Characterization of Antimony-Doped TIN Oxide Catalysts

2001 ◽  
Vol 7 (S2) ◽  
pp. 1094-1095
Author(s):  
K. Sun ◽  
J. Liu ◽  
N.D. Browning

Antimony-doped tin oxide (ATO) catalysts are used for the oxidation of propylene to acrolein, the ammoxidation of propylene to acrylonitrile and the oxidative dehydrogenation of butanes to 1,3- butadiene. The distribution and valence states of Sb in ATOs are key in determining their catalytic activities. While these materials have been subjects of intensive studies for more than 20 years, X-ray photoelectron spectroscopy, Mössbauer spectrometry, and X-ray absorption spectroscopy4 have so far provided only indirect data for the distribution of Sb and its valence states. in particular, while has been hypothesized that the tin (IV) oxide contains Sb (V) within the bulk lattice and Sb (III) located at surface sites, no direct experimental evidence for this has been provided.Here we use electron energy loss spectroscopy (EELS) combined with Z-contrast imaging in a JEOL 2010F field emission STEM/TEM operating at 200 KV to analyze ATO catalysts.

2021 ◽  
Author(s):  
Yuri Mikhlin ◽  
Roman Borisov ◽  
Sergey Vorobyev ◽  
Yevgeny Tomashevich ◽  
Alexander Romanchenko ◽  
...  

Two-dimensional phenomena are attracting enormous interest at present and the search for novel 2D materials is very challenging. We propose here the layered material valleriite composed of altering atomic sheets of Cu-Fe sulfide and Mg-based hydroxide synthesized via a simple hydrothermal pathway as particles of 50-200 nm in the lateral size and 10-20 nm thick. The solid products and aqueous colloids prepared with various precursor ratios were examined using XRD, TEM, EDS, X-ray photoelectron spectroscopy (XPS), reflection electron energy loss spectroscopy (REELS), Raman, Mössbauer, UV-vis-NIR spectroscopies, magnetic, dynamic light scattering, zeta potential measurements. The material properties are largely determined by the narrow-gap (less than 0.5 eV) sulfide layers containing Cu+ and Fe3+ cations, monosulfide and minor polysulfide anions but are strongly affected by the hydroxide counterparts. Particularly, Fe distribution between sulfide (55-90%) and magnesium hydroxide layers is controlled through insertion of Al into the hydroxide part and by Cr and Co dopants entering both layers. Room-temperature Mössbauer signals of paramagnetic Fe3+ transformed to several Zeeman sextets with hyperfine magnetic fields up to 500 kOe in the sulfide layers at 4 K. Paramagnetic or more complicated characters were observed for valleriites with higher and lower Fe concentrations in hydroxide sheets, respectively. Valleriite colloids showed negative zeta potentials, suggesting negative electric charging of the hydroxide sheets, and optical absorption maxima between 500 nm and 700 nm, also depended on the Fe distribution. The last features observed also in the REELS spectra may be due to localized surface plasmon or, more likely, quasi-static dielectric resonance. The tunable composition, electronic, magnetic, optic and surface properties highlight valleriites as a rich platform for novel 2D composites promising for numerous applications.


2000 ◽  
Vol 15 (10) ◽  
pp. 2076-2079
Author(s):  
Chika Nozaki ◽  
Takashi Yamada ◽  
Kenji Tabata ◽  
Eiji Suzuki

Synthesis of a rutile-type lead-substituted tin oxide with (110) face was investigated. The characterization was performed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive x-ray spectroscopy, infrared spectroscopy, x-ray photoelectron spectroscopy, and Brunauer–Emmett–Teller surface area measurements. The homogeneous rutile-type lead-substituted tin oxide was obtained until 4.1 mol% of tin was substituted with lead. The surface of obtained oxide had a homogeneously lead-substituted (110) face.


2010 ◽  
Vol 114 (51) ◽  
pp. 22413-22416 ◽  
Author(s):  
V. R. Galakhov ◽  
A. S. Shkvarin ◽  
A. S. Semenova ◽  
M. A. Uimin ◽  
A. A. Mysik ◽  
...  

2020 ◽  
Vol 105 (6) ◽  
pp. 833-847
Author(s):  
Florence T. Ling ◽  
Jeffrey E. Post ◽  
Peter J. Heaney ◽  
Cara M. Santelli ◽  
Eugene S. Ilton ◽  
...  

Abstract With a focus on a large set of natural birnessites collected from terrestrial, freshwater systems, we applied and compared the capabilities of X-ray diffraction (XRD), extended X-ray absorption fine structure (EXAFS), Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS) to characterize crystal structure and chemistry. Using XRD, we successfully identified 3 of the 11 natural birnessite samples as hexagonal ranciéite-like phases, but the remaining samples yielded less interpretable “3-line” diffraction patterns with broad, asymmetrical peaks at d-spacings of ~7.2, ~2.4, and ~1.4 Å. EXAFS analysis suggested that many of these samples had characteristics of both triclinic and hexagonal birnessite. However, application of EXAFS to the ranciéite-like phases yielded unreasonably high concentrations of triclinic birnessite as an intergrowth, calling into question the use of synthetic hexagonal H-birnessite as an appropriate standard in the linear combination fitting of EXAFS data for natural birnessites. FTIR spectroscopy of the “3-line” birnessite samples successfully distinguished triclinic and hexagonal constituents, and analyses of peak positions suggested that natural birnessites occur as a full spectrum of triclinic and hexagonal intergrowths. XPS analysis of these samples revealed that higher Mn3+ concentrations relative to Mn2+ and Mn4+ are correlated to increased proportions of triclinic birnessite.


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