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Synthesis and crystal structure of chlorate-enclathrated in aluminogermanate sodalite Na8[AlGeO4]6(ClO3)2

100%

Borhade A. V. , Dholi A. G.

Materials Science Poland

2013

tom Vol. 31, No. 2

246--252

Encapsulation of chlorate in sodalite with aluminogermanate host framework has been obtained by one pot hydrothermal synthesis at 393 K. The crystal structure of Na8[AlGeO4]6(ClO3)2; sodalite was refined from X-ray powder data in the space group P43n: a = 9.169 Å, where Al-O-Ge angle is 137.6. The 27Al MAS NMR study confirmed alternate Ge and Al ordering of the sodalite framework, while 23Na gave insight into the structure and dynamics of the cage fillings. Infrared spectrum confirmed the encapsulation of chlorate as well as the framework formation of aluminogermanate sodalite. SEM study showed the retention of cubical morphology of the aluminogermanate sodalite. Thermogravimetric analysis provided information on the extent of chlorate entrapment, stability within the sodalite cages and decomposition properties.

Synthesis and characterization of aluminosilicate and gallosilicate sodalites containing acetate ions

63%

Borhade A. V. , Wakchaure S. G.

Materials Science Poland

2011

tom Vol. 29, No. 2

127--134

One pot synthetic aluminosilicate and gallosilicate sodalites containing acetate guest anion have been synthesized successfully under hydrothermal conditions at 100 °C. This paper deals with the comparison of X-ray powder data with single crystal data for Na8[AlSiO4]6(CH3COO)2 and the characterization of a new Na8[GaSiO4]6(CH3COO)2 sodalite. The products obtained were characterized by IR, X-ray powder diffraction, MAS NMR, SEM and thermogravimetry technique. Crystal structures were refined in the space group P?43n from X-ray powder data using the Rietveld refinement method with the unit cell parameter a = 9.0679 A° , for aluminosilicate and a = 9.2119 A° , for gallosilicate sodalite. The aluminosilicate and gallosilicate framework shows regular bonding with bond angles of Al-O-Si = 146.241°, Ga-O-Si = 141.294°. 29Si MAS NMR chemical shift values verify Al/Si and Ga/Si ordering of the framework constituents.