本論文利用中溫水熱法及高溫高壓水熱法合成兩系列的化合物，第一系列鑭系金屬亞磷酸鹽化合物：[Ln(H2O)(C2O4)0.5(HPO3)]．H2O [Ln = Eu (A1)、Gd (A2)、Tb (A3)；第二系列是混鑭系金屬鍺酸鹽化合物：K3(EuXLn1-x)3Ge6O18 [Ln = Nd (B1)、Tm (B2)]。此兩系列的化合物利用單晶X光繞射儀定出結構及化學式，以粉末X光繞射圖譜比對理論圖譜確定樣品純度後進行物理性質的量測，並針對不同鑭系金屬研究其發光特性。 A系列的三個化合物互為等結構化合物，二維鑭系金屬亞磷酸鹽的無機層狀結構經由雙邊雙螯合的草酸連結，形成結構新穎的三維孔洞化合物。利用熱重分析，得知化合物在 150 ℃ 時會脫去一結晶水分子，但不影響原骨架結構，進一步以變溫粉末 X光繞射研究，證實此系列化合物對水分子有脫附與吸附的能力；此外，針對化合物中心金屬發光特性不同，進行放光與激發光譜的研究與探討，期望未來能藉由掺入不同鑭系金屬合成出發白光的化合物。 B系列的兩個化合物則是以高溫高壓水熱法在先前合成出的化合物K3Eu3Ge6O18 中混入不同鑭系金屬，部份取代原兩種銪金屬的位置，以改變其發光性質，再利用放光、激發光譜與生命期的測量，詳細探討其發光特性。 Two series of lanthanide compounds were synthesized by the hydrothermal method and the high-temperature,high pressure hydrothermal method. The series A denotes lanthanide Oxalatophosphites [Ln(H2O)(C2O4)0.5(HPO3)]．H2O [Ln = Eu (A1)、Gd (A2)、Tb (A3), while the series B denotes lanthanide germanates, K3(Eu0.78Nd0.22)3Ge6O18 (B1) and K3(Eu0.82Tm0.18)3Ge6O18 (B2). All structures and formula of these compounds are determined by single-crystal X-ray diffraction. The purity of each compound was confirmed by the good agreement between the observed powder X-ray diffraction pattern and the calculated pattern based on single-crystal XRD. The properties of these compounds such as thermal stability and luminescence phenomena were further characterized by different physical measurements respectively according to their structural features. A1、A2 and A3 are isostructural. The novel three-dimensional structure is formed by two-dimensional layers of lanthanide phosphites which are linked by bisbidentate oxalates. Studies of thermal stability and guest desorption-sorption properties showed that a dehydrated compound can absorb water reversibly. At the end, the luminescence spectra were successfully recorded and the results will be discussed. B1 and B2 were synthesized by adding a desired combination of lanthanide ions, and both of them are isostructural with K3Eu3Ge6O18. Displacing two different Eu3+ sites partially to investigate their interesting luminescence properties and the results will also be briefly discussed.