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DOI: 10.1039/A608325K (Paper) Reference Section for: J. Mater. Chem., 1997, 7, 1573-1580

\23Na,27Al and31P NMR and X-ray powder diffraction study of Na/Ca/Al phosphate glasses and ceramics

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Isaac Abrahams, Katrin Franks, Geoffrey E. Hawkes, George Philippou, Jonathan Knowles, Philippe Bodart and Teresa Nunes

Abstract

The techniques of X-ray powder diffraction and solid-state magic angle spinning (MAS)23Na, 27Al, and 31P nuclear magnetic resonance (NMR) spectroscopy have been combined to investigate the speciation in a series of glasses and glass ceramics of general formula (P2O5)0.45(CaO)0.24 (Na2O)0.31-x(Al2O 3)x,x=0.0–0.05. The principal phosphate species are shown to be various P2O74- containing phases, and cylic trimetaphosphates bridged by Ca, i.e. Na4Ca(PO3)6 (instead of open-chain metaphosphates). Higher concentrations of Al2O3 result in glass ceramics which are phosphate-depolymerised (Q2 →Q1) with respect to the parent glasses. At a lower level of Al2O3 (2%) the aluminium is present in octahedral coordination, while the higher level (5%) results in the formation of tetrahedrally coordinated aluminium. X-Ray powder diffraction of the ceramic with the higher aluminium content indicated the presence of Na5Ca2Al(PO4)4 , and the 31P NMR spectrum provides evidence for Q12 species similar to phosphorus in aluminium metaphosphate. The more detailed structural information available from the aluminium-free glass ceramic, and the similarity in the Q1 /Q2 ratio between the glass and its derived ceramic leads to the thesis that the ceramic structure may, in favourable cases, be used to model phosphate speciation in the glass.

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