Objectives: The main objective is the characterisation of the setting reaction in glass ionomer cements based on experimental ionomer glasses with different fluorine content and a commercial glass ionomer cement liquid by using 13C CP/MAS-NMR, 29Si, 27Al and 31P MAS-NMR spectroscopy in order to receive information specifically about the cross-linking process. Methods: Different fluorine containing glass compositions based on 4.5SiO2-3Al2O3-1.5P2O5-(5 - z)CaO-zCaF2 where z = 0-3, were mixed with a commercially available polymer liquid to form glass ionomer cements. The cements were subjected to 27Al, 13C CP/MAS, 29Si, and 31P MAS-NMR analysis. Results: : The 27Al spectra showed clearly the formation of six-fold coordinate Al(VI), that may crosslink the carboxyl groups in the poly-acid molecules. A shift towards to more positive values of the carboxyl peak in the 13C CP/MAS-NMR spectra showed clearly the proton dissociation of the carboxyl groups. A shift towards more negative values was observed in the 29Si MAS-NMR spectra, suggesting formation of hydrated silica gel and consequently formation of additional Si-O-Si bonds. 31P MAS-NMR spectra also reflected changes in the coordination state around a PO43- tetrahedron. Increasing the fluorine content of the glasses resulted generally in increased reactivity during setting, due to promoting cross-linking and repolymerisation of the silicate phase, followed by clear changes in the MAS-NMR spectra. Conclusions: : The cross-linking process during the setting reaction of glass ionomer cements can be followed by MAS-NMR spectroscopy observing the conversion of Al(IV) to Al(VI). The acid base setting reaction is completed in 1 day and no further significant changes in the MAS-NMR spectra can be observed. Further study is required in order to understand the role of phosphorus.
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