveal the rate-limiting electrochemical processes that limit the overall electrode performance. The main processes with an impact on the electrode performance were the adsorption of gaseous oxygen O2, dissociation of O2, and charge transfer-diffusion (O2-). The introduction of a nanoporous and nanocrystalline interlayer with extended electrochemically active surface area accelerates the oxygen surface exchange kinetics and oxygen ion diffusions, reducing polarization resistances. The polarization resistance of the reference LSCF was lowered by one order of magnitude from 0.77 to 0.076 Ω·cm2 at 600 °C by the deposition of a 400 nm LSC interlayer at the interface. The developed electrode tested in the anode-supported fuel cell configuration showed a higher cell performance by 20% compared to the cell with the reference electrode. The maximum power density at 700 °C reaches 675 and 820 mW·cm-2 for the reference cell and the cell with the LSC interlayer, respectively. Aging tests at 700 °C under a high load of 1 A·cm2 were performed.

Complex Structural Effects in Deformed High-Manganese Steel.

The research presented in this paper is part of a larger project concerning deformation behavior, microstructure and mechanical properties of high-manganese steels with different chemical compositions and processed under various conditions. The current investigation deals with the development of microstructure and crystallographic texture of Fe-21.2Mn-2.73Al-2.99Si steel deformed in tension until fracture at ambient temperature. The deformation process of the examined steel turned out to be complex and included not only dislocation slip and twinning but also strain induced phase transformations (γ → ε) and (γ → α'). The formation of ε-martensite with hexagonal structure was observed within the microstructure of the steel starting from the range of lower strains. With increasing deformation degree, the α'-martensite showing a cubic structure gradually began to form. Attempts have been made to explain the circumstances or conditions for the occurrence of the deformation mechanisms mentioned above and their impact on the mechanical properties. The obtained results indicate that the strength and plastic properties of the steel substantially exceed those of plain carbon steels. Since both, mechanical twinning and the strain-induced phase transformations took place during deformation, it seems that both types of deformation mechanisms contributed to an increase in the mechanical properties of the examined manganese steel.

Multiscale Characterization of an Oxide Scale Formed on the Creep-Resistant ATI 718Plus Superalloy during High-Temperature Oxidation.

The ATI 718Plus® is a creep-resistant nickel-based superalloy exhibiting high strength and excellent oxidation resistance in high temperatures. The present study is focused on multiscale 2D and 3D characterization (morphological and chemical) of the scale and the layer beneath formed on the ATI 718Plus superalloy during oxidation at 850 °C up to 4000 h in dry and wet air. The oxidized samples were characterized using various microscopic methods (SEM, TEM and STEM), energy-dispersive X-ray spectroscopy and electron diffraction. The 3D visualization of the microstructural features was achieved by means of FIB-SEM tomography. When oxidized in dry air, the ATI 718Plus develops a protective, dense Cr2O3 scale with a dual-layered structure. The outer Cr2O3 layer is composed of coarser grains with a columnar shape, while the inner one features fine, equiaxed grains. The Cr2O3 scale formed in wet air is single-layered and features very fine grains. The article discusses the difference between the structure, chemistry and three-dimensional phase distribution of the oxide scales and near-surface areas developed in the two environments. Electron microscopy/spectroscopy findings combined with the three-dimensional reconstruction of the microstructure provide original insight into the role of the oxidation environment on the structure of the ATI 718Plus at the nanoscale.

The Influence of the Electrodeposition Parameters on the Properties of Mn-Co-Based Nanofilms as Anode Materials for Alkaline Electrolysers.

In this work, the influence of the synthesis conditions on the structure, morphology, and electrocatalytic performance for the oxygen evolution reaction (OER) of Mn-Co-based films is studied. For this purpose, Mn-Co nanofilm is electrochemically synthesised in a one-step process on nickel foam in the presence of metal nitrates without any additives. The possible mechanism of the synthesis is proposed. The morphology and structure of the catalysts are studied by various techniques including scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and transmission electron microscopy. The analyses show that the as-deposited catalysts consist mainly of oxides/hydroxides and/or (oxy)hydroxides based on Mn2+, Co2+, and Co3+. The alkaline post-treatment of the film results in the formation of Mn-Co (oxy)hydroxides and crystalline Co(OH)2 with a ß-phase hexagonal platelet-like shape structure, indicating a layered double hydroxide structure, desirable for the OER. Electrochemical studies show that the catalytic performance of Mn-Co was dependent on the concentration of Mn versus Co in the synthesis solution and on the deposition charge. The optimised Mn-Co/Ni foam is characterised by a specific surface area of 10.5 m2·g-1, a pore volume of 0.0042 cm3·g-1, and high electrochemical stability with an overpotential deviation around 330-340 mV at 10 mA·cm-2geo for 70 h.

A bottom-up process of self-formation of highly conductive titanium oxide (TiO) nanowires on reduced SrTiO3.

Reduced titanium oxide structures are regarded as promising materials for various catalytic and optoelectronic applications. There is thus an urgent need for developing methods of controllable formation of crystalline nanostructures with tunable oxygen nonstoichiometry. We introduce the Extremely Low Oxygen Partial Pressure (ELOP) method, employing an oxygen getter in close vicinity to an oxide during thermal reduction under vacuum, as an effective bottom-up method for the production of nanowires arranged in a nanoscale metallic network on a SrTiO3 perovskite surface. We demonstrate that the TiO nanowires crystallize in a highly ordered cubic phase, where single nanowires are aligned along the main crystallographic directions of the SrTiO3 substrate. The dimensions of the nanostructures are easily tunable from single nanometers up to the mesoscopic range by varying the temperature of reduction. The interface between TiO and SrTiO3 (metal and insulator) was found to be atomically sharp providing the unique possibility of the investigation of electronic states, especially since the high conductivity of the TiO nanostructures is maintained after room temperature oxidation. According to the growth model we propose, TiO nanowire formation is possible due to the incongruent sublimation of strontium and crystallographic shearing, triggered by the extremely low oxygen partial pressure (ELOP). The controlled formation of conductive nanowires on a perovskite surface holds technological potential for implementation in memristive devices, organic electronics, or for catalytic applications, and provides insight into the mechanism of nanoscale phase transformations in metal oxides. We believe that the ELOP mechanism of suboxide formation is suitable for the formation of reduced suboxides on other perovskite oxides and for the broader class of transition metal oxides.