The Polar Phase of NaNbO: A Combined Study by Powder Diffraction, Solid-State NMR, and First-Principles Calculations.

A polar phase of NaNbO has been successfully synthesized using sol-gel techniques. Detailed characterization of this phase has been undertaken using high-resolution powder diffraction (X-ray and neutron) and Na multiple-quantum (MQ) MAS NMR, supported by second harmonic generation measurements and d...

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Published in:Journal of the American Chemical Society Vol. 132; no. 25; pp. 8732 - 8747
Main Authors: Johnston, Karen E., Tang, Chiu C., Parker, Julia E., Knight, Kevin S., Lightfoot, Philip, Ashbrook, Sharon E.
Format: Article
Published: American Chemical Society 6/30/2010
Subjects:
Online Access:View this record in EBSCOhost
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      dt: 6/30/2010
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        10.1021/ja101860r
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        atl: The Polar Phase of NaNbO: A Combined Study by Powder Diffraction, Solid-State NMR, and First-Principles Calculations.
      aug:
        au:
          Johnston, Karen E.
          Tang, Chiu C.
          Parker, Julia E.
          Knight, Kevin S.
          Lightfoot, Philip
          Ashbrook, Sharon E.
        affil:
          School of Chemistry and EaStCHEM, University of St. Andrews, St. Andrews, KY16 9ST, U.K.
          Diamond Light Source Ltd., Harwell Science and Innovation Campus, Didcot, Oxfordshire, OX11 0DE, U.K.
          ISIS Facility, Rutherford Appleton Laboratory, Chilton, Didcot, OX11 0QX, U.K.
      su:
        Sodium compounds
        Optical diffraction
        Nuclear magnetic resonance spectroscopy
        Particles (Nuclear physics)
        Second harmonic generation
        Colloids
      sug:
        subj:
          Sodium compounds
          Optical diffraction
          Nuclear magnetic resonance spectroscopy
          Particles (Nuclear physics)
          Second harmonic generation
          Colloids
      ab: A polar phase of NaNbO has been successfully synthesized using sol-gel techniques. Detailed characterization of this phase has been undertaken using high-resolution powder diffraction (X-ray and neutron) and Na multiple-quantum (MQ) MAS NMR, supported by second harmonic generation measurements and density functional theory calculations. Samples of NaNbO were also synthesized using conventional solid-state methods and were observed to routinely comprise of a mixture of two different polymorphs of NaNbO, namely, the well-known orthorhombic phase (space group Pbcm) and the current polar phase, the relative quantities of which vary considerably depending upon precise reaction conditions. Our studies show that each of these two polymorphs of NaNbO contains two crystallographically distinct Na sites. This is consistent with assignment of the polar phase to the orthorhombic space group P2ma, although peak broadenings in the diffraction data suggest a subtle monoclinic distortion. Using carefully monitored molten salt techniques, it was possible to eradicate the polar polymorph and synthesize the pure Pbcm phase.
      pubtype: Academic Journal
      doctype: Article
      src: R
    language: English
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