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In this study Fe2O3/SBA-15 catalyst was synthesized via direct synthesis method under acidic conditions using triblock copolymer Pluronic P123 as template, tetraethyl orthosilicate as a silica source and Fe (NO3)3∙9H2O as iron source. Template was removed using extraction and calcination. The obtained catalyst was characterized using XRD analysis, WDXRF spectroscopy, N2 adsorption-desorption analysis and STEM–EDX measurements. Results of catalyst characterization showed that the synthesized Fe2O3/SBA-15 is mesoporous silica with 2D p6mm hexagonal mesostructure loaded with 15.6 wt.% Fe2O3. Average pore size was 6.95 nm, homogeneous immobilized Fe2O3 nanoparticles do not disrupt the porous hexagonal structure of the support.

The microstructure of a René 108 Ni-based superalloy was systematically investigated by X-ray diffraction, light microscopy, energy-dispersive X-ray spectroscopy, and electron microscopy techniques. The material was investment cast in a vacuum and then solution treated (1200 °C-2h) and aged (900 °C-8h). The γ matrix is mainly strengthened by the ordered L12 γ′ phase, with the mean γ/γ′ misfit, δ, +0.6%. The typical dendritic microstructure with considerable microsegregation of the alloying elements is revealed. Dendritic regions consist of secondary and tertiary γ′ precipitates. At the interface of the matrix with secondary γ′ precipitates, nano M5B3 borides are present. In the interdendritic spaces additionally primary γ′ precipitates, MC and nano M23C6 carbides were detected. The γ′ precipitates are enriched in Al, Ta, Ti, and Hf, while channels of the matrix in Cr and Co. The highest summary concentration of γ′-formers occurs in coarse γ′ surrounding MC carbides. Borides M5B3 contain mostly W, Cr and Mo. All of MC carbides are enriched strongly in Hf and Ta, with the concentration relationship between these and other strong carbide formers depending on the precipitate’s morphology. The nano M23C6 carbides enriched in Cr have been formed as a consequence of phase transformation MC + γ → M23C6 + γ′ during the ageing treatment.

Structural defects such as voids and compositional inhomogeneities may affect the performance of Cu(In,Ga)Se 2 (CIGS) solar cells. We analyzed the morphology and elemental distributions in co-evaporated CIGS thin films at the different stages of the CIGS growth by energy-dispersive x-ray spectroscopy in a transmission electron microscope. Accumulation of Cu-Se phases was found at crevices and at grain boundaries after the Cu-rich intermediate stage of the CIGS deposition sequence. It was found, that voids are caused by Cu out-diffusion from crevices and GBs during the final deposition stage. The Cu inhomogeneities lead to non-uniform diffusivities of In and Ga, resulting in lateral inhomogeneities of the In and Ga distribution. Two and three-dimensional simulations were used to investigate the impact of the inhomogeneities and voids on the solar cell performance. A significant impact of voids was found, indicating that the unpassivated voids reduce the open-circuit voltage and fill factor due to the introduction of free surfaces with high recombination velocities close to the CIGS/CdS junction. We thus suggest that voids, and possibly inhomogeneities, limit the efficiency of solar cells based on three-stage co-evaporated CIGS thin films. Passivation of the voids' internal surface may reduce their detrimental effects.

The replacement of noble metal catalysts by abundant iron as an active compound in CO oxidation is of ecologic and economic interest. However, improvement of their catalytic performance to the same level as state-of-the-art noble metal catalysts requires an in depth understanding of their working principle on an atomic level. As a contribution to this aim, a series of iron oxide catalysts with varying Fe loadings from 1 to 20 wt% immobilized on a γ-Al2O3 support is presented here, and a multidimensional structure–activity correlation is established. The CO oxidation activity is correlated to structural details obtained by various spectroscopic, diffraction, and microscopic methods, such as PXRD, PDF analysis, DRUVS, Mössbauer spectroscopy, STEM-EDX, and XAS. Low Fe loadings lead to less agglomerated but high percentual amounts of isolated, tetrahedrally coordinated iron oxide species, while the absolute amount of isolated species reaches its maximum at high Fe loadings. Consequently, the highest CO oxidation activity in terms of turnover frequencies can be correlated to small, finely dispersed iron oxide species with a large amount of tetrahedrally oxygen coordinated iron sites, while the overall amount of isolated iron oxide species correlates with a lower light-off temperature.

