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研究生:嚴豐年
研究生(外文):Feng-Nien Yen
論文名稱:Cu摻雜至La0.8Sr0.2CuxMn1-xO3 (LSCxM,x=0.1、0.2、0.3) 作為中低溫SOFC陰極之可行性研究
論文名稱(外文):On the copper doping of La0.8Sr0.2MnO3 (LSM) cathode for IT-SOFCs
指導教授:林景崎
指導教授(外文):Jing-Chie Lin
學位類別:碩士
校院名稱:國立中央大學
系所名稱:材料科學與工程研究所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2019
畢業學年度:107
語文別:中文
論文頁數:118
中文關鍵詞:固態氧化物燃料電池燃燒合成法LSM陰極材料銅摻雜
外文關鍵詞:Solid oxide fuel cell(SOFC)Lanthanum-strontium- manganese-oxideCopper doping
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本研究使用甘胺酸-硝酸鹽燃燒合成法製備具有鈣鈦礦結晶結構(La0.8Sr0.2MnO3;LSM,La0.8Sr0.2CuxMn1-xO3 x=0.1、0.2、0.3;LSC1M;LSC2M;LSC3M)之陰極粉末。探討前驅硝酸鹽溶液經由調整不同pH值,甘胺酸硝酸比(g/n ratio),以及初生粉體在不同煆燒溫度(800、900、1000、1100 ℃)之結晶結構、形貌、熱機械性質等,再利用最好之參數製成固態氧化物燃料電池(SOFC),進行電化學測試。經由X光繞射分析結晶結構以及掃描式電子顯微鏡觀察表面微結構,發現在pH=3、4以及g/n=1.00、1.25有最完整之特徵峰以及粉體形貌,由熱膨脹分析發現LSM4/1.25與電解質BCZY之熱膨脹係數最為相近;導電度可達495.38 S/cm,進行性能測試結果顯示在操作溫度800℃擁有最高之功率密度:41.8 mW/cm2,而摻雜銅進入LSM之實驗發現,導電度分析在LSC2M有最高之導電度提升,由495.38 S/cm提升到858.26 S/cm,進行性能結果測試發現LSM4/1.25摻雜銅取代錳有效能60%之提升,在操作溫度700℃從22.33 mW/cm2提升到37.20 mW/cm2,EIS實驗發現極化阻抗Rp下降了4.55 Ωcm2。
In this study, the nanostructured perovskite La0.8Sr0.2MnO3 (LSM) and La0.8Sr0.2Mn1-xCuxO3 (note as x=0.1; LSC1M, 0.2; LSC2M, 0.3; LSC3M) prepared by the glycine-nitrate combustion synthesis method were considered as a potential candidate for use as cathode in solid oxide fuel cells (SOFC) operated at intermediate-temperature. In the present work, combustion synthesis method was investigated by adjusting the pH of LSM nitrate solution (pH=2, 3, 4, 5) and ratio between glycine and nitrate (G/N= 0.75, 1.00, 1.25). The crystal structure and morphology of the powders after calcining were analyzed and also its thermal properties and electrochemical characteristic were discussed. The optimal combustion synthesis parameters (pH and G/N) were used to synthesize the LSCxM. Then the crystal structure and electrochemical properties were investigated. Finally, the feasibility for using as cathode in P-SOFC though combining LSM as cathode backbone and doping Cu to replace Mn. The results of LSM analysis showed that LSM1.00/3, LSM1.00/4, LSM1.25/3 and LSM1.25/4 were the optimal parameters for combustion synthesis whose crystal structure and morphology were the most suitable as cathode for SOFC. Among all, LSM1.25/4 was analyzed that its average particle size around 30nm. For the measurement of thermal expansion coefficient (TMA), the coefficient of LSM1.25/4 was about 14.36 × 10-6 K-1 which was the closest to that of electrolyte BCZY. In the results of four-probe DC conductivity measurement, LSM1.25/4 had the highest conductivity near 495.38 S/cm.The performance test results show that the highest power density is 41.8 mW/cm2 at 800 °C, and the experiment of doping copper into LSM found that the conductivity analysis has the highest conductivity increase in LSC2M, from 495.38 S/cm improved to 858.26 S/cm. The performance test showed that the LSM4/1.25 doped 0.2 copper-substituted manganese had a 60% improvement in efficiency, and the operating temperature was increased from 22.33 mW/cm2 to 37.20 mW/cm2 at 700 °C. The resistance Rp drops by 4.55 Ωcm2.
