TY - JOUR
T1 - Phase Transition upon K+ Ion Exchange into Na-Low Silica X
T2 - Combined NMR and Synchrotron X-ray Powder Diffraction Study
AU - Lee, Yongjae
AU - Carr, Stuart W.
AU - Parise, John B.
N1 - Copyright:
Copyright 2020 Elsevier B.V., All rights reserved.
PY - 1998/9
Y1 - 1998/9
N2 - The mechanism by which K+ ions exchange into zeolite Na-low silica X (LSX) (Na96Al96-Si96O384·nH 2O) has been determined by studying structures of the Na-LSX and K-LSX end members in the Na-K LSX solid solution series as well as samples exchanged at the 20%, 42% and 80% K+ levels. A preliminary investigation using 29Si MAS NMR spectroscopy revealed a two-phase region in the solid solution near 80% K+ exchange. Rietveld analysis of the powder diffraction data collected from hydrated samples showed that, up to 42% of K+ exchange, K+ ions were located preferentially at site I′, just outside the double 6-ring (D6R) in the sodalite cage, and at site II, above the single 6-ring (S6R) in the supercage. Introduction of K+ ions into site I′ repositioned Na+ ions into site I, at the center of the D6R. An abrupt change in the cubic lattice parameter from 25.0389(5) to 25.2086(5) Å marked the formation of a second phase at the 80% K+-exchange level as K+ ions began to occupy site I. No coexistence of phases was observed for the fully K+-exchanged sample (a = 25.2486(2) Å), where sites I and II were fully occupied by K+ ions.
AB - The mechanism by which K+ ions exchange into zeolite Na-low silica X (LSX) (Na96Al96-Si96O384·nH 2O) has been determined by studying structures of the Na-LSX and K-LSX end members in the Na-K LSX solid solution series as well as samples exchanged at the 20%, 42% and 80% K+ levels. A preliminary investigation using 29Si MAS NMR spectroscopy revealed a two-phase region in the solid solution near 80% K+ exchange. Rietveld analysis of the powder diffraction data collected from hydrated samples showed that, up to 42% of K+ exchange, K+ ions were located preferentially at site I′, just outside the double 6-ring (D6R) in the sodalite cage, and at site II, above the single 6-ring (S6R) in the supercage. Introduction of K+ ions into site I′ repositioned Na+ ions into site I, at the center of the D6R. An abrupt change in the cubic lattice parameter from 25.0389(5) to 25.2086(5) Å marked the formation of a second phase at the 80% K+-exchange level as K+ ions began to occupy site I. No coexistence of phases was observed for the fully K+-exchanged sample (a = 25.2486(2) Å), where sites I and II were fully occupied by K+ ions.
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U2 - 10.1021/cm980342s
DO - 10.1021/cm980342s
M3 - Article
AN - SCOPUS:0001661263
VL - 10
SP - 2561
EP - 2570
JO - Chemistry of Materials
JF - Chemistry of Materials
SN - 0897-4756
IS - 9
ER -