This study focuses on NMC 811 (LiNi0.8Mn0.1Co0.1O2), a promising material for high-capacity batteries, and investigates the challenges associated with its use, specifically the formation of the cathode electrolyte interphase (CEI) layer due to chemical reactions. This layer is a consequence of the position of the Lowest Unoccupied Molecular Orbital (LUMO) energy level of NMC 811 that is close to the Highest Occupied Molecular Orbital (HOMO) level of liquid electrolytes, resulting in electrolyte oxidation and cathode surface alterations during charging. A stable CEI layer can mitigate further degradation by reducing the interaction between the reactive cathode material and the electrolyte. Our research analyzed the CEI layer on NMC 811 using advanced techniques, such as 4D-STEM ACOM (automated crystal orientation mapping) and STEM-EDX, focusing on the effects of different charging voltages (4.3 V and 4.5 V). The findings revealed varying degrees of degradation and the formation of a fluorine-rich layer on the secondary particles. Detailed analysis showed that the composition of this layer differed based on the voltage: only LiF at 4.5 V and a combination of lithium fluoride (LiF) and lithium hydroxide (LiOH) at 4.3 V. Despite LiF’s known stability as a CEI protective layer, our observations indicate that it does not effectively prevent degradation in NMC 811. The study concluded that impurities and unwanted chemical reactions leading to suboptimal CEI formation are inevitable. Therefore, future efforts should focus on developing protective strategies for NMC 811, such as the use of specific additives or coatings.

High-entropy alloy nanoparticles (HEA NPs) represent a promising material class with significant potential in various applications, such as heterogeneous catalysis or magnetic devices. This is due to their exceptional compositional tunability arising from the synergistic interplay of multiple elements within a single particle. While laser-synthesized, surfactant-free colloidal HEA NPs have already been reported, the underlying formation mechanism remains unknown, particularly the underexplored preference of amorphous over crystalline structures warrants further investigation. Herein, we present a systematic study of laser-generated equimolar CrMnFeCoNi nanoparticles, focusing on structural differences, arising from varying pulse durations during synthesis in organic solvents (acetone, ethanol, acetonitrile). In a systematic experimental series using high-resolution transmission electron microscopy, scanning transmission electron microscopy with energy-dispersive X-ray spectroscopy, selected-area electron diffraction, X-ray diffraction, electron energy loss spectroscopy, in situ heating, post-irradiation experiments, and differential scanning calorimetry we demonstrate that a pulse-duration-driven structural difference occurs during laser ablation in liquid is observable to the three utilized solvents. While picosecond-pulsed laser ablation in liquid produces polycrystalline HEA NPs, nanosecond-pulsed laser ablation favors a metastable amorphous structure. Particle cores in all cases exhibit a homogeneous distribution of the metals Cr, Mn, Fe, Co, and Ni, while particle shells were found to vary between manganese-enriched oxide layers and thin graphitic carbon coatings. The discovery of the structure-directing mechanism allows one to select between crystalline or amorphous HEA NP products, simply by choice of the laser pulse duration in the same, well-scalable setup, giving access to colloidal particles that can be further downstream processed to heterogeneous catalysts or magnets. In that context, the outstanding temperature stability up to 375 °C (differential scanning calorimetry) or 500 °C (transmission electron microscopy) may motivate future application-relevant work.

PdRe/Al2O3 catalysts are highly selective for hydrogenation of furfural to furfuryl alcohol (FAL). Moreover, the synergy between the metals can result in greater specific activity (higher turnover frequency, TOF) than exhibited by either metal alone. Bimetallic catalyst structure depends strongly on the metal precursors employed and their addition sequence to the support. In this work, PdRe/Al2O3 catalysts were prepared by: (i) co-impregnation (CI) and sequential impregnation (SI) of γ-Al2O3 using HReO4 and Pd(NO3)2, (ii) SI using NH4ReO4 and [Pd(NH3)4(NO3)2], (iii) HReO4 addition to a reduced and passivated Pd/Al2O3 catalyst, and (iv) impregnation with the double complex salt (DCS), [Pd(NH3)4(ReO4)2]. Raman spectroscopy and temperature-programmed reduction (TPR) evidence larger supported PdO crystallites in catalysts prepared using Pd(NO3)2 than [Pd(NH3)4(NO3)2]. Surface [ReO4]− species detected by Raman exhibit TPR peak temperatures from ranging 85 to 260 °C (versus 375 °C for Re/Al2O3). After H2 reduction at 400 °C, the catalysts were characterized by chemisorption, temperature-programmed hydride decomposition (TPHD), CO diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), and scanning transmission electron microscopy (STEM) with energy-dispersive x-ray (EDX) spectroscopy. The CI catalyst containing supported Pd–Re alloy crystallites had a TOF similar to Pd/Al2O3 but higher (61%) FAL selectivity. In contrast, catalysts prepared by methods (ii–iv) containing supported Pd-Re nanoparticles exhibit higher TOFs and up to 78% FAL selectivity.