Structural and Chemical Characterization of Yb2O3-ZrO2 System by HAADF-STEM and HRTEM

2009 ◽  
Vol 15 (1) ◽  
pp. 46-53 ◽  
Author(s):  
C. Angeles-Chavez ◽  
P. Salas ◽  
L.A. Díaz-Torres ◽  
E. de la Rosa ◽  
R. Esparza ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Crystalline Structure ◽  
Sol Gel ◽  
Tetragonal Zirconia ◽  
Chemical Characterization ◽  
Dark Field ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractZrO2:Yb3+ nanocrystalline phosphors with high concentrations of ytterbium ions were prepared using the sol-gel method. X-ray diffraction, high-angle annular-dark-field scanning transmission electron microscopy (HAADF-STEM), energy dispersive X-ray spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to characterize the nanocrystalline phosphors annealed at 1000°C. Unit-cell distortion and changes in the crystalline structure of the monoclinic zirconia to tetragonal zirconia, and subsequently cubic zirconia, were observed with increased Yb concentration. Yb ions were randomly distributed into the lattice of the crystalline structure. No segregation of Yb2O3 phase was observed. The substitution of Zr atoms by Yb atoms on different crystalline phases was confirmed by the experimental results and theoretical simulations of HRTEM and HAADF-STEM.

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.

scholarly journals Obtaining and Characterization of TiO2-GO Composites for Photocatalytic Applications

2020 ◽  
Vol 2020 ◽  
pp. 1-9 ◽  
Author(s):  
D. K. Calvo Ramos ◽  
M. Vega González ◽  
R. A. Esparza Muñóz ◽  
J. Santos Cruz ◽  
F. J. De Moure-Flores ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Uv Radiation ◽  
Uv Light ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

Titanium dioxide (TD) and graphene oxide (GO) were synthesized by sol-gel and improved Hummers method, respectively. This study shows the results of the incorporation through four different conditions (sol-gel, sol-gel and ultrasonic, annealed, and UV radiation, C1 to C4, respectively). It was observed that a homogeneous incorporation of TD on sheets of GO was obtained satisfactorily. The composites of TiO2/GO were characterized using different techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), energy dispersive X-ray spectroscopy (EDS), Raman spectroscopy, and infrared spectroscopy (IR). The photocatalytic activity of the composites was determined from the degradation of the dye azo tartrazine using UV and solar radiation. The best incorporation of TD nanoparticles on GO was obtained with condition C3 (thermal incorporation method) at a temperature of 65°C. This shows a uniformity in the size and shape of the TD as well as an excellent adherence to the sheet of GO. This addition is accomplished by ionic bonding in the presence of electrostatic Coulomb forces. The C3 composite degraded the tartrazine dye using UV radiation and sunlight. With the latter, the degradation time was three times faster than using UV light.

Magnesium and sulfur in mast cell and basophil granules of lower vertebrates in relation with histamine

1992 ◽  
Vol 50 (2) ◽  
pp. 1596-1597
Author(s):  
Kenichi Takaya
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Mast Cell ◽  
Mast Cells ◽  
Tree Frog ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Fresh Frozen ◽  
Ultrathin Sections

Mast cell and basophil granules of the vertebrate contain heparin or related sulfated proteoglycans. Histamine is also present in mammalian mast cells and basophils. However, no histamine is detected in mast cell granules of the amphibian or fish, while it is shown in those of reptiles and birds A quantitative x-ray microanalysis of mast cell granules of fresh frozen dried ultrathin sections of the tongue of Wistar rats and tree frogs disclosed high concentrations of sulfur in rat mast cell granules and those of sulfur and magnesium in the tree frog granules. Their concentrations in tree frog mast cell granules were closely correlated (r=0.94).Fresh frozen dried ultrathin sections and fresh air-dried prints of the tree frog tongue and spleen and young red-eared turtle (ca. 6 g) spleen and heart blood were examined by a quantitative energy-dispersive x-ray microanalysis (X-650, Kevex-7000) for the element constituents of the granules of mast cells and basophils. The specimens were observed by transmission electron microscopy (TEM) (80-200 kV) and followed by scanning transmission electron microscopy (STEM) under an analytical electron microscope (X-650) at an acceleration voltage of 40 kV and a specimen current of 0.2 nA. A spot analysis was performed in a STEM mode for 100 s at a specimen current of 2 nA on the mast cell and basophil granules and other areas of the cells. Histamine was examined by the o-phthalaldehyde method.

scholarly journals Revisiting the Bøggild Intergrowth in Iridescent Labradorite Feldspars: Ordering, Kinetics, and Phase Equilibria

Minerals ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 727
Author(s):  
Shiyun Jin ◽  
Huifang Xu ◽  
Seungyeol Lee
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Atom Probe ◽  
Phase Region ◽  
Two Phase ◽  
Subsolidus Phase ◽  
Plagioclase Feldspar ◽  
X Ray ◽  
Transmission Electron ◽  
Scanning Transmission

The enigmatic Bøggild intergrowth in iridescent labradorite crystals was revisited in light of recent work on the incommensurately modulated structures in the intermediated plagioclase. Five igneous samples and one metamorphic labradorite sample with various compositions and lamellar thicknesses were studied in this paper. The lamellar textures were characterized with conventional transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM). The compositions of individual lamellae were analyzed with high-resolution energy-dispersive X-ray spectroscopy (EDS) mapping and atom probe tomography (APT). The average structure states of the studied samples were also compared with single-crystal X-ray diffraction data (SC-XRD). The Na-rich lamellae have a composition of An44–48, and the Ca-rich lamellae range from An56 to An63. Significant differences between the lamellar compositions of different samples were observed. The compositions of the Bøggild intergrowth do not only depend on the bulk compositions, but also on the thermal history of the host rock. The implications on the subsolidus phase relationships of the plagioclase feldspar solid solution are discussed. The results cannot be explained by a regular symmetrical solvus such as the Bøggild gap, but they support an inclined two-phase region that closes at low temperature.

Intergrowth of niobium tungsten oxides of the tetragonal tungsten bronze type

2020 ◽  
Vol 75 (11) ◽  
pp. 913-919
Author(s):  
Frank Krumeich
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Tungsten Bronze ◽  
Structural Complexity ◽  
Dark Field ◽  
Tetragonal Tungsten Bronze ◽  
Tungsten Oxides ◽  
Transmission Electron ◽  
Scanning Transmission

AbstractSince the 1970s, high-resolution transmission electron microscopy (HRTEM) is well established as the most appropriate method to explore the structural complexity of niobium tungsten oxides. Today, scanning transmission electron microscopy (STEM) represents an important alternative for performing the structural characterization of such oxides. STEM images recorded with a high-angle annular dark field (HAADF) detector provide not only information about the cation positions but also about the distribution of niobium and tungsten as the intensity is directly correlated to the local scattering potential. The applicability of this method is demonstrated here for the characterization of the real structure of Nb7W10O47.5. This sample contains well-ordered domains of Nb8W9O47 and Nb4W7O31 besides little ordered areas according to HRTEM results. Structural models for Nb4W7O31 and twinning occurring in this phase have been derived from the interpretation of HAADF-STEM images. A remarkable grain boundary between well-ordered domains of Nb4W7O31 and Nb8W9O47 has been found that contains one-dimensionally periodic features. Furthermore, short-range order observed in less ordered areas could be attributed to an intimate intergrowth of small sections of different tetragonal tungsten bronze (TTB) based structures.

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.

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