本論文利用高溫高壓水熱合成法在600 °C 155 MPa 的狀態下，合成出兩個鈾磷酸鹽化合物Na2U(PO4)2 (A1)和K4[(UO2)3O2(PO4)2] (A2)。利用單晶X 光繞射方法收集數據後進行結構解析，並以粉末X 光圖譜與理論圖譜做比對以確定樣品純度供後續分析，再以X 光能量散布分析和高解析度場發射電子微微探儀等方式進行定量與定性分析。 A1 結構是一個新的四價鈾磷酸鹽化合物，結構中的鈾氧多面體以共角 跟共邊的方式連接形成一維的無限鏈，再與磷氧多面體與鈾氧多面體以共 角的方式形成三維結構。晶體數據如下: Na2U(PO4)2, orthorhombic, Fddd (No.70), a = 6.9485(5) Å， b = 11.7506(8) Å， c =17.3544(11) Å， V = 1416.97(17)Å 3， Z = 6， R1 = 0.0120 和 wR2 = 0.0368。 A2 為一個六價鈾磷酸鹽化合物，兩個鈾具有不同配位數，U(1) 是UO7 pentagonal bipyramid，U(2) 是UO8 hexagonal bipyramid，以anion-topology來描述其結構，屬於Phosphuranylite type。晶體數據如下: K4[(UO2)3O2(PO4)2],monoclinic, P21/c (No. 14)， a = 6.7323(4) Å ， b = 16.8465(10) Å ， c =7.0415(4) Å，= 99.250(2)°， V = 788.23(8) Å 3， Z = 2， R1 = 0.0261 和 wR2 = 0.0674。;Two uranium phosphates, Na2U(PO4)2 (A1) and K4[(UO2)3O2(PO4)2] (A2), were synthesized under hydrothermal conditions at 600 °C and 155 MPa. Both of these two structures were determined by single-crystal X-ray diffraction. The purity of each compound was confirmed by powder X-ray diffraction. These compounds were further characterized by EDS, EPMA and UV-vis spectroscopy. Compound A1 is a new uranium(IV) phosphate. Its crystal structure contains 1D chains of vertex- and edge-sharing UO8 snub-disphenoidal polyhedra, which are linked by sharing edges with PO4 tetrahedra to form a 3D framework. Crystal data: Na2U(PO4)2, orthorhombic, Fddd (No. 70), a = 6.9485(5) Å ， b = 11.7506(8) Å ， c = 17.3544(11) Å ， V = 1416.97(17) Å 3，Z = 6， R1 = 0.0120 and wR2 = 0.0368. Compound A2 is a uranium(VI) phosphate. Its crystal structure contains two unique U atoms with different coordination environments. U(1) is pentagonal bipyramidal and U(2) is hexagonal bipyramidal. The compound adopts the phosphuranylite type structure. The sheet anion topology approach was used for the description of this complex structure. Crystal data: K4[(UO2)3O2(PO4)2], monoclinic, P21/c (No. 14)， a = 6.7323(4) Å ， b = 16.8465(10) Å， c = 7.0415(4) Å， = 99.250(2)°， V = 788.23(8) Å 3， Z = 2， R1 = 0.0261 and wR2 = 0.0674.
