最適化鉬摻雜NiCoP與CoFe層狀雙氫氧化物異質結構應用於電催化5-羥甲基糠醛選擇性氧化為2,5-呋喃二甲酸

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蔡峻維(Jun-Wei Cai) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

最適化鉬摻雜NiCoP與CoFe層狀雙氫氧化物異質結構應用於電催化5-羥甲基糠醛選擇性氧化為2,5-呋喃二甲酸
(Optimized Heterostructure of Molybdenum-doped NiCoP and CoFe Layered Double Hydroxides for Electrocatalytic Selective Oxidation of 5-Hydroxymethylfurfural to 2,5-Furandicarboxylic acid)

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至系統瀏覽論文 (2027-8-20以後開放)

摘要(中)

在追求具有成本效益的儲能材料以及可再生能源的過程中，電化學水分解系統是個可行的解方，因陰極反應生成的氫氣被視為是極具潛力的清潔能源。然而，陽極緩慢的析氧反應 (OER) 阻礙了其應用。因此本研究利用生物質的選擇性氧化取代陽極析氧反應，生成高附加價值的產物，不僅可改善現今過度依賴石化燃料的問題，同時也有效利用再生資源。
實驗使用木質素衍生物5-羥甲基糠醛 (HMF) 作為反應物，藉此生成目標產物2,5-呋喃二甲酸 (FDCA) ，由FDCA聚合而成的聚乙烯 2,5-呋喃二甲酸酯 (PEF) 樹脂有望成為聚對苯二甲酸乙二醇酯 (PET) 之替代品。我們以水熱法和爐管磷化熱處理在泡沫鎳 (Nickel foam) 上原位 (in situ) 合成了三維分層結構的NiCoP，並透過裝載CoFe層狀雙氫氧化物 (Layered double hydroxides, LDHs) ，形成n-n型異質結構的CoFe LDH@NiCoP/NF的電觸媒，該異質接面促進表面電子重排，不僅有效改善電化學性能，還提高了催化劑的穩定性。我們進一步以調節Ni-Co前驅液濃度與水熱沉積時間做為變因，找出合成CoFe LDH@NiCoP/NF的最適化條件。最後摻雜適量的鉬 (Mo) 元素，可以有效調節NiCoP的電子結構，從而增加活性位點。
結果顯示用前驅液鎳與鈷莫爾比為1比1，水熱6小時製備的CoFe@NiCoP-6h，在HMF選擇性氧化反應有最佳表現。與未裝載CoFe LDH的NiCoP相比，施加偏壓1.50 V vs. RHE 並反應6小時後，FDCA的選擇率從79.73 % 提升至83.72 %，產率也從64.51 %增加至79.91 %。不僅如此，摻雜2.5 mole % Mo的CoFe@2.5 Mo-NiCoP-6h，HMF轉化率、FDCA產率和選擇率甚至分別達到100 %、98.34 %和98.34 %。綜上所述，作為HMF選擇性氧化的電催化劑，CoFe LDH@Mo-NiCoP/NF是十分具潛力的選擇。

摘要(英)