摘要 i
Abstract ii
目錄 v
表目錄 viii
圖目錄 ix
第一章 緒論 1
1-1前言 1
1-2研究動機與目的 2
第二章 實驗原理與文獻回顧 5
2-1燃料電池簡介 5
2-1-1固態氧化物燃料電池原理與簡介 6
2-1-2固態氧化物燃料電池類型 7
2-2固態氧化物電池元件 8
2-2-1電解質(Electrolyte) 8
2-2-2陽極(Anode) 9
2-2-3陰極(Cathode) 9
2-3陰極元件 10
2-3-1陰極傳導機制 10
2-3-2陰極晶體結構 11
2-3-3陰極材料製備方式 13
2-4電化學分析原理 15
2-4-1直流電極化曲線(I-V Curve)原理 16
2-4-2電化學交流阻抗頻譜(EIS)原理 18
2-5文獻回顧 21
2-5-1固態氧化物燃料電池陰極材料 21
2-5-2固態氧化物燃料電池陰極合成法 23
2-5-3 複合陰極製程 24
第三章 實驗方法 25
3-1 實驗原料 25
3-2元件樣品製備、條件與時驗流程 25
3-2-1陰極粉末製備流程 25
3-2-2陰極導電度樣品製備流程 27
3-2-3陰極熱膨脹量測樣品製備流程 27
3-2-4陰極膏製備流程 27
3-2-5電解質製備 28
3-2-6半電池製備 28
3-3分析設備 29
3-3-1 X光晶體繞射儀器(X-Ray diffraction; XRD) 29
3-3-2掃描式電子顯微鏡(Scanning Electron Microscope; SEM) 30
3-3-4比表面積與孔隙分佈分析儀(Specific Surface Area and Porosimetry Analyzer;BET) 31
3-3-5導電度量測 31
3-3-6直流極化曲線測試平台 32
3-3-7電化學交流阻抗頻譜儀 32
第四章 結果 34
4-1X光晶體繞射分析 34
4-1-1LSM之X光繞射圖譜 34
4-1-2LSCxM之X光繞射圖譜 35
4-2LSM陰極表面形貌觀察 35
4-3陰極粉末熱種分析 36
4-4LSM熱膨脹係數分析 36
4-5陰極長碇導電度量測 36
4-5-1LSM之導電度 36
4-5-2LSCxM之導電度 37
4-6直流極化曲線測試分析 37
4-6-1LSM之直流極化曲線 37
4-6-2LSCxM之直流極化曲線 38
4-7電化學交流阻抗頻譜分析 38
4-7-1LSM之交流阻抗頻譜 38
4-7-2LSCxM之交流阻抗頻譜 39
第五章 討論 39
5-1燃燒合成法製備LSM與LSCxM粉末之探討 39
5-1-1LSM 39
5-1-2LSCxM 40
5-2陰極樣品特性分析之探討 41
5-2-1氧空缺 41
5-2-2熱膨脹係數 41
5-2-3導電性 42
5-3全電池性能分析 42
第六章 結論與未來工作 44
6-1結論 44
6-2未來工作 45
參考文獻 46

表目錄
表1- 1目前商用陰極材料[13-16] 50
表2-1 不同種類燃料電池之特性比較 51
表2-2 陰極材料合成法比較 52
表2-3 LSM不同元素比例之熱膨脹係數與測量溫度表 52
表2-4 以不同有機酸作為燃料,進行硝酸鹽燃燒合成法,其燃燒之結果比較 53
表3-1 實驗使用之化學藥劑與材料之廠牌與功用列表 54
表3-2 製備La0.8Sr0.2MnO3 (LSM)所需硝酸鹽水溶液中配置比例 55
