鎳鈷氧化物水熱合成參數之最佳化與在可撓式鋅空氣電池之應用

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研究生：	林志修 Lin, Zhi-Xiu
論文名稱：	鎳鈷氧化物水熱合成參數之最佳化與在可撓式鋅空氣電池之應用 Hydrothermal Synthesis Parameter Optimization of NiCo2O4 and its Application to Flexible Zinc Air Batteries
指導教授：	胡啟章 Hu, Chi-Chang
口試委員:	劉英麟 Liu, Ying-Ling 陳翰儀 Chen, Han-Yi
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	中文
論文頁數：	125
中文關鍵詞：	鋅空氣電池、雙效催化劑、可撓式電池、膠態電解質、尖晶石氧化物
外文關鍵詞：	Zinc Air Battery, Bifunctional Catalyst, Flexible Battery, Gel Electrolyte, Spinel Oxide
相關次數：	點閱：2 下載：0
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隨著環保意識抬頭，傳統內燃機以及火力發電所造成的空氣汙染也逐漸受到重視，尋找下一代可應用於電動汽車以及大型儲電網的儲能裝置成為重要的研究方向。鋅空氣電池因其高能量密度、原料可取得性、高電壓而成為潛在的人選。然而，鋅空氣電池目前也存在著一些問題：鋅極晶枝、雙效催化劑材料等。在雙效催化劑部分，鎳鈷系尖晶石氧化物(NiCo2O4)獲得極大的關注。
本研究有兩個部分。第一部分本研究採用部分因素設計法對前驅物價數、水熱合成溫度、熱處理時間以及熱處理溫度進行參數的最佳化。接著，使用最佳化參數合成出觸媒，並使用旋轉盤環電極進行基礎的電化學性質量測。
接著，本研究使用最佳化參數合成之NiCo2O4，組成全電池進行穩定性以及電流掃描計時電位法的測試。在穩定性測試中，電池在10 mAcm-2的電流密度下能夠穩定運作超過60小時且無明顯的老化現象。在電流掃描計時電位法測試中，在截止電壓0.4V下，電池能夠工作的最大電流密度為425 mAcm-2；而在電流密度322 mAcm-2時，電池有最大功率密度186.44 mWcm-2。
在第二部分，本研究嘗試使用PVA作為膠態電解質基材組成可撓式鋅空氣電池，並使用最佳化觸媒作為空氣極催化劑。試著透過改善膠態電解質製程以及添加PAAK改善電池表現。
雖然最後結果顯示改善製程以及添加PAAK對電化學性質無明顯差異，本研究仍取得一些初步的成果。本研究成功製備出導電度達到60 mS/cm之膠態電解質。膠態電解質組裝之可撓電池在10 mA/cm2的電流密度下(20分鐘一個循環)充放電循環壽命約可達到30小時。極化曲線顯示最大電流密度約為90 mA/cm2，最大功率密度約為60 mW/cm2。電池容量則在1 mA/cm2以及10 mA/cm2的電流密度下皆可達到35 mAh/cm2。另外，本研究組成之可撓電池經過實測能夠在0度和90度間反覆彎折並持續充放電，可看出其優越的可撓性。

With the rising environmental awareness, the air pollution caused by traditional internal combustion engines and thermal power plants has gradually gained attention. A lot of research is invested in finding the next generation of energy storage devices applied to electric vehicles and large-scale power storage systems. Zinc air batteries are potential candidates because of their high energy density, availability of raw materials and the high voltage. However, there are some issues with zinc air batteries like zinc dendrite growth and bifunctional catalyst materials. In searching for the bifunctional catalyst materials, spinel nickel cobalt oxide has received great attention.
There are two parts in this study. In the first part, we focus on the optimization of hydrothermal synthesis parameters such as precursor valence states, hydrothermal synthesis temperature, calcination time and temperature by using fractional factorial design. Then, with the optimized parameters, we synthesized the catalyst and did some electrochemical measurements using a rotating ring disk electrode.
Next, this study fabricated full zinc air batteries using the parameter optimized NiCo2O4. The cyclability and battery performance were also tested by CP and CPCR. In the cyclability test, the battery can stably cycle for more than 60 hours at a current density of 10 mAcm-2 without significant decay. In the CPCR test, the battery can operate at a maximum current density of 425 mAcm-2 with the cutoff voltage being 0.4 V. The maximum power density is 186.44 mWcm-2 at a current density of 322 mAcm-2.
In the second part, this study fabricates flexible zinc-air batteries with the optimized catalyst and PVA being the gel electrolyte substrate. We try to improve the battery performance by changing the gel electrolyte preparing process and adding PAAK as the additive.
Although the final results showed no significant differences as mentioned above, this study still achieved some preliminary results. In this study, a gel electrolyte with the conductivity of 60 mS/cm was successfully prepared. The flexible battery assembled with the gel electrolyte can reach a cycle life of about 30 hours with the current density being 10mA/cm2 for 20-minute cycle. The polarization curve shows that the maximum current density is about 90 mA/cm2 and the maximum power density is about 60 mW/cm2. The battery capacity can reach 35 mAh/cm2 at both current densities of 1 mA/cm2 and 10 mA/cm2. In addition, the flexible batteries can be repeatedly bent between 0 degree and 90 degrees and continuously charged and discharged, which shows its superior flexibility.

