A. Nordmann et al., STRUCTURAL CHARACTERIZATION OF LITHIUM ALUMINOSILICATE GLASS AND GLASS-CERAMICS DERIVED FROM SPODUMENE MINERAL, Journal of physics. Condensed matter, 7(16), 1995, pp. 3115-3128
Lithium aluminosilicate (LAS) glass and glass ceramics derived from sp
odumene mineral have been studied by transmission electron microscopy
(TEM), x-ray diffraction (XRD), positron annihilation lifetime spectro
scopy (PALS) and solid state nuclear magnetic resonance (NMR) as as-ca
st glass, as partially crystallized glasses, and as fully crystalline
glass ceramics. The nucleation and growth of the crystalline phases at
725 degrees C up to 1000 degrees C have been studied as functions of
varying time and temperature. Both TEM and PALS are effective tools fo
r studying the development of the nanophase structure in the partially
crystallized glass. TEM observation established the size and number o
f crystallites present in the glassy matrix, whilst the PALS component
attributed to orthopositronium (oPs) pickoff annihilation was remarka
bly sensitive to the nucleation and growth of the crystalline phases i
n the glass ceramic. This oPs component was associated either with the
nuclei/glass interface or with the nuclei structure. XRD and NMR were
used to study the evolution of the two crystalline phases which form
from the glass in the temperature range 725 degrees C to 1000 degrees
C, the beta-quartz solid solution (ss) phase below 900 degrees C and t
he beta-spodumene ss phase above 900 degrees C. The Si-29 NMR spectra
of both beta-quartz ss and beta-spodumene ss phases show structures as
sociated with the next nearest neighbour configurations of the central
SiO4 units. The Si-29 and Al-27 NMR spectra of alpha-spodumene minera
l and beta-spodumene ss phase formed by annealing alpha-spodumene are
compared to the spectra for the glass and crystalline phases formed fr
om the melt.