表3-3 製備La0.8Sr0.2Mn0.9Cu0.1O3 (LSC1M)所需硝酸鹽水溶液中配置比例 55
表3-4 製備La0.8Sr0.2Mn0.8Cu0.2O3 (LSC2M)所需硝酸鹽水溶液中配置比例 56
表3-5 製備La0.8Sr0.2Mn0.7Cu0.3O3 (LSC3M)所需硝酸鹽水溶液中配置比例 56
表3-6 LSM、LSCxM初生粉末煆燒條件 57
表3-7 陰極膏配製比例 57
表3-8 電解質BaCe0.6Zr0.2Y0.2O3 (BCZY)配方比例 57
表3-9 BCZY電解質粉末煆燒條件 58
表3-10 BCZY電解質基板燒結條件 58
表3-11 LSM、LSCxM陰極膏燒結條件 58
表3-12 白金膏燒結條件 58
表3-13 LSM與LSCxM陰極粉末熱重分析(TGA)之實驗溫度設定 59
表4-1 LSM1.00、LSM1.25粉末樣品經1100°C煆燒後之半高寬(FWHM) 59
表4-2 LSM1.00/3、LSM1.00/4、LSM1.25/3與LSM1.25/4粉末樣品經1100°C煆燒後之比表面積(BET) 59
表4-3 LSM1.00/3、LSM1.00/4、LSM1.25/3與LSM1.25/4粉末樣品經1200°C燒結後之熱重分析(TGA) 60
表4- 4 LSM1.00/3、LSM1.00/4、LSM1.25/3與LSM1.25/4陰極最高功率密度(單位: mW/cm2) 60
表4- 5 LSCxM陰極最高功率密度(單位: mW/cm2) 60
表4- 6 LSM1.25/3與LSC2M-1.25/3銅摻雜陰極最高功率密度(單位: mW/cm2) 61
表4- 7 LSM1.00/3、LSM1.00/4、LSM1.25/3與LSM1.25/4半電池之歐姆阻抗Rohm、極化阻抗Rp及總阻抗Rt (單位: Ωcm2) 61
表4- 8 LSCxM半電池之歐姆阻抗Rohm、極化阻抗Rp及總阻抗Rt (單位: Ωcm2) 61
圖目錄
圖1- 1固態氧化物燃料電池理論計算所得與實際測量所得之面積比電阻隨操作溫度之變化情形,其中包含電池元件(陰極、電解質、陽極)與擴散之對面積比電阻 62
圖2- 1燃料電池種類及其工作環境與能源堆疊規模圖 62
圖2- 2燃料電池運作示意圖 63
圖2- 3 O-SOFC與P-SOFC傳導機制比較圖 63
圖2- 4平版型SOFC及其封裝架設 64
圖2- 5鈕扣型SOFC及其封裝架設 64
圖2- 6 SOFC電池支撐類型示意圖 65
圖2- 7陰極材料傳導類型(a)電子導體;(b)電子離子混合導體;(c)電子質子混合導體;(d)電子、質子與離子混合導體 65
圖2- 8 SOFC之三相界示意圖 66
圖2- 9以La0.6Sr0.4MnO3-δ作說明之三相界示意圖 66
圖2- 10鈣鈦礦結構示意圖 67
圖2- 11A、B位元素離子半徑對於鈣鈦礦結構之偏差影響 67
圖2- 12可應用在鈣鈦礦A、B位置的元素 68
圖2- 13 Ruddlesden-Popper(RP)層狀結構示意圖 68
圖2- 14理想與實際狀況之燃料電池直流極化曲線 69
圖2- 15電化學交流阻抗頻譜之施加電壓與電流回饋關係示意圖 69
圖2- 16正弦電壓擾動與正弦電流響應關係示意圖 70
圖2- 17交流阻抗Nyquist示意圖 70
圖2- 18等效電路模型示意圖 71
