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研究生： 黃鈺昇
Huang, Yu-Sheng
論文名稱： 連續性少層數二硫化鉬薄膜與金奈米顆粒於增益光催化產氫之研究
Improvement of Hydrogen Production with Continuous Few-Layer MoS2 Thin Film and Au Nanoparticles as Photocatalysts
指導教授： 陳力俊
Chen, Lih-Juann
口試委員: 彭宗平
Perng, Tsong-Pyng
呂明諺
Lu, Ming-Yen
鄭晃忠
Cheng, Huang-Chung
吳文偉
Wu, Wen-Wei
學位類別： 博士
Doctor
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2021
畢業學年度： 109
語文別： 英文
論文頁數： 96
中文關鍵詞： 局域性電漿表面共振 、二硫化鉬 、光催化
外文關鍵詞： Localized Surface Plasmon Resonance, Molybdenum Disulfide, Photocatalyst
相關次數： 點閱：3  下載：0 
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    • 20世紀以來，因化石能源的漸趨枯竭以及全球暖化加劇，使得以氫能源作為一種替代能源受到矚目；光催化分解水產氫的研究是一極俱潛力的能源再生方法。近年來，電漿子金屬與適當能隙半導體材料所形成的複合奈米結構因其特殊的表面電漿特性以及良好的光吸收性質而受到許多重視，並且許多研究也指出此等複合奈米結構能有效提升半導體材料的光催化能力。
    研究指出因表面電漿共振所產生在奈米金屬顆粒表面的電場強度，會隨著在與表面距離的增加而產生指數性的遞減。因此本論文中，我們設計大面積薄膜的形式與金奈米顆粒-二硫化鉬複合奈米結構，以此為基礎探討不同的金奈米顆粒尺寸及分布對近表面電場的強度影響，進而研究其對光催化分解水產氫的影響。透過熱裂解的方式成長出連續堆積的大面積二硫化鉬薄膜並與金奈米顆粒結合，形成二硫化鉬薄膜在金奈米顆粒上方與下方兩種結構，並依此兩種複合結構進行光催化分解水的比較。結果顯示二硫化鉬薄膜覆蓋在金顆粒上方的複合結構更能有效的利用金顆粒表面電漿共振所產生的近表面電場，因此也擁有較佳的光催化能力。此外，在該結構中，適當的金顆粒的尺寸及間隙距離會使該結構擁有最高的單位面積產氫量，相較於原生二硫化鉬薄膜有了3.8倍的增益，產氫效率也高達279 〖mmol〗^(-1)∙g^(-1)∙h^(-1)。
    此外，我們使用電漿表面處理技術，在二硫化鉬表面形成硫缺陷，使得光催化分解水的的活化點增加，進而增強光催化分解水的能力。我們利用適當強度的氬電漿與試片表面作用，形成最佳比例的硫缺陷，以此進一步使金奈米顆粒-二硫化鉬薄膜試片擁有更高的單位面積產氫量，達到334 〖mmol〗^(-1)∙g^(-1)∙h^(-1)。透過本篇論文的研究，對於未來設計電漿子金屬-半導體複合結構應用時，能有更深一層了解並有望達到更大的增益作用。

    Since the late 20th century, due to the exhaustive consumption of petrochemical fuels and the intensification of global warming, hydrogen fuel has attracted much attention as an alternative energy source. Photocatalytic water splitting for hydrogen production has become a promising energy regeneration method in recent years. The hybrid nanostructures formed by plasmonic metals and narrow-gap semiconductor materials have received a lot of attention due to their special surface plasmonic properties and appropriate light absorption properties. Moreover, many studies have also found that such hybrid nanostructures can effectively improve the photocatalytic ability of semiconductor materials.
    Previous research has indicated that the intensity of localized surface plasmon resonance (LSPR) induced electric field near the surface of plasmonic nanoparticles would decrease exponentially as the distance from the surface increases. Thus, in this thesis work, we designed the form of large-area thin film molybdenum disulfide/gold nanoparticle hybrid structures to explore the influence of different gold nanoparticle sizes and distributions on the near-surface electric field intensity, and then further study the effect on photocatalytic decomposition of water to produce hydrogen. Through the thermal decomposition method, large-area continuously stacked molybdenum disulfide films were grown and combined with the gold nanoparticle to form two hybrid structures: molybdenum disulfide film above and below the gold nanoparticle. Two forms of hybrid structures were used for the comparison of photocatalytic water splitting hydrogen production. The results show that the hybrid structures with the molybdenum disulfide film covering the gold particles could more effectively utilize the near-surface electric field generated by the LSPR of the gold particles, and therefore, they also have better photocatalytic water splitting ability. In addition, in this structure, the proper size and gap distance of the gold particles would enable the structure to have the highest hydrogen production per unit area, which was achieved to be 3.8 times higher than the pristine molybdenum disulfide film, and the hydrogen production efficiency was as high as 279 〖mmol〗^(-1)∙g^(-1)∙h^(-1).
    In addition, we used plasma surface treatment technology to form sulfur defects on the surface of molybdenum disulfide, which increases the active sites for photocatalytic water splitting, thereby enhancing the ability of photocatalytic water splitting. Argon plasma generated with appropriate power was used to bombard the surface of the samples to form a suitable proportion of sulfur defects, so as to further enable the gold nanoparticle-molybdenum disulfide film samples to have higher hydrogen production, reaching 334 〖mmol〗^(-1)∙g^(-1)∙h^(-1). The investigation not only achieves superb photocataytic performance but also leads to basic understanding of controlling mechanism to enhance the hydrogen production of few layer MoS2/Au nanoparticles composite structures.

