本論文利用中溫水熱合成法合成出三個含鉛離子和三價金屬陽離子之 混亞磷酸 -磷酸鹽化合物， Pb2Al(HPO3)3(H2PO4) (A1)、 Pb2Ga(HPO3)3(H2PO4) (A2)和 Pb2Fe(HPO3)2(HPO4)(H2PO4) (A3)。三個化合物皆由單晶 X光繞射實 驗解析出化合物的晶體結構，再用 EDS 確定化合物元素組成，而當中化合 物 A1、 A2有進一步測量紅 外光 光譜和固態核磁共振來進行定性及光學性 質的分析。化合物 A1、 A2和 A3 三個化合物皆為透明片狀的三維網狀結構 且三個化合物為等結構化合物，三個化合物的空間群皆為中心對稱的 Cmcm 三個化合物 的結構都具有三價陽離子的亞磷酸層狀結構和磷酸二氫鉛層狀 結構。兩 種 層狀結構在以共享氧原子的方式互相連接 形成三維的網狀結構。 A1和 A2化合物 的 紅外 光 光譜儀的測量， 顯示 化合物結構中有 P-H鍵結存 在 因此確認兩個化合物具有亞磷 酸基團 ，兩個化合物在經由固態核磁共振 的測量確認鋁、鎵和磷原子的配位環境。本論文三個化合物皆為混亞磷酸 -磷酸鹽化合物，這類型的化合物在現有的文獻中相當稀少 ，顯示中溫水熱合 成法可以合成新結構的化合物 。;mixed phosphite-phosphates containing lead cation and trivalent metal cations, Pb2Al(HPO3)3(H2PO4) (A1), Pb2Ga(HPO3)3(H2PO4) (A2) and Pb2Al(HPO3)2(HPO4)(H2PO4) (A3), were synthesized in a Teflon-lined autoclave under middle-temperature hydrothermal conditions. Their structures were characterized by single-crystal X-ray diffraction and their contents were verified by energy dispersive spectroscopy. The purity was confirmed by powder X-ray diffraction. The presence of the P-H group in [HPO3] and the hydrogen bonding interactions in the structures were studied by infrared spectroscopy. In addition solid state NMR spectra of A1 and A2 were measured to study the coordination environments of P, Al, and Ga atoms. The three compounds are isostructural with the centrosymmetric orthorhombic space group Cmcm. The structure contains [MO6] (M=Al、Ga、Fe) octahedra which are linked by phosphite and dihydrogen phosphate ligands to from 2D layers with the eight-coordinate lead ions being located in the interlayer region. Few well-characterized trivalent metal phosphite-phosphates have been documented. A comparison with related compounds in the literature will also be reported.
