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Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO 6 ] Octahedra Prepared by Different Reaction Routes
Author(s) -
Kowalke Janine,
Arnold Christine,
Ponomarev Ilia,
Jäger Christian,
Kroll Peter,
Brendler Erica,
Kroke Edwin
Publication year - 2019
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201801321
Subject(s) - octahedron , chemistry , silicon , crystallite , crystallography , phosphoric acid , alkoxy group , inorganic chemistry , nuclear chemistry , crystal structure , organic chemistry , alkyl
The layered silicophosphate Si(HPO 4 ) 2 was prepared via a novel synthesis approach using silicon nanopowder and ortho ‐phosphoric acid at 150 °C providing a polycrystalline product. Silicophosphate compounds with sixfold coordinated silicon atoms obtained from pyrophosphoric acid H 4 P 2 O 7 and tetraalkoxysilanes via a sol‐gel route exhibit the same short‐range order. The solid products were analyzed with XRD, elemental analysis (ICP‐AES), and detailed NMR spectroscopic studies, including 1 H, 13 C, 29 Si, and 31 P MAS‐, 31 P‐ 29 Si‐REDOR, HETCOR, and CP‐RFDR experiments. DFT calculations support the structure of Si(HPO 4 ) 2 consisting of layers of [SiO 6 ] octahedra linked by [O 3 P(OH)] tetrahedra. The OH groups point to the neighboring layers and may be substituted by ethoxy or other groups.