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Synthesis, Rietveld Analysis, and Solid State Nuclear Magnetic Resonance of X 2 ‐Sc 2 SiO 5
Author(s) -
Alba María D.,
Chain Pablo,
GonzálezCarrascosa Triana
Publication year - 2009
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1551-2916.2008.02877.x
Subject(s) - monoclinic crystal system , crystallography , valence (chemistry) , rietveld refinement , materials science , powder diffraction , solid state nuclear magnetic resonance , nuclear magnetic resonance spectroscopy , spectroscopy , x ray crystallography , crystal structure , space group , chemistry , diffraction , nuclear magnetic resonance , analytical chemistry (journal) , stereochemistry , physics , organic chemistry , quantum mechanics , chromatography , optics
Compounds containing rare earths are of increasing technological interest especially because of their unique mechanical, magnetic, electrical, and optical properties. Among them, rare earth oxyorthosilicates are attractive scintillators for γ‐ and X‐ray spectroscopy and detection. However, there are many structural aspects of those compounds that are not clear. In this research, the structure parameters for Sc 2 Si 2 O 5 , X 2 ‐polymorph, have been refined from powder X‐ray diffraction (XRD) data and the 29 Si MAS NMR spectrum is reported for the first time. X 2 ‐Sc 2 SiO 5 polymorph was synthesized by the sol–gel method and characterized by XRD and 29 Si MAS NMR. The XRD pattern was indexed in a monoclinic unit cell with space group I 2/ c ; the resulting unit cell parameters were a =9.9674(2) Å, b =6.4264(9) Å, c =12.0636(2) Å, and β=103.938(1)°. The 29 Si MAS NMR spectrum showed a unique signal at −79.5 ppm, compatible with the unique Si crystallographic site in the unit cell. Finally, the band valence method has been applied to the calculation of a “shift parameter,” which is correlated with the NMR chemical shift.