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Silicon Clathrates: Synthesis and Characterization

  • Ganesh K. Ramachandran (a1), Jason Diefenbacher (a2), Otio F. Sankey (a3), Renu Sharma (a4), Robert F. Marzke (a3), Michael O'keeffe (a5), Jan Gryko (a6) and Paul F. Mcmillan (a4)...

Abstract

Two types of silicon clathrates, NaxSi136 (0≤ × ≤ 24) and Na8Si46 and a mixed clathrate (Na,Ba)Si46 were synthesized and characterized by X-ray diffraction, 23Na NMR and high resolution TEM. Systematic changes in X-ray diffraction intensities enabled the sodium content and site occupancy in the NaxSi136 series to be followed and then refined by Rietveld profile analysis. 23Na NMR spectra of Na8Si46 and NaxSi136 samples reveals two peaks with large paramagnetic shifts (1600-2000 ppm) for each phase, associated with the presence of Na atoms in two different environments. High resolution electron microscopy reveals the clathrate structures of these samples, and allows classes of defects to be characterized.

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