Structural changes above the glass transition and crystallization in aluminophosphate glasses: an in situ high-temperature MAS NMR study

J Phys Chem B. 2007 Jul 5;111(26):7529-34. doi: 10.1021/jp070692e. Epub 2007 Jun 9.

Abstract

We present an in situ high-temperature nuclear magnetic resonance study on the structural changes in aluminophosphate glasses occurring in the temperature range between the glass transition temperature Tg and the crystallization temperature Tc, Tg < T < Tc. Decisive changes in the network organization between Tg and Tc in potassium aluminophosphate glasses in the compositional range 50K2O-xAl2O3-(50 - x)P2O5 with 2.5 < x < 20 could be monitored for the first time employing 1D 31P- and 27Al-MAS NMR. Accompanying ex situ NMR experiments (31P-RFDR NMR and 31P-{27Al} CP-HETCOR NMR) on devitrified samples were performed at room temperature to further characterize the phases formed during the crystallization process. The structural role of boron-which is known to inhibit the crystallization process in these aluminophosphate glasses-on short and intermediate length scales was analyzed employing 11B-MQMAS, 11B-{27Al} TRAPDOR and 11B-{31P} REDOR NMR spectroscopy.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Aluminum Compounds / chemistry*
  • Crystallization
  • Glass / chemistry*
  • Hot Temperature*
  • Magnetic Resonance Spectroscopy*
  • Phosphates / chemistry*

Substances

  • Aluminum Compounds
  • Phosphates
  • aluminum phosphate