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系統識別號 U0002-0508201013080100
中文論文名稱 (A,Li)2Ti2O7 (A = Y、Gd) 固態電解質的製備與離子導電性研究
英文論文名稱 Preparation and ionic conductivity of (A,Li)2Ti2O7 (A = Y, Gd) solid electrolyte
校院名稱 淡江大學
系所名稱(中) 化學學系碩士班
系所名稱(英) Department of Chemistry
學年度 98
學期 2
出版年 99
研究生中文姓名 謝欣諭
研究生英文姓名 Shin-Yu Shieh
學號 697160603
學位類別 碩士
語文別 中文
口試日期 2010-07-20
論文頁數 93頁
口試委員 指導教授-高惠春
委員-黃炳照
委員-許火順
中文關鍵字 固態電解質  焦綠石結構  離子導體 
英文關鍵字 solid state electrolyte  pyrochlore structure  ionic conductivity  lithium ion  solid oxide fuel cell  crystal structure 
學科別分類 學科別自然科學化學
中文摘要 (A2-xLix)Ti2O7-x (A1LT, x = 0.04 – 0.11) (A = Y、Gd),兩系列樣品分別在1150和1250 oC下燒結10 h。比較A1LT和 A2-xTi2O7 (AT)系列樣品的晶胞參數,發現在相同取代量x的情況下,A1LT系列的晶胞參數會大於AT系列的晶胞參數,這表示Li+成功的取代至A1LT樣品A site的位子。利用添加兩倍的Li2O至A1LT系列樣品,即為(A2-xLi3x)Ti2O7 (A3LT)系列,A3LT與A1LT在相同取代量x的條件下,會有相同的晶胞參數。因此,添加額外的Li2O可當作助熔劑的功用,藉由固態共熔點的產生而降低A3LT樣品的熔點,使A3LT材料獲得改善,且有較大的晶粒。添加Li2O當助熔劑至A1LT系列樣品和燒結時的溫度控制,可使(A2-xLix)Ti2O7-x (A1LT, x = 0.04 – 0.11) (A = Y 、Gd)系列在相同的燒結溫度(分別為1150和1250 oC 10 h),樣品的相對緻密度均在90 % 以上。Y3LY系列中取代量為x = 0.06樣品在700 ℃時的導電度時為4.07 × 10-4S.cm-1;而根據報導指出,相較於Y2Ti2O7樣品在700度C的導電度為2.03X10-4S.cm-1,卻要以1600度C燒結。
英文摘要 Two series of (A2-xLix)Ti2O7-x (A1LT, x = 0.04 – 0.11) with A = Y and Gd were sintered at 1150 and 1250 oC respectively for 10 h in the static air atmosphere. Unit cell a-axis of the A1LT is longer than that of the A2-xTi2O7 (AT) with the same amount of x and the same A site cation, indicating a successful substitution of the Li+ ion into the A site of A1LT. Addition of extra Li2O (2x) into A1LT, the nominal composition becomes (A2-xLi3x)Ti2O7 (A3LT), which has the same unit cell a-axis as A1LT with the same amount of x. Therefore, the extra Li2O added in the A3LT is probably acting as a self flux to lower the melting point of the mixture. As a result, materials become more compact and grains grow bigger. Adding Li2O as a flux and the heating history is carefully controlled, compact samples of (A2-xLix)Ti2O7-x (A1LT, x = 0.04 – 0.11) with A = Y and Gd with relative density higher than 90% can be obtained at a temperature as low as 1150C and 1250C respectively. One compound of Y3LT with x=0.06 prepared at 1150C had an AC conductivity of 4.07 x10-4S/cm at 700C, the ionic conductivity is comparable to a Y2Ti2O7 prepared at 1600C that is 2.03x10-4 S/cm reported.
論文目次 目 錄
目錄І
圖索引Ⅲ
表索引Ⅸ
第一章 緒論1
1-1 固體氧化物燃料電池(Solid Oxide Fuel Cell)1
1-2 固態電解質4
1-3 氧離子導體10
1-4 常用的固態氧化物電解質材料11
1-5 研究動機及目的12
第二章 實驗13
2-1 藥品13
2-2 實驗流程14
2-3 樣品的物性分析14
2-3-1 X-光粉末繞射圖譜鑑定15
2-3-2 Rietveld精算法17
2-3-3 掃描式電子顯微鏡19
2-3-5 X-光吸收近邊緣光譜21
第三章 結果與討論.............................
22
3-1 樣品單相鑑定.....................................
26
3-2 結構分析.........................................
