Abstract

Perchlorate enclathrated sodalite with gallosilicate host framework has been synthesized under low temperature (100 o C) hydrothermal technique and characterized by X-ray powder diffraction, IR, Raman spectroscopy, UV DRS, SEM, MAS NMR spectroscopy and thermogravimetry. The structural features were investigated by IR, MAS NMR spectroscopy of 29 Si and 23 Na nuclei and by Reitveld refinement of X-ray powder diffraction data. IR and Raman spectroscopy confirms formation of framework and presence of ClO4 - group. The tetrahedral framework T-atoms are completely ordered and the chloride atoms are located at the centre of the sodalite cages. The crystal structure of this new sodalite was refined in the space group P 4 3n with a = 9.15788 A, V = 768.5 A, Z =1, Rwp = 0.0611, Rp = 0.1079 and Si-O-Ga is 144.036 o . The surface area of single entity with stoichiometry Na8[GaSiO4]6(ClO4)2 was found to be 8.385x10 -15 cm 2 /g. 29 Si MAS NMR study confirms complete ordering of Si and Ga in the gallosilicate framework. Thermo gravimetric analysis has provided information on the extent of perchlorate entrapment, stability within the cage and decomposition properties.

Highlights

  • The cubic framework structure of sodalites with general composition Na8[T1T2O4]6X2 is formed by a space filling array of truncated octahedral cages each built up of tetrahedral TO4 units

  • Sodalites are expected to be an interesting model system for studying simple principle of perchlorate storage in small cavities of framework structure (Weitkamp et al, 1995), we extend our experimental work here on synthesis, characterization and structure of perchlorate encapsulated sodalite with gallosilicate framework

  • Perchlorate anions have been successfully encapsulated within gallosilicate sodalite

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Summary

Introduction

The cubic framework structure of sodalites with general composition Na8[T1T2O4]6X2 is formed by a space filling array of truncated octahedral cages each built up of tetrahedral TO4 units. According to the host guest interactions the cage filling ions and the type of framework T-atoms are both responsible for the chemical and physical properties of a certain sodalite species. Mean while many sodalites have been synthesized with large number of element combinations with compositions Na8[AlSiO4]6X2, where X is a monovalent guest anion, X= Cl-, Br-, ClO4-, is formed by TO4 tetrahedra as elementary building unit (Pauling, 1930; Lons et al, 1967). Depending on the composition sodalite posses photochromic, cathodochromic, ion conducting properties and as high density optical data storage materials. Little attention is given on synthesis and detailed characterization of gallosilicate sodalite

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