Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO 6 ] Octahedra Prepared by Different Reaction Routes: Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO 6 ] Octahedra Prepared by Different Reaction Route
Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO 6 ] Octahedra Prepared by Different Reaction Routes: Structural Insight into Layered Silicon Hydrogen Phosphates Containing [SiO 6 ] Octahedra Prepared by Different Reaction Route
复制标题
不同反应路线制备的含[SiO 6 ]八面体的层状磷酸氢硅盐的结构见解： 不同反应路线制备的含[SiO 6 ]八面体的层状磷酸氢硅盐的结构见解
DOI：
10.1002/ejic.201801321
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发表时间：
2019
影响因子：
2.3
通讯作者：
Kroke, Edwin
中科院分区：
文献类型：
--
作者：
Kowalke, Janine;Arnold, Christine;Ponomarev, Ilia;Jäger, Christian;Kroll, Peter;Brendler, Erica;Kroke, Edwin
采用纳米硅粉和正磷酸在150 °C下合成了层状磷酸硅Si（HPO 4）2，得到了多晶产物。由焦磷酸H4 P2 O 7和四烷氧基硅烷通过溶胶-凝胶路线获得的具有六配位硅原子的硅磷酸盐化合物表现出相同的短程有序。用XRD、元素分析（ICP-AES）和详细的NMR光谱研究（包括1H、13 C、29 Si和31 P MAS-、31 P-29 Si-REDOR、HETCOR和CP-RFDR实验）分析固体产物。DFT计算支持Si（HPO 4）2的结构，该结构由[O3 P（OH）]四面体连接的[SiO 6]八面体层组成。OH基团指向相邻层，并且可以被乙氧基或其他基团取代。
The layered silicophosphate Si(HPO4)2was prepared via a novel synthesis approach using silicon nanopowder andortho‐phosphoric acid at 150 °C providing a polycrystalline product. Silicophosphate compounds with sixfold coordinated silicon atoms obtained from pyrophosphoric acid H4P2O7and 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, including1H,13C,29Si, and31P MAS‐,31P‐29Si‐REDOR, HETCOR, and CP‐RFDR experiments. DFT calculations support the structure of Si(HPO4)2consisting of layers of [SiO6] octahedra linked by [O3P(OH)] tetrahedra. The OH groups point to the neighboring layers and may be substituted by ethoxy or other groups.