    Abstract I 摘要 III 誌謝 IV Content V Chapter 1.Introduction 1 1.1.Overview of Nanotechnology 1 1.2.Two-Dimensional Materials 2 1.2.1.Overview of Two-Dimensional Materials 2 1.2.2.Transition Metal Dichalcogenides 2 1.2.3.Molybdenum Disulfide 4 1.3.Water Splitting 6 1.3.1.Background 6 1.3.2.Photocatalytic Water Splitting 6 1.4.Plamonic Properties of Nanomaterials 9 1.4.1.Overview 9 1.4.2.Localized Surface Plasmon Resonance (LSPR) 10 1.4.3.Plasmonic Materials 12 1.4.4.Mechanisms of Photocatalytic Plasmon Enhancement 14 1.5.Scope and Organization 16 Chapter 2.Experimental Section 17 2.1.Experimental Flowchart 17 2.2.Experimental Procedures 17 2.2.1.The Synthesis of Few-Layered MoS2 Thin Films 18 2.2.2.The Fabrication of MoS2 Thin-film above Au Nanoparticles Heterostructures (MaA) 20 2.2.3.The Fabrication of Au Nanoparticles above MoS2 Thin Film Heterostructures (AaM) 21 2.2.4.The Ar Plasma Treatment of MoS2 Thin Film 22 2.2.5.The Measurement of Photocatalytic Properties 23 2.2.6.The LSPR induced near-electric field simulations 23 2.2.7.Photoelectrochemical (PEC) measurement 24 2.3.Introductions of Instruments 25 2.3.1.Spin Coater 25 2.3.2.Three Zone Furnace 26 2.3.3.Electron Beam Gun Evaporation (E-Gun Evaporation) 26 2.3.4.Optical Microscope (OM) 27 2.3.5.Raman Spectrometer 28 2.3.6.Scanning Electron Microscope (SEM) 29 2.3.7.Focused Ion Beam System (FIB System) 30 2.3.8.Transmission Electron Microscope (TEM) 31 2.3.9.Xray photoelectron spectroscopy (XPS) 32 2.3.10. Gas Chromatography (GC) 33 2.3.11.Plasma Surface Treatment System 34 2.3.12.Atomic Force Microscope 35 2.3.13.Finite-Difference Time-Domain (FDTD) simulation 36 Chapter 3.Fabrication and Properties of MoS2 Thin Films 37 3.1.Introduction and Motivation 37 3.2.Results and Discussion 39 3.2.1.Analysis of Photocatalytic Properties of As Grown MoS2 Thin Films 39 3.2.2.Characterization of MoS2_4000 43 3.3.Conclusions 51 Chapter 4.LSPR Properties and Photocatalytic Performance of AaM and MaA Hybrid Heterostructures. 52 4.1.Introduction and Motivation 52 4.2.Results and Discussion 54 4.3.Conclusions 63 Chapter 5.Photocatalytic Performance Enhanced by Argon Plasma Treatment 64 5.1.Introduction and Motivation 64 5.2.Results and Discussion 65 5.3.Conclusions 75 Chapter 6.Summary and Conclusions 76 Chapter 7.Future Prospects 78 7.1.Fabrication of 3D hybrid structure 78 7.2.Phase transformation from 2H-MoS2 to 1T-MoS2 79 References 81

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