42
3-3掃描式電子顯微鏡(SEM).............................
54
3-4樣品緻密度........................................
57
3-5交流阻抗分析(Ac Impedance) .........................
84
3-6 X-光吸收近邊緣光譜.................................
87
第四章 結論與未來計畫88
4-1 結論89
4-2 未來計畫89
參考文獻91
圖 索 引
圖1-1
SOFC簡單示意圖............................
2
圖1-2
1/8焦綠石的單位晶胞結構....................
4
圖1-3
氯化鈉結構示意圖...........................
4
圖1-4
螢石單位晶胞................................
6
圖1-5
ABO3 的結構................................
8
圖1-6
焦綠石的單位晶胞結構........................
9
圖1-7
Ln2Zr2O7 (Ln = La、Nd、Sm、Eu、Gd、Y、Yb)焦綠石結構導電度..............................
10
圖2-1
AUTOLAB PGSTAT30交流阻抗分析量測示意圖..
19
圖3-1
Y2-xLi3xTi2O7 (Y3LT), (x = 0.04 – 0.11) X-光繞射圖譜
23
圖3-2
Y2-xLixTi2O7-x (Y1LT), (x = 0.04 – 0.11) X-光繞射圖譜.........................................
23
圖3-3
Y2-xTi2O7-3x/2(YT), (x = 0.04 – 0.11) X-光繞射圖譜..
24
圖3-4
Y2-xLi3xTi2O7(Y3LT), (x = 0.11)X-光繞射圖譜....
24
圖3-5
Gd2-xLi3xTi2O7 (G3LT), (x = 0.04 – 0.11) X-光繞射圖譜.........................................
25
圖3-6
Gd2-xLixTi2O7-x (G1LT), (x = 0.04 – 0.11) X-光繞射圖譜.........................................
25
IV
圖3-7
Gd2-xTi2O7-3x/2(GT), (x = 0.04 – 0.11) X-光繞射圖譜.
26
圖3-8
Y2-xLi3xTi2O7 (Y3LT), (x = 0.04)樣品的精算結果....
28
圖3-9
Y2-xLi3xTi2O7 (Y3LT), (x = 0.08)樣品的精算結果....
28
圖3-10
Y2-xLi3xTi2O7 (Y3LT), (x = 0.11)樣品的精算結果....
29
圖3-11
Y2-xLixTi2O7-x (Y1LT), (x = 0.04)樣品的精算結果...
29
圖3-12
Y2-xLixTi2O7-x (Y1LT), (x = 0.08)樣品的精算結果...
30
圖3-13
Y2-xLixTi2O7-x (Y1LT), (x = 0.11)樣品的精算結果...
30
圖3-14
Y2-xTi2O7-3x/2(YT), (x = 0.04)樣品的精算結果......
31
圖3-15
Y2-xTi2O7-3x/2(YT), (x = 0.08)樣品的精算結果......
31
圖3-16
Y2-xTi2O7-3x/2(YT), (x = 0.11)樣品的精算結果......
32
圖3-17
Gd2-xLi3xTi2O7 (G3LT), (x = 0.04)樣品的精算結果...
32
圖3-18
Gd2-xLi3xTi2O7 (G3LT), (x = 0.08)樣品的精算結果...
33
圖3-19
Gd2-xLi3xTi2O7 (G3LT), (x = 0.11)樣品的精算結果...
33
圖3-20
(Gd2-xLix)Ti2O7-x (G1LT), (x = 0.04)樣品的精算結果.
34
圖3-21
(Gd2-xLix)Ti2O7-x (G1LT), (x = 0.08)樣品的精算結果.
34
圖3-22
(Gd2-xLix)Ti2O7-x (G1LT), (x = 0.11)樣品的精算結果.
35
圖3-23
Gd2-xTi2O7-3x/2(GT), (x = 0.04)樣品的精算結果.....
35
圖3-24
Gd2-xTi2O7-3x/2(GT), (x = 0.08)樣品的精算結果.....
36
圖3-25
Gd2-xTi2O7-3x/2(GT), (x = 0.11)樣品的精算結果.....
36
圖3-26
(a) Y3LT、Y1LT、YT系列,取代量對晶格參數作圖(b) Y1LT、YT系列原子體積對晶格體積作圖..
42
圖3-27
(a) G3LT、G1LT、GT系列,取代量對晶格參數作圖(b) G1LT、GT系列原子體積對晶格體積作圖..
42
圖3-28
Y2-xTi2O7-3x/2 (YT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.08, (c) x = 0.11................
45
圖3-29
Gd2-xTi2O7-3x/2 (GT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.08, (c) x = 0.11..............
