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

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

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

Aktivierte Modifikation der Träger‐Metall‐Wechselwirkungen als Schlüssel für hochaktive Ru/γ‐Al2O3‐Katalysatoren für die COx‐Methanisierung

Ru/Al2O3 ist ein außerordentlich stabiler, aber weniger aktiver Katalysator für Methanisierungs-Reaktionen. Hier berichten wir über einen neuartigen Ansatz, mit dem die Aktivität dieser Katalysatoren bei der Methanisierung von CO2 in CO2/H2-Gemischen erheblich gesteigert werden kann. Hochaktive und -stabile Ru/γ-Al2O3-Katalysatoren wurden über eine Hochtemperatur-Behandlung im reduktiven Reaktionsgasgemisch erhalten. Operando/In-situ-Spektroskopie und Rastertransmissionselektronenmikroskopie (STEM)-Abbildungen zeigen, dass die deutlich erhöhte Aktivität für die Methanisierung von CO bzw. CO2 mit einer Abflachung der Ru-Nanopartikel und der Bildung von stark basischen Plätzen auf dem hydroxylierten Aluminiumoxid einhergeht. Die erhöhte Aktivität der Katalysatoren um Faktoren von 5 (CO) bzw. 14 (CO2) führen wir auf eine aktivierte Modifikation der Träger-Metall-Wechselwirkungen zurück, die durch eine reaktive Modifizierung der Al2O3-Oberfläche im Reaktionsgas und eine erhöhte thermische Mobilität der Ru-Nanopartikel verursacht wird.Projekt DEALHorizon 2020 EC ProgrammDES

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.Projekt DEA