圖2- 19 Nd0.6Sr0.4Co0.8M0.2O3-δ(M=Ti、Cr、Mn、Fe、Co、Cu)在空氣氣氛下之氧空缺變化量 71
圖2- 20 Nd0.6Sr0.4Co0.8M0.2O3-δ(M=Ti、Cr、Mn、Fe、Co、Cu)在空氣氣氛下之導電度量測 72
圖2- 21 Nd0.6Sr0.4Co0.8M0.2O3-δ(M=Ti、Cr、Mn、Fe、Co、Cu)單電池在800°C下之直流極化曲線(陽極為Ni-GDC、電解質為LSGM) 72
圖2- 22以不同有機酸作為燃燒法燃料合成Ni0.5Zn0.5Fe2O4陶瓷粉末之XRD圖譜 73
圖2- 23甘胺酸-硝酸鹽燃燒法合成Ba0.5Sr0.5Co0.8Fe0.2O3,不同G/n比(a)0.25、(b)0.56、(c)0.84之XRD圖譜 73
圖2- 24甘胺酸在不同酸鹼值之硝酸鹽水溶液中,經燃燒法生成之粉末經1000°C煆燒5h後之XRD圖譜 74
圖2- 25固態反應法與燃燒合成法合成CuCrO2之BET吸附曲線比較圖 74
圖2- 26以LSM與YSZ製成電子離子混合導體之複合陰極示意圖 75
圖3- 1實驗架構圖 76
圖3- 2甘胺酸-硝酸鹽燃燒合成法粉末製備流程 77
圖3- 3長方形樣品之模具 78
圖3- 4圓形小碇樣品之模具 79
圖3- 5電解質BCZY粉末之XRD 79
圖3-6 圓形電解質基板之模具 80
圖3-7 四點式導電性量測示意圖 80
圖3-8 SOFC量測平台內部示意圖 81
圖4-1 燃燒法初生LSM粉末之XRD 81
圖4-2燃燒法初生LSM粉末與此粉末經不同溫度煆燒後所得之XRD圖譜 82
圖4-3 改變燃燒法製程參數(硝酸鹽溶液pH控制在2, 3, 4, 5;而 83
圖4-4 LSCxM (x = 0.1, 0.2, 0.3)粉末經1100°C煆燒2h後之XRD疊圖 84
圖4-5 控制燃燒法製程參數G/N固定在0.75,硝酸鹽溶液pH值分別在(a)2, (b) 3,(c) 4,(d) 5所得初生粉末,再經1100°C煆燒2h後之LSM0.75/2, LSM0.75/3, LSM0.75/4, LSM0.75/5樣品表面形貌,放大倍率為50000倍 85
圖4- 6控制燃燒法製程參數G/N固定在1.00,硝酸鹽溶液pH值分別在(a)2, (b) 3,(c) 4,(d) 5所得初生粉末,再經1100°C煆燒2h後之LSM1.00/2, LSM1.00/3, LSM1.00/4, LSM1.00/5樣品表面形貌,放大倍率為50000倍 86
圖4- 7 控制燃燒法製程參數G/N固定在1.25,硝酸鹽溶液pH值分別在(a)2, (b) 3,(c) 4,(d) 5所得初生粉末,再經1100°C煆燒2h後之LSM1.25/2, LSM1.25/3, LSM1.25/4, LSM1.25/5樣品表面形貌,放大倍率為50000倍 87
圖4- 8 燒結過之陰極(LSM1.25/4)與電解質(BCZY)介面處,放大倍率為50K 88
圖4- 9LSM1.00/3、LSM1.00/4、LSM1.25/3、LSM1.25/4陰極粉末經1100°C燒結1h後之熱重分析圖 88
圖4- 10LSM1.00/3、LSM1.00/4、LSM1.25/3、LSM1.25/4陰極樣品之熱膨脹係數對溫度作圖 89
圖4- 11LSM1.00/3、LSM1.00/4、LSM1.25/3、LSM1.25/4陰極樣品之導電度對溫度作圖 89
