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Aza-enamines X - Formylation of Pyrazole-4-carbaldehyde Hydrazones at the Hydrazonoazomethine C-Atom
(2003)
1,3-Disubstituted 1H-pyrazole-4-carbaldehyde-N,N-dimethylhydrazones 1 reacted with the Vilsmeier-Haackreagent, corresponding to the aza-enamine concept, in an electrophilicsubstitution reaction at the azomethine C-atom yielding the 1,4,5-triaza-pentadieniumsalts 2. These were hydrolysed to give2-hydrazono-2-(1H-pyrazole-4-yl)ethanals 3. The electrophilic attack did not takeplace at the vinylogous position 5' of the pyrazoles.
Quantification of nanoparticle (NP) uptake in cells or tissues is very important for safety assessment. Often, electron microscopy based approaches are used for this purpose, which allow imaging at very high resolution. However, precise quantification of NP numbers in cells and tissues remains challenging. The aim of this study was to present a novel approach, that combines precise quantification of NPs in individual cells together with high resolution imaging of their intracellular distribution based on focused ion beam/ scanning electron microscopy (FIB/SEM) slice and view approaches.
CrOx/La2O3 mixed oxides, prepared by impregnating La2O3 with appropriate aqueous solutions of (NH4)2CrO4 and calcining at 600 °C for 4 h, have been investigated by means of XRD, TPR, XPS, DRIFTS, and Raman spectroscopy (RS). The formation of the compounds La2CrO6, La(OH)CrO4 and LaCrO4 under these conditions was evidenced. Strong peaks at 864, 884, 913, and 921 cm-1, as well as weak peaks at 136, 180, 354, 370, and 388 cm-1 in the RS spectrum of CrOx/La2O3 have been assigned to La2CrO6.
The present work describes the combination of electrochemical investigations by using a gel‐type electrolyte with Fourier‐transformed infrared spectroscopy to investigate partially extremely thin corrosion product films on titanium‐zinc. The gel pad method enables the determination of corrosion relevant parameters such as the potential and the linear polarization resistance without altering the corrosion product layers, which are extremely prone to re‐dissolution when freshly formed. Complementary infrared spectroscopy enables the determination of main compounds of even very thin surface layers of few tenth of nanometers with a certain lateral resolution. It was found that zinc forms mostly zinc carboxy‐hydroxides such as hydrozincite, under various exposure conditions. The protective properties of these hydrozincite layers depend on the structure of the corrosion product film rather than on its thickness. In mid‐term exposure tests, shallow corrosion pits were found even in the absence of corrosive agents such as chloride.
27Al nuclear magnetic resonance spectra of polycrystalline aluminium borate 9Al2O3 · 2B2O3 have been measured in double rotation at 11.7 and 7.0 T and high-speed magic-angle spinning at 7.0, 9.4, 11.7, 14.1 and 17.6 T. Spinning sidebands from the satellite transitions were observed at 7.0 and 14.1 T. Each of the four structural aluminium sites [Al(IV), Al(V)(1), Al(V)(2) and Al(VI)] are observed, characterised and assigned in the spectra. The obtained parameter set gives a fully consistent interpretation in agreement with the crystal structure of the compound.
AbstractThe high-temperature corrosion behaviors of the equimolar CrCoNi medium-entropy alloy and CrMnFeCoNi high-entropy alloy were studied in a gas atmosphere consisting of a volumetric mixture of 10% H2O, 2% O2, 0.5% SO2, and 87.5% Ar at 800 °C for up to 96 h. Both alloys were initially single-phase fcc with a mean grain size of ~ 50 μm and a homogeneous chemical composition. The oxide layer thickness of CrMnFeCoNi increased linearly with exposure time while it remained constant at ~ 1 μm for CrCoNi. A Cr2O3 layer and minor amounts of (Co,Ni)Cr2O4 developed on the latter while three oxide layers were detected on the former, i.e., a thin and continuous chromium rich oxide layer at the oxide/alloy interface, a dense (Mn,Cr)3O4 layer in the center and a thick and porous layer of Mn3O4 and MnSO4 at the gas/oxide interface. Additionally, a few metal sulfides were observed in the CrMnFeCoNi matrix. These results were found to be in reasonable agreement with thermodynamic calculations.