In the pursuit of cost-effective energy storage materials and renewable energy, electrochemical water splitting systems present a viable solution, as the hydrogen generated by the cathode reaction is a promising clean energy source. However, the slow oxygen evolution reaction (OER) at the anode hampers its application. To address this, our study employs the selective oxidation of biomass to replace the anode OER, generating high value-added products. This approach not only mitigates the current over-reliance on fossil fuels but also effectively utilizes renewable resources.
In this study, we use the lignin derivative 5-hydroxymethylfurfural (HMF) as the reactant to produce 2,5-furandicarboxylic acid (FDCA). FDCA can be polymerized into polyethylene 2,5-furandicarboxylate (PEF) resin, which is a potential substitute for polyethylene terephthalate (PET). We synthesized NiCoP with a three-dimensional layered structure in situ on nickel foam using a hydrothermal method followed by furnace tube phosphating heat treatment. We then loaded CoFe layered double hydroxides (LDHs) to form an n-n type heterostructure CoFe LDH@NiCoP/NF electrocatalyst. This heterojunction promotes surface electron rearrangement, enhancing both the electrochemical performance and stability of the catalyst. We optimized the synthesis conditions of CoFe LDH@NiCoP/NF by adjusting the Ni-Co precursor solution concentration and hydrothermal deposition time. Additionally, doping with an appropriate amount of molybdenum (Mo) effectively adjusted the electronic structure of NiCoP, increasing active sites.
Our results demonstrate that CoFe@NiCoP-6h, prepared with a nickel-to-cobalt molar ratio of 1:1 and hydrothermal treatment for 6 hours, exhibited the best performance in the HMF selective oxidation reaction. Compared to NiCoP without CoFe LDH, the FDCA selectivity increased from 79.73 % to 83.72 %, and the yield from 64.51 % to 79.91 % after applying a constant voltage of 1.50 V vs. RHE for 6 hours.
Remarkably, for CoFe@2.5 Mo-NiCoP-6h doped with 2.5 mole % Mo, the HMF conversion rate, FDCA yield, and selectivity reached 100 %, 98.34 %, and 98.34 %, respectively. In summary, CoFe LDH@Mo-NiCoP/NF shows great promise as an electrocatalyst for the HMF selective oxidation reaction.

關鍵字(中)

★ 過渡金屬磷化物
★ 鉬摻雜
★ 層狀雙氫氧化物
★ 異質結構
★ 電催化選擇性氧化

關鍵字(英)

★ Transition metal phosphides
★ Molybdenum doping
★ Layered double hydroxides
★ Heterostructures
★ Electrocatalytic selective oxidation

論文目次

摘要 i
Abstract iii
誌謝 v
目錄 vii
圖目錄 xi
表目錄 xvii
第一章、緒論 1
1-1 前言 1
1-2 電觸媒發展 3
1-3 研究動機 6
第二章、文獻回顧 10
2-1 電化學分解水 10
2-1-1 HER的基本原理 11
2-1-2 OER的基本原理 13
2-1-3 電催化動力學與重要參數 14
2-2 CoFe LDH@NiCoP異質結構觸媒 23
2-2-1 NiCoP簡介 23
2-2-2 提高NiCoP催化性能的調節策略 26
2-3-3 層狀雙氫氧化物簡介 35
2-3 電催化生物質與選擇性氧化 37
2-3-1 電催化生物質 37
2-3-2 電催化HMF選擇性氧化之反應機制 41
2-3-3 應用於HMF選擇性氧化之電觸媒發展 46
第三章、研究方法 52
3-1 實驗藥品 52
3-2 實驗儀器 55
3-3 實驗步驟 61
3-3-1 電極製備 61
3-3-2 電化學量測 66
3-3-3 HMF選擇性氧化反應 68
第四章、結果與討論 72
4-1 NiCoP電極 72
4-1-1 NiCoP形貌分析 (SEM/FIB) 73
4-1-2 X光繞射分析 75
4-2 CoFe LDH電極 76
4-2-1 CoFe LDH形貌分析 (SEM/FIB) 78
4-2-2 X光繞射分析 79
4-3 CoFe LDH@NiCoP電極 81
4-3-1 CoFe LDH@NiCoP形貌分析 (SEM/FIB) 82
4-3-2 X光繞射分析 84
4-3-3 X-ray光電子能譜儀 85
4-3-4 極化曲線與塔佛爾斜率分析 91
4-3-5 電化學活性面積分析 93
4-3-6 交流阻抗頻譜 97
4-3-7 HMF選擇性氧化反應 98
4-4 CoFe LDH@NiCoP之最適化條件 107
4-4-1 改變Ni/Co前驅液濃度 107
4-4-2 改變Ni-Co前驅液水熱時間 118
4-4-3 鉬摻雜 128
第五章、結論 141
第六章、未來建議 143
參考文獻 145
附錄 163

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指導教授

李岱洲(Tai-Chou Lee)

審核日期

2024-8-20

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