應用脈衝雷射鍛燒法製備高效能之 高熵氧化物/多孔鎳超電容器電極

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姓名

余佳宣(Jia-Xuan Yu) 查詢紙本館藏

畢業系所

材料科學與工程研究所

論文名稱

應用脈衝雷射鍛燒法製備高效能之高熵氧化物/多孔鎳超電容器電極
(Fabrication of Highly Efficient High Entropy Oxide/Ni Porous Substrate Supercapacitor Electrodes Using Pulsed Laser Calcination)

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摘要(中)

近年來隨著科技快速發展，能源消耗與環境汙染問題與日俱增，促使全球能源議題的重視，也象徵著可再生能源與能源裝置的使用不可或缺。超級電容器其具有快速充放電、高比電容值與功率密度且耐高溫高壓等優異性能，而被認為是高效的儲能設備之一。在一般傳統超級電容器製造上，通常會採用漿料塗布技術，然而此技術易使得製程複雜性提升，因此如何開發無添加劑電極，成為研究人員新的研究課題。
　　本研究致力於開發無須添加黏合劑與助導劑，製作可直接進行量測之高熵氧化物/壓錠多孔鎳電極。研究總共可分為三部分，第一部份為探討使用鎳粉末以壓錠技術製成壓錠多孔鎳基板(Ni porous, NP)與商用發泡鎳，並作為超級電容之集電層進行電化學性能比較，第二部分為利用脈衝雷射鍛燒法探討活性材料高熵氧化物、錳鐵氧化物、鐵氧化物，三者晶體結構與電化學性能差異，第三部分則為將壓錠多孔鎳基板，浸泡高熵金屬鹽類前驅物一段時間後烘乾，並分別使用高溫熱裂解法與脈衝雷射鍛燒法，於壓錠多孔鎳基板上生成高熵氧化物。
　　透過微觀結構分析，相較商用發泡鎳基板，壓錠多孔鎳基板呈現顆粒狀形貌，由電化學電性分析，脈衝雷射功率1W下之高熵氧化物/壓錠多孔鎳電極，於1A/g電流密度比電容值為870 F/g，且高熵氧化物作為活性物質其性能要優異於單一與雙金屬氧化物，而高溫熱裂解法之電極由於高熵氧化物相較於脈衝雷射鍛燒法緻密，造成電極阻抗大，在電化學分析下，於1A/g電流密度下比電容明顯遠低於脈衝雷射鍛燒法。透過本研究結果顯示，利用脈衝雷射鍛燒法，其具有操作簡易與製造省時的特性，可有效合成無須添加劑之超級電容活性材料高熵氧化物。

摘要(英)

High-entropy oxides have attracted researcher′s interest due to the entropy stabilization effects caused by the interaction between different ions. Slurry coating technology is often used in the manufacturing of supercapacitors, however, the residual binder may influence the performance of fabricated supercapacitor.
　　This research is dedicated to the development of binder-free fabrication process and characterization of highly efficient high entropy oxide/Ni porous substrate electrodes. In the first part, the of ingot porous nickel substrate (Ni porous, NP) made of nickel powder is used as current collector layer, and the electrochemical performance of the NP supercapacitor is compared with that of commercial foamed nickel substrate. In the second part, electrodes with active materials of high entropy oxide, manganese iron oxide, and iron oxide are fabricated by using pulsed laser calcination. The materials are characterized by using X-ray diffraction (XRD). Lastly, performance of high entropy oxide/Ni porous substrate electrodes fabricated by using pulsed laser calcination is compared with that of high temperature pyrolysis process.
　　The SEM results show that the microstructure of ingot porous nickel substrate is consist of porous backbones with nanostructures of particles. High-entropy oxides show better performance than single and bimetallic oxide. The electrochemical analysis of HEO/NP electrode with a pulsed laser power of 1W shows a specific capacitance value of 870 F/g at 1A/g. These results show that pulsed laser calcination is a facile and time-saving manufacturing process for effectively synthesizing high-entropy oxides on porous nickel substrate.

關鍵字(中)

★ 超級電容器
★ 高熵氧化物
★ 脈衝雷射鍛燒法
★ 無黏結劑電極
★ 壓錠多孔鎳

關鍵字(英)

★ Supercapacitors
★ High-entropy oxides
★ Pulsed laser calcination
★ Binder-free electrodes
★ Ni porous substrate

論文目次

摘要I
AbstractIII
致謝IV
目錄V
圖目錄IX
表目錄XIII
第一章　緒論1
1.1　前言1
1.2　基本原理與文獻回顧2
1.2.1 超級電容器簡介2
1.2.2 超級電容器之儲能機制4
1.2.2.1 電雙層電容器(EDLC)5
1.2.2.2 擬電容器(Pseudocapacitor)7
1.2.2.3 混合電容器(Hybrid supercapacitor)9
1.2.3 超級電容之結構組成10
1.2.3.1 超級電容器之電解質11
1.2.3.2 超級電容器之集電層14
1.2.3.3 超級電容器之活性材料17
1.2.4 高熵氧化物(High entropy oxides, HEO)23
1.2.5 脈衝雷射鍛燒法(Pulsed laser calcination)27
1.2.6 超級電容器之電化學分析技術28
1.2.6.1 循環伏安法(Cyclic voltammetry, CV)28
1.2.6.2 恆電流充放電法(Galvanostatic charge-discharge, GCD) 30
1.2.6.3 電化學交流阻抗頻譜(Electrochemical impedance spectroscopy, EIS)31
1.3 研究動機與目的32
第二章實驗方法33
2.1 實驗藥品33
2.2 製程與分析儀器34
2.2.1紫外光臭氧清洗機(UV-ozone stripper)34
2.2.2 恆電位儀(Potentiostat)35
2.2.3脈衝雷射(Pulsed laser)35
2.2.4 光學顯微鏡(Optical microscope,OM)36
2.2.5 掃描式電子顯微鏡(Scanning electron microscopy, SEM) 36
2.2.6 X光繞射技術(X-ray diffraction, XRD)37
2.2.7 X射線光電子能譜(X-ray photoelectron spectrscopy, XPS) 37
2.3 實驗流程38
2.4 實驗製程39
2.4.1 多孔鎳基板製作39
2.4.2 試片前置處理39
2.4.3 脈衝雷射鍛燒法製程參數設置40
2.4.4 脈衝雷射鍛燒法製備高熵活性物質41
2.4.5 高溫爐熱裂解法製備高熵活性物質41
2.4.6 電化學系統42
第三章結果與討論43
3.1 壓錠多孔鎳與商用發泡鎳之基板分析43
3.1.1 掃描電子顯微鏡分析(SEM)43
3.1.2 X射線光電子能譜分析(XPS)45
3.1.3 電化學分析47
3.2於壓錠多孔鎳表面生成HEO、MnFexOy、FexOy活性物質之分析50
3.2.1 掃描電子顯微鏡分析(SEM)50
3.2.2 X光繞射技術(X-Ray diffraction, XRD)50
3.2.3 電化學分析52
3.3脈衝雷射鍛燒法與高溫熱裂解法製作高熵氧化物55
3.3.1掃描電子顯微鏡分析(SEM)55
3.3.2 X光繞射技術(X-Ray diffraction, XRD)55
3.3.3電化學分析56
第四章結論61
第五章參考文獻62

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指導教授

李勝偉(Sheng-Wei Lee)

審核日期

2023-8-17

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