High-entropy alloys (HEAs) and compositionally complex alloys (CCAs) represent new classes of materials containing five or more alloying elements (concentration of each element ranging from 5 to 35 at. %). In the present study, HEAs are defined as single-phase solid solutions; CCAs contain at least two phases. The alloy concept of HEAs/CCAs is fundamentally different from most conventional alloys and promises interesting properties for industrial applications (e.g., to overcome the strength-ductility trade-off). To date, little attention has been paid to the weldability of HEAs/CCAs encompassing effects on the welding metallurgy. It remains open whether welding of HEAs/CCAs may lead to the formation of brittle intermetallics and promote elemental segregation at crystalline defects. The effect on the weld joint properties (strength, corrosion resistance) must be investigated. The weld metal and heat-affected zone in conventional alloys are characterized by non-equilibrium microstructural evolutions that most probably occur in HEAs/CCAs. The corresponding weldability has not yet been studied in detail in the literature, and the existing information is not documented in a comprehensive way. Therefore, this study summarizes the most important results on the welding of HEAs/CCAs and their weld joint properties, classified by HEA/CCA type (focused on CoCrFeMnNi and AlxCoCrCuyFeNi system) and welding process.
Selective Catalytic Reduction of Nitric Oxide by Ammonia over Egg-Shell MnOx/NaY Composite Catalysts
(2002)
A novel composite catalyst system for the selective catalytic reduction (SCR) of NOx by NH3 is described operating at temperatures lower than 470 K in the presence of water with NO conversions of 80100% at space velocities of 30,00050,000 h-1. The catalyst is prepared by egg-shell precipitation of MnO2 on the external surface of zeolite NaY. Structural and thermal stability of precipitated MnO2 as well as of the MnO2/NaY composite catalyst were characterized by N2 adsorption, X-ray diffraction, laser Raman spectroscopy, temperature-programmed reduction, and electron microscopy. MnO2 precipitated on zeolite NaY (15 wt% loading) retained its amorphous state up to calcination temperatures of 775 K. The zeolite component remained structurally intact. Calcination at higher temperatures destroyed the zeolite structure and transformed MnO2 into Mn3O4. DRIFT spectroscopic investigations revealed the presence of symmetric O=NON=O species formally corresponding to N2O3 on the composite catalyst after contact with NO. Catalytic measurements under integral flow conditions showed that the catalyst performance is associated with a close coupling of nitrite formation and its drain off from equilibria with NO/NO2 and nitrate by ammonia. Several results are in line with the diazotation mechanism, including NH3 protonation to NH4+, whereas prevailing Lewis acid sites should enable NH3 activation via amide species, thus leading to a parallel amide/nitrosamide SCR reaction route. The activity-temperature profile fulfills the requirements of a low-temperature NOx reduction catalyst for mobile diesel engines if an ammonia supply is implemented on board, e.g., by urea decomposition.
High- and medium-entropy alloys (HEAs) are a quite new class of materials. They have a high potential for applications from low to high temperatures due to the excellent combination of their structural properties.
Concerning their application as components; processing properties, such as machinability, have hardly been investigated so far. Hence, machinability analyses with a focus on the influence of the milling process and its basic parameters (cutting speed, feed per cutting edge) on the resulting surface integrity of specimens from an equiatomic high- (CoCrFeMnNi) and a medium- (CoCrNi) entropy alloy have been carried out. A highly innovative milling process with ultrasonic assistance (USAM) was compared to conventional milling processes.
Recent studies have shown that USAM has a high potential to significantly reduce the mechanical load on the tool and workpiece surface during milling. In this study, the basic machining and ultrasonic parameters were systematically varied. After machining, the surface integrity of the alloys was analyzed in terms of topography, defects, subsurface damage, and residual stresses. It was observed that USAM reduces the cutting forces and increases the surface integrity in terms of lower tensile residual stresses and defect density near the surfaces for the CoCrFeMnNi alloy. It was shown that the cutting forces and the metallurgical influence in the sub surface region are reduced by increasing the cutting speed and reducing the feed rate per cutting edge. With the CoCrNi alloy, the tool revealed severe wear. As a result, for this alloy no influence of the parameters on the machinability could be determined.