46
圖3-30
Y2-xLixTi2O7-x (Y1LT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.05, (c) x = 0.06, (d) x = 0.07.
47
圖3-31
Y2-xLixTi2O7-x (Y1LT)樣品放大倍率5000倍的SEM圖(a) x = 0.08, (b) x = 0.09, (c) x = 0.10, (d) x = 0.11.
48
圖3-32
Gd2-xLixTi2O7-x (G1LT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.05, (c) x = 0.06, (d) x = 0.07.
49
圖3-33
Gd2-xLixTi2O7-x (G1LT)樣品放大倍率5000倍的SEM圖(a) x = 0.08, (b) x = 0.09, (c) x = 0.10, (d) x = 0.11.
50
圖3-34
Y2-xLi3xTi2O7 (Y3LT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.05, (c) x = 0.06, (d) x = 0.07...
51
圖3-35
Y2-xLi3xTi2O7 (Y3LT)樣品放大倍率5000倍的SEM圖(a) x = 0.08, (b) x = 0.09, (c) x = 0.10, (d) x = 0.11...
52
圖3-36
Gd2-xLi3xTi2O7 (G3LT)樣品放大倍率5000倍的SEM圖(a) x = 0.04, (b) x = 0.05, (c) x = 0.06, (d) x = 0.07.
53
圖3-37
Gd2-xLi3xTi2O7 (G3LT)樣品放大倍率5000倍的SEM圖(a) x = 0.08, (b) x = 0.09, (c) x = 0.10, (d) x = 0.11.
54
圖3-38
Y3LT、YLT取代量對相對緻密度作圖...........
56
圖3-39
G3LT、GLT取代量對相對緻密度作圖...........
57
圖3-40
Y3LT (x =0.04)在450 oC~550 oC時的交流阻抗圖...
60
圖3-41
Y3LT (x =0.04)在300 oC-700 oC時的交流阻抗圖...
60
圖3-42
Y3LT (x =0.05)在450 oC~550 oC時的交流阻抗圖...
61
圖3-43
Y3LT (x =0.05)在300 oC-700 oC時的交流阻抗圖...
61
圖3-44
Y3LT (x =0.06)在450 oC~550 oC時的交流阻抗圖...
62
圖3-45
Y3LT (x =0.06)在300 oC-700 oC時的交流阻抗圖...
62
圖3-46
Y3LT (x =0.07)在450 oC~550 oC時的交流阻抗圖...
63
圖3-47
Y3LT (x =0.07)在300 oC-700 oC時的交流阻抗圖...
63
圖3-48
Y3LT (x =0.08)在450 oC~550 oC時的交流阻抗圖...
64
圖3-49
Y3LT (x =0.08)在300 oC-700 oC時的交流阻抗圖...
64
圖3-50
Y3LT (x =0.09)在450 oC~550 oC時的交流阻抗圖...
65
圖3-51
Y3LT (x =0.09)在300 oC-700 oC時的交流阻抗圖...
65
圖3-52
Y3LT (x =0.10)在450 oC~550 oC時的交流阻抗圖...
66
圖3-53
Y3LT (x =0.10)在300 oC-700 oC時的交流阻抗圖...
66
圖3-54
Y3LT (x =0.11)在450 oC~550 oC時的交流阻抗圖...
67
圖3-55
Y3LT (x =0.11)在300 oC-700 oC時的交流阻抗圖...
67
圖3-56
Y3LT (x =0.04)在300 oC時交流阻抗圖譜的等效電路圖........................................
68
圖3-57
Y3LT (x =0.04)在500 oC時交流阻抗圖譜的等效電路圖........................................
69
圖3-58
Y3LT (x =0.04)在300 oC–700 oC 時的相位角......
70
圖3-59
Y3LT (x =0.05)在300 oC–700 oC 時的相位角......
70
圖3-60
Y3LT (x =0.06)在300 oC–700 oC 時的相位角......
71
圖3-61
Y3LT (x =0.07)在300 oC–700 oC 時的相位角......
71
圖3-62
Y3LT (x =0.08)在300 oC–700 oC 時的相位角......
72
圖3-63
Y3LT (x =0.09)在300 oC–700 oC 時的相位角......
72
圖3-64
Y3LT (x =0.10)在300 oC–700 oC 時的相位角......
73
圖3-65
Y3LT (x =0.11)在300 oC–700 oC 時的相位角......
73
圖3-66
Y3LT (x = 0.04-0.11)系列在700 oC測量下晶粒、晶界和整體導電度取對數作圖...................