摘要    I
Abstract    III
謝誌    V
圖目錄    IX
表目錄    XII
第一章 緒論及文獻回顧    1
1-1 鋅空氣電池    1
1-1-1 前言    1
1-1-2 金屬空氣電池簡介    2
1-1-3 鋅空氣電池基本工作原理以及挑戰    5
1-2 用於可充式鋅空氣電池催化劑簡介    8
1-2-1 二次鋅空氣電池氧氣還原反應(ORR)及氧氣產生反應(OER)    8
1-2-2 雙效催化劑    10
1-3 尖晶石氧化物    14
1-3-1 尖晶石氧化物介紹    14
1-3-2 尖晶石鎳鈷氧化物    15
1-4 常見電池組裝方式    17
1-4-1 常規平面(Conventional Planar)結構    17
1-4-2 液流電池(Flow Battery)    18
1-4-3 可撓式電池(Flexible Battery)    19
1-4-4 電池組(Multi-Cell Configuration)    21
1-4-5 二極式與三極式組裝    23
1-5 實驗設計(Design of Experiments, DOE)法    25
1-5-1 實驗設計法簡介    25
1-5-2 全因素設計法與部分因素設計法    26
1-6 研究動機與研究大綱    28
第二章 實驗方法、步驟與儀器    30
2-1 儀器與藥品    30
2-2 水熱法製備NiCo2O4    33
2-2-1 25-1部分因素設計    33
2-2-2 實驗步驟    34
2-3 電化學分析    37
2-3-1 旋轉盤電極(Rotating Disk Electrode, RDE)基本原理    37
2-3-2 旋轉盤-環電極(Rotating Ring-Disk Electrode, RRDE)基本原理    39
2-3-3 RRDE觸媒塗佈與相關數據處理    41
2-3-4 循環伏安法(Cyclic Voltammetry, CV)    42
2-3-5 線性伏安掃描(Linear Sweep Voltammetry, LSV)    42
2-3-6 塔弗圖(Tafel plot)    43
2-3-7 全電池測試與測試前處理    44
2-4 可撓式鋅空氣電池    46
2-4-1 PVA膠態電解質製備    46
2-4-2 可撓式電池電化學量測    47
2-5 材料分析儀器簡介    50
2-5-1 X光繞射分析(X-Ray Diffraction Analysis, XRD)    50
2-5-2 掃描式電子顯微鏡(Scanning Electron Microscopy, SEM)    50
2-5-3 比表面積與孔徑分析(Surface Area and Porosity Analyzer)    51
2-5-4 感應耦合電漿質譜儀(Inductively Coupled Plasma-Mass Spectrometer, ICP-MS)    53
2-5-5 X射線光電子能譜儀(X-ray Photoelectron Spectroscopy, XPS)    54
2-5-6 傅立葉紅外光譜(Fourier Transform Infrared Spectroscopy, FTIR)    54
2-5-7 熱重分析(Thermogravimetric Analysis, TGA)    55
第三章 最佳化水熱合成NiCo2O4之參數    57
3-1 部分因子設計    57
3-1-1 循環伏安(CV)結果    57
3-1-2 線性掃描伏安法分析ORR催化效果    59
3-1-3 線性掃描伏安法與塔弗斜率分析OER催化效果    61
3-1-4 計算出最佳合成參數並驗證    63
3-1-5 實驗設計結果討論    68
3-2 材料分析    70
3-2-1 XRD結果分析    70
3-2-2 SEM結果分析    71
3-2-3 XPS結果分析    72
3-2-4 ICP-MS測試結果    77
3-2-5 比表面積與孔徑分布測試結果    78
3-3 鋅空氣電池全電池測試    80
3-3-1 充放電極化曲線    80
3-3-2 穩定性(Cyclability)測試    82
第四章 NiCo2O4觸媒應用於可撓式鋅空氣電池    86
4-1 探討冷凍次數影響    86
4-1-1 導電度測試    86
4-1-2 穩定性(cyclability)測試    87
4-1-3 電池容量(capacity)測量    89
4-2 添加保水劑影響    92
4-2-1 導電度測試    92
4-2-2 充放電極化曲線    93
4-2-3 穩定性(cyclability)測試    97
4-2-4 電池容量(capacity)測量    103
4-2-5 可撓度測試    106
4-3 高分子材料鑑定    109
4-3-1 FTIR鑑定結果    109
4-3-2 TGA鑑定結果    111
第五章 結論與未來展望    114
5-1 結論    114
5-2 未來展望    117


                                

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