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  The structural genesis of a complex (MoVW)5O14 oxide during thermal treatments and its redox behavior at elevated temperatures

Zenkovets, G. A., Kryukova, G. N., Gavrilov, V. Y., Tsybulya, S. V., Anufrienko, V. A., Larina, T. A., et al. (2007). The structural genesis of a complex (MoVW)5O14 oxide during thermal treatments and its redox behavior at elevated temperatures. Materials Chemistry and Physics, 103(2-3), 295-304. doi:10.1016/j.matchemphys.2007.02.029.

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 Creators:
Zenkovets, Galina A., Author
Kryukova, Galina N., Author
Gavrilov, Vladimir Yu., Author
Tsybulya, Sergei V., Author
Anufrienko, Vladimir A., Author
Larina, Tatiana A., Author
Khabibulin, Dzhalil F., Author
Lapina, Olga B., Author
Rödel, Eva1, Author              
Trunschke, Annette1, Author              
Ressler, Thorsten1, Author              
Schlögl, Robert1, Author              
Affiliations:
1Inorganic Chemistry, Fritz Haber Institute, Max Planck Society, ou_24023              

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Free keywords: Nanostructures, molybdenum oxide, Mo5O14, electron microscopy 4, Molybdates in C3 selective oxidations
 Abstract: The structural genesis of a Mo0.68V0.23W0.09 oxide with Mo5O14-like structure has been examined. A precursor prepared by spray-drying of mixed aqueous metal salt solutions was calcined in air and subsequently treated in helium at different temperatures. X-ray diffraction, HRTEM, 51V MAS NMR, ESR, UV/Vis DR spectroscopy and oxygen and hydrogen adsorption measurements have been applied to monitor the preparation procedure. It was found that a structure closely related to that of Mo5O14 already appears at nano-scale level after calcination of the spray-dried precursor in air at 350°C. At this stage, the material comprises of crystalline particles less than 3 nm in size stabilized by an amorphous matrix. Further heating causes nano-structural rearrangements that lead to the formation of the final Mo0.68V0.23W0.09 oxide with phase-pure polycrystalline structure. Molybdenum and tungsten ions are hexavalent and coordinated in an octahedral environment. Furthermore, vanadium is present as V4+ and V5+ ions which partially occupy octahedral sites, whereas highly distorted trigonal pyramidal sites could be accommodated in pentagonal bipyramids of the Mo5O14 structure, however, displaced away from the center. According to the results of H2 and O2 adsorption the crystalline ternary oxide does not possess accessible micropores. Oxygen pulses at 450oC and reductive treatment with pure hydrogen at 300oC did not cause noticeable changes of the bulk structure thus indicating a remarkable structural stability of the complex MoVW oxide under redox conditions at elevated temperature.

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Language(s): eng - English
 Dates: 2007
 Publication Status: Published in print
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 Table of Contents: -
 Rev. Type: Peer
 Identifiers: eDoc: 299668
DOI: 10.1016/j.matchemphys.2007.02.029
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Title: Materials Chemistry and Physics
  Alternative Title : Mat. Chem. Phys.
Source Genre: Journal
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Pages: - Volume / Issue: 103 (2-3) Sequence Number: - Start / End Page: 295 - 304 Identifier: -