77
圖3-67
Y3LT系列相對緻密度與在700oC時測得的整體導電度作圖 電度作圖..................................
77
圖3-68
Y3LT(x=0.04-0.11)系列300oC-700 oC 晶粒導電度Arrhenius圖.................................
78
圖3-69
Y3LT(x=0.04-0.11)系列300oC-700 oC 晶界導電度Arrhenius圖.................................
79
圖3-70
Y3LT(x=0.04-0.11)系列300oC-700 oC 整體導電度Arrhenius圖.................................
80
圖3-71
log σgT對1000/T作圖晶粒的活化能與取代量關係.
82
圖3-72
log σgb.T對1000/T作圖晶界的活化能與取代量關係
82
圖3-73
log σtT對1000/T作圖整體的活化能與取代量關係.
82
圖3-74
log σg對1000/T作圖晶粒的活化能與取代量關係..
84
圖3-75
log σgb.對1000/T作圖晶界的活化能與取代量關係..
84
圖3-76
log σt對1000/T作圖晶粒的活化能與取代量關係...
84
圖3-77
Y3LT和G3LT系列樣品Ti K-edge XANES光譜圖
86
圖3-78
Y3LT和G3LT系列樣品與Ti2O3和TiO2 rutile做標準物比較Ti氧化態改變的情形.................
87


表 索 引
表1-1
Bi2O3各結晶相在不同溫度下的導電度.........
7
表2-1
固態球磨法所用到的藥品....................
13
表3-1
Y3LT和Y1LT系列的空間結構與原子位置.....
37
表3-2
YT系列的空間結構與原子位置...............
37
表3-3
G3LT和G1LT系列的空間結構與原子位置.....
38
表3-4
GT系列的空間結構與原子位置...............
38
表3-5
Y3LT系列Rietveld精算的晶格參數與座標整理.
39
表3-6
Y1LT系列Rietveld精算的晶格參數與座標整理.
39
表3-7
YT系列Rietveld精算的晶格參數與座標整理...
40
表3-8
G3LT系列Rietveld精算的晶格參數與座標整理.
40
表3-9
G1LT系列Rietveld精算的晶格參數與座標整理.
41
表3-10
GT系列Rietveld精算的晶格參數與座標整理...
41
表3-11
Y3LT(x = 0.04–0.11)系列樣品添加額外Li2O的重量百分比. ...............................
57
表3-12
G3LT(x = 0.04–0.11)系列樣品添加額外Li2O的重量百分比. .................................
57
表3-13
Y3LT系列300 oC-700 oC所使用的等效電路{1:R1Q1R2Q2 ;2:R1(R2Q2)} .................
74
表3-14
Y3LT (x = 0.04) 300oC-700oC導電度測量結果(L = 0.114 cm, A = 0.798 cm3) ...................
74
表3-15
Y3LT (x = 0.05) 300oC-700oC導電度測量結果(L = 0.075 cm, A = 0.846 cm3) ...................
74
表3-16
Y3LT (x = 0.06) 300oC-700oC導電度測量結果(L = 0.070 cm, A = 0.795cm3) ...................
75
表3-17
Y3LT (x = 0.07) 300oC-700oC導電度測量結果(L = 0.112 cm, A = 0.789 cm3) ...................
75
表3-18
Y3LT (x = 0.08)300oC-700oC導電度測量結果(L = 0.084 cm, A = 0.793cm3) .....................
76
表3-19
Y3LT (x = 0.09)300oC-700oC導電度測量結果(L = 0.093 cm, A = 0.789cm3) .....................
76
表3-20
Y3LT (x = 0.10)300oC-700oC導電度測量結果(L = 0.075 cm, A = 0.846cm3) .....................
76
表3-21
Y3LT (x = 0.11)300oC-700oC導電度測量結果(L = 0.153 cm, A = 0.874cm3) .....................
81
表3-22
Y3LT (x=0.04-0.11)系列log σgT對1000/T作圖晶粒的活化能................................
81
表3-23
Y3LT (x=0.04-0.11)系列log σgb.T對1000/T作圖晶界的活化能................................
81
表3-24
Y3LT (x=0.04-0.11)系列log σtT對1000/T作圖整體的活化能................................
83
表3-25
Y3LT (x=0.04-0.11)系列log σg對1000/T作圖的活化能......................................
83
表3-26
Y3LT (x=0.04-0.11)系列log σgb.對1000/T作圖晶界的活化能...............................
83
表3-27
Y3LT (x=0.04-0.11)系列log σt對1000/T作圖整體的活化能.................................83
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