scholarly journals Synthesis of nickel/gallium nanoalloys using a dual-source approach in 1-alkyl-3-methylimidazole ionic liquids

2019 ◽  
Vol 10 ◽  
pp. 1754-1767
Author(s):  
Ilka Simon ◽  
Julius Hornung ◽  
Juri Barthel ◽  
Jörg Thomas ◽  
Maik Finze ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Dual Source ◽  
Induced Decomposition

NiGa is a catalyst for the semihydrogenation of alkynes. Here we show the influence of different dispersion times before microwave-induced decomposition of the precursors on the phase purity, as well as the influence of the time of microwave-induced decomposition on the crystallinity of the NiGa nanoparticles. Microwave-induced co-decomposition of all-hydrocarbon precursors [Ni(COD)2] (COD = 1,5-cyclooctadiene) and GaCp* (Cp* = pentamethylcyclopentadienyl) in the ionic liquid [BMIm][NTf2] selectively yields small intermetallic Ni/Ga nanocrystals of 5 ± 1 nm as derived from transmission electron microscopy (TEM) and high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) and supported by energy-dispersive X-ray spectrometry (EDX), selected-area energy diffraction (SAED) and X-ray photoelectron spectroscopy (XPS). NiGa@[BMIm][NTf2] catalyze the semihydrogenation of 4-octyne to 4-octene with 100% selectivity towards (E)-4-octene over five runs, but with poor conversion values. IL-free, precipitated NiGa nanoparticles achieve conversion values of over 90% and selectivity of 100% towards alkene over three runs.

scholarly journals (Al,Mg)3La: a new phase in the Mg–Al–La system

2018 ◽  
Vol 74 (4) ◽  
pp. 370-375 ◽  
Author(s):  
Charlotte Wong ◽  
Mark J. Styles ◽  
Suming Zhu ◽  
Dong Qiu ◽  
Stuart D. McDonald ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Powder Diffraction ◽  
Dark Field ◽  
Transmission Electron Microscopy Analysis ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field ◽  
Electron Microscopy Analysis

During an investigation of the Mg-rich end of the Mg–Al–La system, a new ternary phase with the composition of (Al,Mg)3La was identified. The crystal structure of this phase was determined by conventional X-ray powder diffraction and transmission electron microscopy analysis and refined using high-resolution X-ray powder diffraction. The (Al,Mg)3La phase is found to have an orthorhombic structure with a space group of C2221 and lattice parameters of a = 4.3365 (1) Å, b = 18.8674 (4) Å and c = 4.4242 (1) Å, which is distinctly different from the binary Al3La phase (P63/mmc). The resolved structure of the (Al,Mg)3La phase is further verified by high-angle annular dark-field scanning transmission electron microscopy.

Atomic-scale structural and compositional analyses of Ruddlesden-Popper planar faults in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics

2009 ◽  
Vol 24 (8) ◽  
pp. 2596-2604 ◽  
Author(s):  
Sašo Šturm ◽  
Makoto Shiojiri ◽  
Miran Čeh
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Dark Field ◽  
Atomic Scale ◽  
Transmission Electron ◽  
Initial Stage ◽  
Final Microstructure ◽  
Scanning Transmission ◽  
The Matrix ◽  
Annular Dark Field

The microstructure in AO-excess SrTiO3 (A = Sr2+, Ca2+, Ba2+) ceramics is strongly affected by the formation of Ruddlesden-Popper fault–rich (RP fault) lamellae, which are coherently intergrown with the matrix of the perovskite grains. We studied the structure and chemistry of RP faults by applying quantitative high-resolution transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy analyses. We showed that the Sr2+ and Ca2+ dopant ions form RP faults during the initial stage of sintering. The final microstructure showed preferentially grown RP fault lamellae embedded in the central part of the anisotropic perovskite grains. In contrast, the dopant Ba2+ ions preferably substituted for Sr2+ in the SrTiO3 matrix by forming a BaxSr1−xTiO3 solid solution. The surplus of Sr2+ ions was compensated structurally in the later stages of sintering by the formation of SrO-rich RP faults. The resulting microstructure showed RP fault lamellae located at the surface of equiaxed BaxSr1-xTiO3 perovskite grains.

scholarly journals Ru Catalyst Encapsulated into the Pores of MIL-101 MOF: Direct Visualization by TEM

Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4531
Author(s):  
Maria Meledina ◽  
Geert Watson ◽  
Alexander Meledin ◽  
Pascal Van Der Voort ◽  
Joachim Mayer ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Scanning Transmission Electron Microscopy ◽  
Dark Field ◽  
Catalyst Nanoparticles ◽  
Ru Catalyst ◽  
Ru Nanoparticles ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field

Ru catalyst nanoparticles were encapsulated into the pores of a Cr-based metal-organic framework (MOF)—MIL-101. The obtained material, as well as the non-loaded MIL-101, were investigated down to the atomic scale by annular dark-field scanning transmission electron microscopy using low dose conditions and fast image acquisition. The results directly show that the used wet chemistry loading approach is well-fitted for the accurate embedding of the individual catalyst nanoparticles into the cages of the MIL-101. The MIL-101 host material remains crystalline after the loading procedure, and the encapsulated Ru nanoparticles have a metallic nature. Annular dark field scanning transmission electron microscopy, combined with EDX mapping, is a perfect tool to directly characterize both the embedded nanoparticles and the loaded nanoscale MOFs. The resulting nanostructure of the material is promising because the Ru nanoparticles hosted in the MIL-101 pores are prevented from agglomeration—the stability and lifetime of the catalyst could be improved.

A further investigation of the complex M3 murataite structure using Hf substitution and STEM-EELS techniques

2019 ◽  
Vol 75 (3) ◽  
pp. 442-448
Author(s):  
Ryosuke S. S. Maki ◽  
Peter E. D. Morgan
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Radioactive Waste ◽  
Scanning Transmission Electron Microscopy ◽  
Dark Field ◽  
Site Preference ◽  
Scanning Transmission Electron ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Annular Dark Field

Many members of the complex crystalline fluorite supercell structures (e.g. zirconolite, pyrochlore and murataite polytypes) have been considered/studied for possible long-term radioactive-waste immobilization. The eight-coordinated sites in these crystals are of particular importance because they are preferred for the accommodation of trivalent rare earths and actinides present in radioactive waste from fuel element processing. The fluorite-type supercell structures include the murataites, M3, M5, M7, M8, having those numbers of repeating fluorite sub-cell units. One simple technique, as shown here, namely the substitution of Hf into the Zr site, is very helpful for structural analysis in these very complex cases in order to further illuminate the site preference of the Zr ion. Three M3 murataite samples, Ca-Mn-Ti-Zr-Al-Fe-O (regular M3), Ca-Ti-Zr-Al-Fe-O (Mn-free M3) and Ca-Mn-Ti-Hf-Al-Fe-O (Hf-substituted M3) are investigated and, through techniques described for larger cells, show that the Zr is very likely not to be hosted in the [6] Ti site in the M3 murataite structure, as suggested by Pakhomova et al. [(2013), Z. Kristallogr. Cryst. Mater. 228, 151–156], but more likely replaces the [8] Ca1 site and less likely the [8] Ca2 site. This adjusted site preference for each cation from the powder X-ray diffraction (PXRD) and scanning transmission electron microscopy electron energy-loss spectroscopy (STEM-EELS) methods, agrees well with the high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) image.

scholarly journals Heterogeneous Fenton-like oxidation of p-hydroxybenzoic acid using Fe/CeO2-TiO2 catalyst

2019 ◽  
Vol 79 (7) ◽  
pp. 1276-1286 ◽  
Author(s):  
Tijani Hammedi ◽  
Mohamed Triki ◽  
Mayra G. Alvarez ◽  
Jordi Llorca ◽  
Abdelhamid Ghorbel ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
Catalytic Properties ◽  
Molar Ratio ◽  
Hydroxybenzoic Acid ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Temperature Programmed

Abstract This paper is built on the Fenton-like oxidation of p-hydroxybenzoic acid (p–HBZ) in the presence of H2O2 and 3%Fe supported on CeO2-TiO2 aerogels under mild conditions. These catalysts were deeply characterized by X-ray diffraction (XRD), hydrogen temperature programmed reduction (H2-TPR), transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM) and X-ray photoelectron spectroscopy (XPS). The effect of thermal treatment, pH (2–3, 5, 7), H2O2/p–HBZ molar ratio (5, 15, 20, 25) and reaction temperature (25 °C, 40 °C and 60 °C) on the catalytic properties of supported Fe catalysts are studied. Our results highlight the role of CeO2 and the calcination of the catalyst to obtain the highest catalytic properties after 10 min: 73% of p–HBZ conversion and 52% of total organic carbon (TOC) abatement.

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