超聲波輔助水解共沉澱法製備β-Ni(OH)2 應用於鎳基電池

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研究生：	蔡盈榛 Ying-Chen Tsai
論文名稱：	超聲波輔助水解共沉澱法製備β-Ni(OH)2 應用於鎳基電池 Preparation of β-Ni(OH)2 electrode using ultrasonic-assisted hydrolysis co-precipitation method for rechargeable Ni-based batteries
指導教授：	李岱洲 Tai-Chou Lee
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 化學工程與材料工程學系 Department of Chemical & Materials Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	中文
論文頁數：	142
中文關鍵詞：	氫氧化鎳、摻雜元素、高比表面積
外文關鍵詞：	β-Ni(OH)2, co-precipitating method, nickel acetate
相關次數：	點閱：8 下載：0
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本研究於超音波環境下以水解共沉澱法製備β-Ni(OH)¬2正極材料，探討不同前驅物、鹼性沉澱環境、摻雜元素對於材料性質及電化學分析的影響。研究分為三個部分，第一部分探討NiCH¬¬3¬COOH、NiNO¬3、NiSO¬¬4、NiCl¬¬¬2四種前驅物於不同沉澱環境下(pH 8-pH 12)製備氫氧化鎳的材料分析，由XRD證實高於pH 10環境下¬¬得到純相且發現結晶強度隨著環境越趨鹼性，結晶性越好，以NiCH3COOH前驅物製備時有最小晶粒；而BET比表面積結果顯示NiCH¬3¬COOH前驅物製備氫氧化鎳具有高比表面積131.54 m2/g、較大的中孔體積93.04 Å、孔洞分布均勻。
第二部分為四種前驅物於pH 12環境下製備氫氧化鎳電極於6 M KOH (pH 14)電解液中進行電化學分析，當晶粒越小時充放電循環穩定性增加，由循環伏安法測得NiCH¬3¬COOH前驅物電化學可逆性較好且有最佳的充電效率；電解液可有效地進入電極內部，於高比表面積中進行反應，有效使電化學反應增加，於300 mA/g下充放電，其電容值達246 mAh/g；經抗腐蝕測試結果發現有最低腐蝕電流181.52 μA/cm2¬¬，於強鹼電解液具高抗腐蝕能力。
第三部分沿用前兩部分最佳參數於pH 12環境下利用NiCH¬3¬COOH前驅物製備氫氧化鎳，並摻雜錳元素提升比表面積及電化學表現。隨著錳含量增加，XRD繞射峰(001)面的β-Ni(OH)¬2¬¬特徵峰值明顯增強並有位移趨勢；由循環伏安法證實0.05 Mn有最佳的充電性能及穩定的可逆性，添加過量錳含量雖然能夠抑制氧氣產生，提升充電效率，但氧化還原的可逆穩定性較差；循環充放電測試於0.05 Mn有最高電容值258 mAh/g，由BET結果顯示0.05 Mn摻雜比表面積高達158.8 m2/g，使電解液擴散活材面積上升，證實添加錳可以提升電化學面積，增加電容值；腐蝕測試大幅降低腐蝕電流值為24.84¬¬ μA/cm2¬¬，進行長時間充放電時，極片結構不容易損壞。由以上實驗結果說明於pH 12鹼性環境下以NiCH¬3¬COOH作為前驅物並摻雜0.05 Mn製備氫氧化鎳極片改質作為鋅鎳電池之正極，有效提高電化學效能，於儲能電池上的應用有相當大的發展。

β-Ni(OH)2 as positive electrode materials were prepared by using the ultrasonic hydrolysis co-precipitating method. Different precursors, alkaline precipitation environment, and doping element on the material properties and electrochemical characteristics were discussed. The materials prepared by nickel acetate, nickel nitrate, nickel sulfate, and nickel chloride under different pH values (pH 8 to pH 12) .The BET results show that nickel hydroxide prepared from nickel acetate precursor has a high specific surface area 131.54 m2/g, a large mesopore volume 93.04 Å, uniform pore distribution .
The electrochemical properties of various nickel hydroxide electrode were investigated in 6 M KOH electrolyte. Nickel acetate precursor exhibited a good electrochemical reversibility and an excellent rechargeable efficiency; the electrolyte can effectively enter the interior of the electrode and react with high specific surface area, increasing electrochemical reaction, and capacitance value reaches 246 mAh/g at 300 mA/g; The corrosion test results showed that nickel acetate precursor electrode has the lowest corrosion current of 121.34 μA/cm2, which has high corrosion resistance in strong alkaline electrolyte.
We then prepared nickel hydroxide under pH 12 using nickel acetate as precursor, and doped with manganese to increase the specific surface area thus improve the electrochemical performance. As the level of manganese content increases, the characteristic peak of β-Ni(OH)2 on the (001) surface of the XRD diffraction peak enhanced significantly and shifted to a high angle ; Cyclic voltammetry showed 0.05 Mn possessed the best rechargeable performance and stability . The specific capacitance reaches 258 mAh/g. BET results show the specific surface area is as high as 158.8 m2/g, which increases the electrochemical area, the corrosion test greatly reduces the corrosion current, meaning structure is not easy to damage when charging and discharging.
Above experimental results show nickel acetate as the precursor and 0.05 Mn doped nickel hydroxide prepared at pH 12 is used as the positive electrode of the zinc-nickel battery, which effective improves the electrochemical performance and them applying to energy storage rechargeable battery.

