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Determination of the crystallized fractions of a largely amorphous multiphase material by the Rietveld method
Author(s) -
Orlhac X.,
Fillet C.,
Deniard P.,
Dulac A. M.,
Brec R.
Publication year - 2001
Publication title -
journal of applied crystallography
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.429
H-Index - 162
ISSN - 1600-5767
DOI - 10.1107/s0021889800017908
Subject(s) - borosilicate glass , amorphous solid , rietveld refinement , materials science , powder diffraction , ceramic , analytical chemistry (journal) , mineralogy , phase (matter) , crystal structure , crystallography , chemistry , composite material , chromatography , organic chemistry
The Rietveld method has proved to be a very effective means to characterize and quantify the crystalline phases and the amorphous phase in glass ceramic materials using X‐ray powder diffraction data. The technique was applied to a borosilicate glass of the type used for high‐level nuclear‐waste containment, in order to measure the proportions of the crystallized phases after heat treatment and, thus, to qualify the thermal stability of the glass. Six crystalline phases were analysed in this way in an almost entirely (>95 wt%) amorphous material after adding a known proportion of an internal standard (TiO 2 ). The quantitative analyses were corrected to allow for microabsorption effects resulting from grain‐size and absorption‐contrast effects. In addition to the quantitative data, unit‐cell parameters and site‐occupancy refinements revealed solid‐solution and substitution phenomena in the crystal.