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Preparation and characterization of Si modified Ge 9 cluster
Author(s) -
Ren Tiezhen,
Xiao Pengyan,
Xing XiangYing,
Christensen K. E.
Publication year - 2010
Publication title -
crystal research and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.377
H-Index - 64
eISSN - 1521-4079
pISSN - 0232-1300
DOI - 10.1002/crat.201000369
Subject(s) - germanate , ethylene diamine , powder diffraction , hydrothermal circulation , diffraction , cluster (spacecraft) , amine gas treating , crystallography , hydrothermal synthesis , tetrahedron , materials science , chemistry , chemical engineering , nuclear chemistry , organic chemistry , physics , computer science , ion , programming language , optics , engineering
Open‐framework germanates show interesting pore structures due to their flexible building units. Germanates with different topology built from the Ge 9 cluster can be prepared in several amine systems. This paper reports, the Si modified germanate ICMM6 (denoted as HUT‐2) prepared in ethylene diamine solution through a hydrothermal synthesis route. HUT‐2 is a silicogermanate with space group C222 1 (a=12.1299(6) Å, b=13.9329(11) Å, c=14.2205(6) Å, V=2403.33(25) Å 3 ) formed by the Si modified Ge 9 cluster. A variation of unit cell parameters is observed that is in accordance with Si‐content. Powder X‐ray diffraction, ICP and TGA‐DSC analysis were recorded to determine the Si‐composition at the tetrahedral sites. Structure refinements against the X‐ray powder diffraction (XRPD) pattern determined the occupancy of Si at the two tetrahedral sites. An approximate Si/Ge ratio of 0.13‐0.18 is obtained based on these characterizations. TGA‐DSC analysis showed obvious weight loss of amine at 315 °C, which is higher than the reported pure germanate ICMM6. This further confirms the existence of Si within the structure of HUT‐2. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)