本論文使用高溫高壓水熱合成法，合成出 3 個的鋰鈦磷酸鹽化合物 : LiTi2(PO4)3 (A1)、Li1+xTi2-xFex(PO4)3 (x=0.8) (A2)、 Li1+xTi2-xFex(PO4)3 (A3)，藉由單晶 X 光繞射方法鑑定出化合物的晶體結構，並使用粉末 X 光繞射確定樣品純度以供後續分析，再以 X 光能量散佈分析、感應耦合電漿原子發射光譜儀、穆斯堡爾光譜儀等儀器進行定量及鐵離子周圍環境之分析。
A1 和 A3 為 NASICON 結構，它們皆為三方晶系，空間群為 R-3c，結構中的 2 個 MO6 與 3 個 PO4 會以共角的方式式連接成一個燈籠狀結構單元，其燈籠狀結構單元又以平形的方向互相作排列，鋰離子座落於八員環中。
A2 為 anti-NASICON 結構，其為正交晶系，空間群為 Pbcn. A2 也是由燈籠狀結構單元所組成，其燈籠狀結構單元的組成與 A1 (A3) 相同，不同的是其燈籠狀結構單元是以反平形的方向作排列，而鋰離子座落於六員環中。
並且使用溶膠-凝膠法合成出鋰鐵鈦磷酸鹽化合物 : Li1+xTi2-xFex(PO4)3 (x=0.5) (A4, LFTP)，藉由粉末 X 光繞射鑑定其為NASICON結構。A4 可做為穩定的鋰電池之電解質材料，其離子導電度可達到 1 x 10-3 S· cm-1，將 A4 導入陰極材料，其放電電容量可達到 14.6 mAh。

Three lithium titanium phosphates, LiTi2(PO4)3 (A1), Li1+xTi2-xFex(PO4)3 (x=0.8) (A2), Li1+xTi2-xFex(PO4)3 (A3), were synthesized by the high-temperature, high-pressure hydrothermal method, and structurally characterized by powder and single X-ray diffraction. These compounds were further characterized by XRF, ICP-OES and Mössbauer spectroscopy.
A1 and A3 adopt the NASICON structure with the trigonal space group R-3c. They both consist of lantern structure units which are composed of two MO6 octahedra and three PO4 tetrahedra by corner-sharing, and the units are connected in aparallel way. The lithium cations are located in the eight-membered rings.
A2 adopts the anti-NASICON structure with the orthorhombic space group Pbcn, and consist of the same lantern units. But the lantern units are connected in an anti-parallel way and lithium cations are located in the six-membered rings which have different environment from A1(A3).
A lithium iron titanium phosphate Li1+xTi2-xFex(PO4)3 (x=0.5) (A4, LFTP) with the NASICON structure has been synthesized by sol-gel method and characterized by powder X-ray diffraction. It is found that A4 displays good stability as electrolyte material for lithium battery. The ionic conductivity is
1 x 10-3 S· cm-1 and discharge capacity is 14.6 mAh.

摘要 I
Abstract II
目錄 III
附錄之表目錄 XII
第一章 緒論 1
1-1簡介 1
1-2 論文研究動機 9
1-3 合成方法 10
1-3-1 水熱法 10
1-3-2溶膠-凝膠法 (Sol-Gel Method) 13
1-3-3 藥品一覽表 15
1-4 鑑定方法 16
1-4-1 儀器測量簡介 16
1-4-2 單晶 X 光繞射儀與解構分析 18
1-4-3 粉末 X 光繞射儀 (PXRD) 24
1-4-4 X光螢光光譜儀 (XRF) 25
1-4-5感應耦合電漿放射光譜儀 ( ICP-OES ) 26
1-4-6穆斯堡爾光譜儀 (MössbauerSpectroscopy) 27
1-5研究成果摘要 33
2-1 簡介 34
2-2 實驗部分 39
2-2-1 LiTi2(PO4)3 (A1)合成條件 39
2-2-2 Li1+xTi2-xFex(PO4)3 (x=0.8) (A2) 合成條件 40
2-2-3 Li1+xTi2-xFex(PO4)3 (A3) 合成條件 41
2-2-4 Li1+xTi2-xFex(PO4)3 (x=0.5) (A4) 合成條件 43
2-2-5 LiTi2(PO4)3 (A1) 單晶X光結構解析 45
2-2-6 Li1+xTi2-xFex(PO4)3 (x=0.8) (A2) 單晶X光結構解析 46
2-2-7 Li1+xTi2-xFex(PO4)3 (A3) 單晶X光結構解析 48
2-2-8 陰極材料及複合電解質膜製作 50
取鋰鈷氧 ( LiCoO2)、聚氟化二乙烯 ( polyvinylidene fluoride, PVDF)、 50
2-3結果與討論 54
2-3-1 LiTi2(PO4)3 (A1) 結構描述 54
2-3-2 Li1+xTi2-xFex(PO4)3 (x=0.8) (A2) 結構描述 57
2-3-3 Li1+xTi2-xFex(PO4)3 (A3) 結構描述 61
2-3-4 粉末 X 光繞射分析 68
2-3-5 X光螢光光譜分析 (XRF) 72
2-3-6 感應耦合電漿放射光譜儀分析 ( ICP-OES) 74
2-3-7 Mössbauer光譜儀分析 75
2-3-8 複合電解質膜之導電度及耐電壓量測 79
2-3-9 複合電解質膜之耐電壓量測 81
2-3-10 電容量引出率測試 82
2-3-11 不可逆電容量測試 85
第三章 結論 88
參考文獻 90
附錄 92

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