臺灣博碩士論文加值系統

本研究利用簡單的一步驟電沉積合成出鎢摻雜氫氧化鎳，將之做為尿素電解的觸媒進行催化機制的探討，綜合材料鑑定分析，發現樣品為α結晶型態的氫氧化鎳(Nickel hydroxide, Ni(OH)2)，在鎢摻雜之後可觀察到鎳金屬的存在以及電子組態的改變；電化學分析發現鎢摻雜氫氧化鎳展現出較為出色的尿素氧化表現，對比未改質的樣品，有著較高的催化電流(332 vs 108 mA cm-2 at 1.48 V)、較低的塔弗斜率(71 vs 162 mV dec-1)、較高的週轉頻率(0.14 vs 0.07 s-1)以及較大的反應速率常數(6.0 x 105 vs 3.2 x 104 cm3 mol-1 s-1)，更重要的是在大電流100 mA cm-2的操作下表現48小時良好的穩定性。至於陰極析氫反應，鎢摻雜前後並未有顯著差異，說明鎢摻雜的材料改質主要應用於陽極催化尿素氧化反應。本研究後續運用交流阻抗頻譜分析與臨場拉曼光譜分析，搭配非臨場的X射線光電子能譜與高解度電子顯微鏡分析進行催化機制的探討，可以觀察到鎢摻雜氫氧化鎳能在較低的電壓產出Ni3+活性位點，進行直接與間接尿素氧化反應，實驗結果顯示間接尿素氧化反應為主要的催化路徑。

This study adopts a simple and one-step electrodeposition method to prepare tungsten-doped nickel hydroxide for the applications in urea electrolysis. Based on the experimental data, the W-doped sample belongs to α-Ni(OH)2 with the presence of metallic nickel clusters. Moreover, W-doping is found to modulate the electronic configuration of nickel hydroxide, which is beneficial to induce the formation of Ni3+ active site. The results show that the W-doped sample exhibits superior electrochemical performance for urea oxidation, exhibiting higher catalytic current (332 vs 108 mA cm-2 at 1.48 V), lower Tafel slope (71 vs 162 mV dec-1), higher turnover frequency (0.14 vs 0.07 s-1), and larger reaction rate constant (6.0 x 105 vs 3.2 x 104 cm3 mol-1 s-1) compared with the unmodified sample. More importantly, W-doped α-Ni(OH)2 demonstrates stable electro-oxidation of urea even at high current density of 100 mA cm-2 for 48 hours. In regard to the hydrogen evolution reaction, the modified sample exhibits comparable electrochemical performance to the pristine sample. The results illustrate that the W-doping strategy mainly facilitates urea oxidation but not hydrogen evolution. Combining the data from electrochemical impedance spectroscopy, in-situ Raman spectroscopy, ex situ X-ray photoelectron spectroscopy, and ex situ transmission electron microscopy, it is found that W-doping can effectively induce the formation of Ni3+ active site at low overpotential for direct and indirect urea oxidation.

摘要...i
Abstract...ii
目錄...iii
表目錄...v
圖目錄...vi
第一章 緒論...1
1.1前言...1
1.2研究動機...5
第二章文獻回顧...6
2.1氫氧化鎳用於尿素氧化反應...6
2.2氫氧化鎳應用於析氫反應...10
2.3金屬離子摻雜氫氧化鎳對電化學催化表現的影響...12
2.4含有鎳金屬異質結構對電化學催化表現的影響...17
2.5親水性與電極表面氣泡脫附對電化學催化表現的影響...20
2.6臨場拉曼光譜偵測尿素電解反應機制...22
2.6.1臨場拉曼光譜偵測尿素反應機制...22
2.6.2臨場拉曼光譜偵測析氫反應機制...24
第三章 實驗步驟與設備...26
3.1實驗藥品...26
3.2實驗儀器...27
3.3實驗步驟...28
3.3.1泡沫鎳前處理...28
3.3.2電沉積合成鎢摻雜氫氧化鎳...28
3.4材料分析...29
3.4.1接觸角...29
3.4.2 X光繞射分析儀...29
3.4.3共軛拉曼光譜分析儀...29
3.4.4掃描電子顯微鏡...30
3.4.5穿透式電子顯微鏡...30
3.4.6 X射線電子能譜儀...30
3.5電化學分析...31
3.5.1三極式設備操作...31
3.5.2循環伏安法與線性掃描伏安法...31
3.5.3 iR校正方程式...31
3.5.4塔弗方程式...32
3.5.5週轉頻率計算...32
3.5.6電化學活性表面積...32
3.5.7電化學阻抗譜...33
3.5.8電化學電極表面氣泡脫附...33
3.5.9計時電流法...34
3.5.10穩定性測試...34
3.5.11全裝置電池測試...34
第四章 鎢摻雜氫氧化鎳提升尿素催化表現...35
4.1 材料分析...35
4.1.1 XRD分析...35
4.1.2 Raman分析...36
4.1.3 XPS分析...37
4.1.4 TEM分析...38
4.1.5 SEM分析...41
4.1.6親水性分析...42
4.2 電化學表現...43
4.2.1 UOR/OER線性掃描伏安法...43
4.2.2 UOR Tafel分析...44
4.2.3 TOF分析...45
4.2.4電化學活性表面積分析...46
4.2.5計時電流法與速率常數分析...47
4.2.6電極表面氣泡脫附分析...48
4.2.7電化學阻抗譜分析...49
4.2.8 UOR穩定性測試...51
4.2.9 HER分析...51
4.2.10全裝置電化學分析...53
4.2.11尿素氧化電化學觸媒比較表...54
4.3 臨場拉曼光譜分析...57
4.3.1臨場拉曼光譜探討尿素氧化反應機制...57
4.3.2臨場拉曼光譜探討析氫反應機制...60
第五章 總結...61
參考文獻...62

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