圖4- 12 LSC1M、LSC2M與LSC3M陰極樣品之導電度對溫度作圖 90
圖4- 13 Pt|BCZY(450µm)|LSM1.00/3在不同操作溫度下之直流極化曲線 90
圖4- 14 Pt|BCZY(450µm)|LSM1.00/4在不同操作溫度下之直流極化曲線 91
圖4- 15 Pt|BCZY(450µm)|LSM1.25/3在不同操作溫度下之直流極化曲線 91
圖4-16 Pt|BCZY(450µm)|LSM1.25/4在不同操作溫度下之直流極化曲線 92
圖4- 17 Pt|BCZY(450µm)|LSC1M在不同操作溫度下之直流極化曲線 92
圖4- 18 Pt|BCZY(450µm)|LSC2M在不同操作溫度下之直流極化曲線 93
圖4- 19 Pt|BCZY(450µm)|LSC3M在不同操作溫度下之直流極化曲線 93
圖4- 20 Pt|BCZY(450µm)|LSM1.25/3 (Pristine)、Pt|BCZY(450µm)|LSC2M (doped)在800°C之直流極化曲線比較 94
圖4- 21 Pt|BCZY(450µm)|LSM1.25/3 (Pristine)、Pt|BCZY(450µm)|LSC2M (doped)在700°C之直流極化曲線比較 94
圖4- 22 Pt|BCZY(450µm)|LSM1.25/3 (Pristine)、Pt|BCZY(450µm)|LSC2M (doped)在600°C之直流極化曲線比較 95
圖4- 23 本研究所使用之等效電路模型圖 95
圖4- 24 Pt|BCZY(450µm)|LSM1.00/3在不同操作溫度下之交流阻抗頻譜 96
圖4- 25 Pt|BCZY(450µm)|LSM1.25/3在不同操作溫度下之交流阻抗頻譜 96
圖4- 26 Pt|BCZY(450µm)|LSM1.25/4在不同操作溫度下之交流阻抗頻譜 97
圖4- 27 Pt|BCZY(450µm)|LSC1M在不同操作溫度下之交流阻抗頻譜 97
圖4- 28 Pt|BCZY(450µm)|LSC2M在不同操作溫度下之交流阻抗頻譜 98
圖4- 29 Pt|BCZY(450µm)|LSC3M在不同操作溫度下之交流阻抗頻譜 98
圖4- 30 Pt|BCZY(450µm)|LSM1.25/3 (Pristine)、Pt|BCZY(450µm)|LSC2M-1.25/3 (Doped)在不同操作溫度下之交流阻抗頻譜比較 99
圖5- 1 LSM1.00/3、LSM1.25/3與LSM1.25/4陰極阻抗在操作溫度800°C下之比較圖 99
圖5- 2 LSM1.00/3、LSM1.25/3與LSM1.25/4陰極阻抗在操作溫度700°C下之比較圖 100
圖5- 3 LSM1.00/3、LSM1.25/3與LSM1.25/4陰極阻抗在操作溫度600°C下之比較圖 100
圖5- 4 LSC1M、LSC2M與LSC3M陰極阻抗在操作溫度800°C下之比較圖 101
圖5-5 LSC1M、LSC2M與LSC3M陰極阻抗在操作溫度700°C下之比較圖 101
圖5-6 LSC1M、LSC2M與LSC3M陰極阻抗在操作溫度600°C下之比較圖 102
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