研究生: |
黃慧婷 Huei-Ting Huang |
---|---|
論文名稱: |
以常壓電漿噴射束製備鑭鍶錳氧化物固態燃料電池陰極材料之研究 The Study of La0.5Sr0.5MnO3 as SOFC Cathode by Atmospheric Pressure Plasma Jet |
指導教授: |
郭俞麟
Yu-Lin Kuo |
口試委員: |
周宏隆
Hung-lung Chou 施劭儒 Shao-ju Shih 韋文誠 Wen-cheng Wei |
學位類別: |
碩士 Master |
系所名稱: |
工程學院 - 機械工程系 Department of Mechanical Engineering |
論文出版年: | 2015 |
畢業學年度: | 103 |
語文別: | 中文 |
論文頁數: | 113 |
中文關鍵詞: | 常壓電漿噴射束 、固態氧化物燃料電池 、鑭鍶錳氧化物 |
外文關鍵詞: | Atmospheric Pressure Plasma Jet, Solid Oxide Fuel Cell, Strontium-doped Lanthanum Manganite |
相關次數: | 點閱:185 下載:2 |
分享至: |
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本研究利用常壓電漿噴射束系統(Atmospheric pressure plasma jet, APPJ)製備三元鑭鍶錳氧化物(La0.5Sr0.5MnO3, LSM)之奈米顆粒,應用於固態氧化物燃料電池之陰極端。實驗以硝酸鑭、硝酸鍶與硝酸錳混合水溶液作為前驅物來源,結合噴霧熱解法與電漿噴塗法製程之特性製備出其材料。本研究之架構主要分為二大部分,第一部分以粉體之製備為主,藉由氧氣載氣氣體將前驅物通入電漿束口製備出LSM粉體後,分別以X光繞射儀(XRD)分析其熱處理前後之結晶性質、以全反射X光螢光分析儀(TXRF)鑑定其化學成分、雷射粒徑分析(DLS)確定其顆粒尺寸大小,並以掃描式電子顯微鏡(SEM)與穿透式電子顯微鏡(TEM)觀察其表面形貌與微結構。由實驗結果顯示,剛沉積之LSM粉體之表面形貌為接近球狀之中空奈米顆粒,經由1000℃燒結後其相結構鑑定確認為La0.5Sr0.5MnO3晶體,粒徑大小約40nm,其化學成分分析結果也指出經由電漿製程所製備出的LSM與起始所配置之前驅物溶液摻雜比例結果一致。此外亦可推測LSM粉體之顆粒成形機制為溶質過飽和在表面先行析出固相(surface precipitation),產生的中空球狀顆粒隨著熱處理中之燒結聚集效應使得球殼開始塌陷,同時伴隨著氧化反應最後形成多孔之鑭鍶錳氧化物顆粒。第二部分以常壓電漿噴射束沉積LSM薄膜於8YSZ碇材,同樣以O2為載氣氣體,以不同噴塗距離之電漿參數探討對薄膜品質之影響,最後針對LSM鍍層進行電化學分析,以建立常壓電漿噴射束製備多孔陰極薄膜之目標,期望能應用於SOFC之固態陰極材料上。實驗結果顯示,在電漿功率500W、乾燥空氣30 slm、載氣氣體1slm搭配噴塗距離為25mm時,有較多孔隙結構。本研究之電化學分析結果顯示,對稱式半電池(LSM/YSZ/LSM)在操作溫度600~900°C空氣氣氛下,其最大交換電流密度約為65.2 mA/cm2;交流阻抗分析結果也顯示,LSM粗糙的多孔性表面會造成電雙層(Double layer)現象。氫氣氣氛下非對稱式半電池(LSM/YSZ/Pt)發電功率(Power density)之輸出大小約為46 mW/cm^2,換算其ASR值約5.72 Ωcm-2,整體電位輸出介於0.94~1.01 V之間。由上述結果可知,本研究可透過常壓電將噴射束成功製備出LSM薄膜應用於固態氧化物燃料電池之陰極材料。
Strontium-doped lanthanum manganite La1-xSrxMnO3-δ (LSM) has been widely used as a cathode for SOFC, because of its excellent thermal and chemical compatibility with the YSZ electrolyte. However, its catalytic activity is inadequate for low-temperature applications. In order to improve its electrochemical performance and understand the detailed mechanism of oxygen reduction reaction (ORR) at cathode side, novel atmospheric pressure plasma jet (APPJ) process was applied to synthesize LSM cathode materials via precursor solutions of nitrate salts. A modified method combines the atomization process of spray pyrolysis and plasma enhanced chemical vapor deposition technology. Our research group has successfully synthesized the ZrO2, CeO2 and Gd2O3 doped CeO2 (GDC) by this APPJ fabrication. Now we are focus on the he preparation of ternary-metal oxide, La1-xSrxMnO3 as SOFC cathode materials.
In this study, two topics are discussed. First one is the synthesis of LSM particles. XRD results show well-crystalline structure of perovskite La0.5Sr0.5MnO3, while the grain size increased to 40 nm as the sintering temperature increased to 1000℃. The microstructure of LSM was found to be hollow and porous particles by SEM and TEM. The chemical compositions of LSM particles after APPJ process analyzed by TXRF were close to 0.5:0.5:1 for average atomic ratios (La:Sr:Mn) which was the same as the prepared nitrate solution. The results showed that the feasibility of preparation of well-crystallized La0.5Sr0.5MnO3 particles by APPJ system was successfully achieved.
The second part is the investigation of LSM film deposition by changing the distance between nozzle and substrate. The optimal plasma parameters for obtaining LSM film as cathode layer are the distance of 25 mm and applied power at 500 W. The morphology of 1000℃-sintered LSM films represented interconnected particles with near spherical shape and a porosity of 37.8%.
About the electrochemical performance of LSM half cell was measured by two-probe electrode method. The highest exchange current density of symmetric half cell (LSM/YSZ/LSM) is 65.2 mA/cm2 at 900℃. However, rough and porous surfaces result in electrical double layer phenomenon from the ac impedance fitting analysis. Electrochemical behaviors of non-symmetric half cell (LSM/YSZ/Pt) at 900℃ represented the OCV value of 0.94 V, the ASR value of 5.72 Ωcm-2, and power density of 46 mWcm-2, indicating the feasibility of using APPJ to prepare LSM film as cathode mateials was achieved.
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