在本論文中，根據實驗方法，簡單分為二個部分來介紹(1)利用中溫水熱法和離子熔液合成法合成含有有機配位基的金屬磷酸鹽的化合物(2)利用熔鹽法合成鑭系矽酸鹽和銦鍺酸鹽化合物。以下將針對不同的合成方法，簡單的介紹。 (1)含有草酸根配位基的金屬磷酸鹽，依據合成方法不同分為二個方向。 a.中溫水熱法：利用傳統水熱合成法，合成一個新穎的釩草酸磷酸化合物(A1)，並且研究其熱穩定性，此二維結構具有一個特殊的D6R單元。等結構的鐵化合物也被合成。 b.離子熔液法：利用choline chloride/oxalic acid的離子熔液當溶劑，合成三維的鎵草酸磷酸鹽(B1)。在本實驗中，離子熔液除了提供溶劑角色，並同時提供了配位的草酸根。，並且加入有機胺(TMPD)，合成具有3D骨架結構的化合物(B1)。這是第一個利用離子熔液法，合成含有有機胺的金屬草酸磷酸鹽的例子。有機胺在結構中呈現一個非序化的情形，因此特別利用NMR來加以證實有機胺的存在。 (2)金屬矽(鍺)酸鹽 a.鑭系矽酸鹽：利用KF-MoO3熔鹽法，合成了第一個具有salt-inclusion，三個等結構的鑭系矽酸鹽鹽(C1~C3)，並且測量其光譜。 b.銦鍺酸鹽：使用RbF-MoO3當熔鹽，合成一個特殊的二維層狀銦鍺酸鹽結構(D1)，結構的矽酸層為unbranched zweier single layer的鍵結，此結構由於缺陷，UV燈下，有藍光呈現。 This thesis introduces two different experimental systems. (1) Metal oxalatophosphate synthesized by hydrothermal and ionic liquid methods. (2) Metal silicates and a germanate synthesized by flux methods. They are summarized as follows. 1. Metal oxalatophosphates: (1) Mild hydrothermal synthesis: A new vanadium(III) oxalatophosphate (denoted as A1) has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction and thermogravimetric analysis. It is one of the few compounds with 2D layer structures and the second example containing D6R units in the system of metal oxalatophosphates. The iron analogue was also synthesized. (2) Ionothermal synthesis: We have synthesized a new organically templated gallium oxalatophosphate (B1) by using a low-melting-point eutectic mixture of choline chloride and oxalic acid as a solvent. This work reports the first example of ionothermal synthesis of an organically template metal oxalatophosphate. The eutectic mixture not only acts as a solvent but also the source of oxalate ligand. 2. Metal silicates and a germanate: (1) Metal silicates: New salt-inclusion lanthanide silicates, have been synthesized using a KF-MoO3 flux (C1~C3). They are the first examples of salt-inclusion compounds in lanthanide silicate systems. The photoluminescence properties of the Eu compound have also been studied. (2) A metal germanate: A 2-D layered indium germinate was synthesized using a RbF-MoO3 flux (D1). The structure consists of unbranched zweier single layer of germanate with six-membered rings, which are connected via InO6 octahedra to form a 2D layer structure. Its photoluminescence properties were also studied.
