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研究生: 李明曜
Li, Ming-Yao
論文名稱: 還原氧化石墨烯∕三氧化鎢∕二硫化鉬奈米複合材料於電催化裂解水產氫之應用
Electrocatalytic performance of rGO/WO3/MoS2 nanocomposite and its application for hydrogen evolution reaction of water splitting
指導教授: 丁志明
Ting, Jyh-Ming
學位類別: 碩士
Master
系所名稱: 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年: 2019
畢業學年度: 107
語文別: 中文
論文頁數: 95
中文關鍵詞: 二硫化鉬三氧化鎢還原氧化石墨烯微波輔助水熱合成法電催化產氫
外文關鍵詞: MoS2, WO3, Reduce graphene oxide, Microwave-assisted hydrothermal, water splitting, hydrogen generation
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  • 近年來,由於氫能源的高能量密度與無汙染排放的特性,獲得科學家的高度重視,而電催化產氫為現今較成熟且製造高純度氫氣的技術,但由於作為其催化材料的鉑產量稀少,造成成本過高而無法大規模的應用,因此本研究致力於開發用於電催化分解水且低成本的替代催化材料
    本論文以微波輔助水熱合成法製備二硫化鉬奈米複合物,添加還原氧化石墨烯與三氧化鎢前驅物進入反應系統形成三元異質結構,目標藉此增加複合物之比表面積與反應活性。經由微波輔助水熱合成之二硫化鉬具有1T/2H混合相的特性且具有導電性較高的性質,相比於商用之二硫化鉬多為2H半導體相,導電性較差。以此為基礎添加三氧化鎢形成異質結構,增加催化劑的反應活性點。而後再添加還原氧化石墨烯,利用修正漢默法製備之氧化石墨烯經由微波輔助水熱系統還原成還原氧化石墨烯後與二硫化鉬、三氧化鎢形成三元複合物,除了石墨烯本身導電性良好之外,其結構上的缺陷也會增加催化反應進行時的活性點,預期能提高電催化產氫的效果。本實驗使用X光繞射儀、場發射掃描式電子顯微鏡分析其晶體結構、表面形貌,電子能譜儀分析表面化學組成,可見光/紫外光光譜儀分析光學性質,以三電極式電化學裝置進行產氫效能評估以及其長時間反應下的穩定性。

    Hydrogen generation is one of the most important renewable energy technologies in these days, because its high energy density and environmental friendliness. In this study, we have synthesized a novel material, namely, reduced graphene oxide (rGO)/WO3/MoS2 nanocomposites and demonstrated its use as a electrocatalytic water splitting material. The WO3/MoS2 was first synthesized using either one-step or two-step microwave-assisted hydrothermal (MHT) method. Different ratios of the Transition metal dichalcogenides (TMDs) precursors were used in order to obtain WO3/MoS2 having various characteristics. rGO was then added also using the MHT technique. The rGO was added to enhance the electron transfer so that the electron-hole pair recombination is reduced or eliminated. Effects of the synthesis condition on the characteristics of the WO3/MoS2 and rGO/WO3/MoS2 nanocomposite were investigated. The hydrogen generation performance is discussed.

    摘要 I Extended abstract II 誌謝 VII 總目錄 VIII 表目錄 XII 圖目錄 XIV 第1章 緒論 1 1.1 研究背景 1 第2章 文獻回顧 4 2.1 電化學產氫 4 2.1.1 電化學產氫簡介 4 2.1.2 電化學產氫機制 5 2.1.3 電化學產氫材料 7 2.1.4 電催化產氫效能評估方法 8 2.2 二硫化鉬簡介 10 2.3 二硫化鉬製備方法 11 2.3.1 機械剝離法 11 2.3.2 液相剝離法 12 2.3.3 化學合成法 14 2.3.4 微波水熱合成法 16 2.4 二硫化鉬及其複合物用於電催化產氫 18 2.5 過渡金屬氧化物 19 2.6 研究目的與獨特性 20 第3章 實驗方法與分析原理 21 3.1 實驗材料及藥品 21 3.2 實驗儀器設備 22 3.3 實驗流程圖 23 3.3.1二硫化鉬與三氧化鎢 23 3.3.2 三氧化鎢/二硫化鉬複合物 24 3.3.3還原氧化石墨烯/三氧化鎢/二硫化鉬複合物 25 3.4 實驗步驟 26 3.4.1 還原氧化石墨烯之製備 26 3.4.2 二硫化鉬與三氧化鎢之製備 26 3.4.3合成三氧化鎢/二硫化鉬二元複合材料 27 3.4.4還原氧化石墨烯/三氧化鎢/二硫化鉬複合材料 28 3.5 儀器分析 30 3.5.1 拉曼散射光譜 30 3.5.2 XRD晶體結構原理與分析 31 3.5.3 化學鍵結分析 33 3.5.4 比表面積分析儀 ( BET ) 34 3.5.5 材料表面形貌分析 34 3.5.8 電化學性質分析 35 第4章 結果與討論 36 4.1 一步合成三氧化鎢/二硫化鉬二元複合物 36 4.1.1 材料表面形貌與微結構 36 4.1.2 XRD晶體結構分析 40 4.1.3 XPS化學鍵結分析 43 4.1.4 電化學性質分析 51 4.2 兩步合成之三氧化鎢/二硫化鉬二元複合物 55 4.2.1 材料表面形貌與微結構 55 4.2.2 XRD晶體結構分析 56 4.2.3 XPS化學鍵結分析 57 4.2.4 電化學性質分析 63 4.3 一步合成還原氧化石墨烯∕三氧化鎢∕二硫化鉬三元複合物 65 4.3.1 材料表面形貌與微結構 65 4.3.2 XRD晶體結構分析 69 4.3.3 拉曼光譜分析 70 4.3.4 XPS化學鍵結分析 71 4.3.5 電化學性質分析 74 4.4 兩步合成還原氧化石墨烯∕三氧化鎢∕二硫化鉬三元複合物 75 4.4.1 材料表面形貌與微結構 75 4.4.2 XRD晶體結構分析 79 4.4.3 拉曼光譜分析 80 4.4.4 XPS化學鍵結分析 81 4.3.5 電化學性質分析 84 第5章 結論 92 第6章 參考文獻 93

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