目錄
摘要    i
ABSTRACT    iii
誌謝    v
目錄    vi
圖目錄    x
表目錄    xv
第一章、緒論    1
1-1 前言    1
1-2 研究動機    4
第二章、文獻回顧    6
2-1 鋅鎳電池簡介    6
2-1-1 鋅鎳液流電池的發展    7
2-1-2 鋅鎳電池的工作原理與傳導機制    9
2-2 氫氧化鎳正極材料發展與簡介    12
2-2-1 氫氧化鎳的結構與反應機制    13
2-2-2氫氧化鎳物理性質及分析特性    16
2-2-3 氫氧化鎳合成方法    22
2-3 氫氧化鎳正極改良之策略    29
2-3-1 顆粒大小與晶粒結構對於電性的探討    29
2-3-2 元素摻雜促進電性提升之影響    34
2-3-3 添加劑改善正極材料目前困境    38
2-4 尿素水解沉澱法簡介    44
2-5 氫氧化鎳孔洞結構介紹    47
第三章、實驗方法與步驟    49
3-1 實驗藥品與器材    49
3-1-1 實驗藥品    49
3-1-2 實驗儀器與器材    51
3-2 實驗流程與架構    52
3-2-1 流程示意圖    52
3-2-2 不同前驅物之β-Ni(OH)2粉末製備    53
3-2-3    摻雜錳元素之β-Ni(OH)2 粉末製備    56
3-2-4發泡鎳網基材前處理    57
3-2-5 正極材料製備    57
3-2-6 電化學測試裝置    58
3-2-7 電解液流場系統    58
3-3 材料鑑定分析    59
3-3-1 X光繞射儀分析 (X-ray Diffraction, XRD)    59
3-3-2 場發射掃描式電子顯微鏡 (Field Emission Scanning Electron Microscope, FE-SEM)    59
3-3-3 拉曼光譜儀 (Raman Spectrometer)    59
3-3-4傅立葉轉換紅外線光譜儀 (Fourier Transform Infrared Spectroscopy, FTIR)    60
3-3-5 動態光散射粒徑分析儀 (Dynamic Light Scattering, DLS)    60
3-3-6 氮氣吸附孔隙儀    61
3-3-7 感應耦合電漿質譜分析儀 ( Inductively coupled plasma-mass spectrometer, ICP-MS)    61
3-3-8  XPS光電子能譜儀 ( Electron Spectroscopy for Chemical Analysis, XPS)    61
3-4 電化學分析    62
3-4-1 循環伏安法 (Cyclic voltammetry, CV)    62
3-4-2 連續循環充放電性測試 (Charge and discharge test)    62
3-4-3 抗腐蝕性測試 ( Corrosion test – Tafel )    62
第四章、結果與討論    63
4-1 前導    63
4-2 不同前驅物於不同酸鹼值下製備β-Ni(OH)2粉末之材料分析    64
4-2-1 X光繞射分析    65
4-2-2拉曼光譜分析    68
4-2-3傅立葉轉換紅外線光譜分析    69
4-2-4 DLS粒徑大小與SEM表面形貌分析    71
4-2-5 氫氧化鎳孔洞結構分析    79
4-3 不同前驅液於不同酸鹼值製備β-Ni(OH)2電極之電化學分析    82
4-3-1 循環伏安法    82
4-3-2 循環充放電測試    86
4-3-3 抗腐蝕性測試    91
4-4  β-Ni(OH)2 粉末改質摻雜錳之結構性質與電化學探討    93
4-4-1 X光繞射結構分析    94
4-4-2 XPS表面價態元素分析    97
4-4-3 ICP元素定量與EDS定性分析    98
4-4-4 錳摻雜循環伏安法    99
4-4-5 錳摻雜循環充放電測試    101
4-4-6 抗腐蝕性測試    104
4-4-7 循環壽命測試    107
第五章、結論與未來展望    112
參考文獻    114
附錄    121


                                

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