Details

Autor(en) / Beteiligte

• Bischoff, Christine
• Eckert, Hellmut
• Apel, Elke
• Rheinberger, Volker M
• Höland, Wolfram

Titel

Phase evolution in lithium disilicate glass-ceramics based on non-stoichiometric compositions of a multi-component system: structural studies by 29Si single and double resonance solid state NMR

Ist Teil von

• Physical chemistry chemical physics : PCCP, 2011-01, Vol.13 (1), p.454-4551

Ort / Verlag

Cambridge: Royal Society of Chemistry

Erscheinungsjahr

2011

Quelle

Alma/SFX Local Collection

Beschreibungen/Notizen

• The crystallization mechanism of a high-strength lithium disilicate glass-ceramic in the SiO 2 -Li 2 O-P 2 O 5 -Al 2 O 3 -K 2 O-(ZrO 2 ) system, used as restorative dentistry material, has been examined on the basis of quantitative 29 Simagic angle spinning (MAS) and 29 Si{ 7 Li} rotational echo double resonance (REDOR) NMR spectroscopy. Crystallization occurs in two stages: near 650 °C a significant fraction of the Q (3) units disproportionates into crystalline Li 2 SiO 3 and Q (4) units. Upon further annealing of this glass-ceramic to 850 °C the crystalline Li 2 SiO 3 phase reacts with the Q (4) units of the softened residual glass matrix, resulting in the crystallization of Li 2 Si 2 O 5 . The NMR experiments provide detailed insight into the spatial distribution of the lithium ions suggesting the absence of lithium ion clustering in the residual glassy component of the final glass-ceramic. 31 P MAS-NMR spectra indicate that phosphate acts as a lithium ion scavenger, resulting in the predominant formation of orthophosphate (P (0) ) and some pyrophosphate (P (1) ) groups. Crystallization of Li 2 SiO 3 occurs concomitantly with the formation of a highly disordered Li 3 PO 4 phase as evidenced from strong linebroadening effects in the 31 P MAS-NMR spectra. Well-crystallized Li 3 PO 4 is only formed at annealing conditions resulting in the formation of crystalline lithium disilicate. These results argue against an epitaxial nucleation process previously proposed in the literature and rather suggest that the nucleation of both lithium metasilicate and lithium disilicate starts at the phase boundary between the disordered lithium phosphate phase and the glass matrix. NMR yields information regarding the structural transformation processes involved in the two-stage crystallization of non-stoichiometric lithium disilicate glass.