本論文以高溫高壓水熱法以及溶膠－凝膠法，合成出三個鋰鋁鈦磷酸鹽化合物 Li2+xAl1.18Ti0.82(PO4)3 (A1)、Li1+xAlxTi2-x(PO4)3 (A2) 及 Li1.5Fe0.5Ti1.5(PO4)3 (A3)。藉由單晶 X 光繞射方法鑑定出化合物的晶體結構，以粉末 X 光繞射分析儀確定樣品純度以供後續分析，再以 X 光螢光光譜儀、固態核磁共振儀及電化學阻抗譜等方式進行其他化學及電化學性質的分析。化合物 A1 到 A3 的結構皆以兩個 MO¬6 (M = Al, Ti) 八面體搭配三個 [PO4] 四面體以共角方式連接，組成一燈籠型的結構單元。化合物 A1 為 anti-NASICON 結構的鋰鋁鈦磷酸鹽，空間群皆為 Pbcn (No. 60)，一個燈籠型結構單元與六個相同的結構單元連接，為一個反平行結構，其中鋰離子坐落在六員環孔洞中；化合物 A2、A3為 NASICON 結構的鋰鋁鈦磷酸鹽，空間群皆為 R3 ̅c (No. 167)，一個燈籠型結構單元與四個相同的結構單元連接，為一個平行結構，其中鋰離子坐落在八員環孔洞中。將 A3 作為電解質材料，具有較好的導電性並且結構安定不崩解，離子導電度可達到 8.7 × 10-4 S/ cm，將 A2 單晶作為微電極進行導電度測量，離子導電度可達到 7.07 × 10-4 S/cm，可與液態電解質 LA25 相匹敵。;Three lithium aluminum titanium phosphates, Li2+xAl1.18Ti0.82(PO4)3 (A1), Li1+xAlxTi2-x(PO4)3 (A2) and Li1.5Al0.5Ti1.5(PO4)3 (A3) were synthesized by the high-temperature, high-pressure hydrothermal method and sol-gel method. A1 were structurally characterized by powder and single X-ray diffraction, A2 and A3 were structurally characterized by powder X-ray diffraction. These compounds were further characterized by TXRF, EDS and 7Li NMR. A2 and A3 were analyzed for electrochemical properties. Compound A1, A2 and A3 all consist of MO6 octahedral which are corner-shared with [PO4] tetrahedral. Two MO6 octahedra and three [PO4] tetrahedra are connected to form a lantern unit. Compound A1 has an anti-NASICON structure in which the lantern units are connected in an anti-parallel way. The Li+ cations are located at sites in the six-membered rings. Compound A2 and A3 both adopt the NASICON structure in which the lantern units are connected in a parallel way. The Li+ cations are located at sites in the eight-membered rings. Compound A3 shows a bulk conductivity of 8.7 × 10-4 S·cm-1. Microcontact impedance study on a single of A2 shows a very good conductivity of 7.07 × 10-3 S·cm-1 which is comparable to that of the liquid electrolyte LA25.