近年來探討利用二維過渡金屬二硫化合物(TMDCs)之材料做產氫催化反應越來越熱門。為了提升產氫效果，有些文章討論在TMDCs之材料上摻雜金屬來讓產氫效果更好，又有些文章是改變TMDCs材料的結構來使催化點位變多進而提升產氫效率。現今，用簡單的Bottom-up方法製備石墨烯量子點(GQDs)或石墨烯(GO)已經是成熟的技術，利用控制有機前體檸檬酸(CA)的碳化程度來製備石墨烯量子點(GQDs)或石墨烯(GO)。本論文是利用石墨烯量子點(GQDs)修飾MoS2與WSe2這兩種不同的TMDCs材料後，探討這兩種複合材料之產氫效率。
論文分成兩部分，第一部分是用離子插層法製備出1T相與2H相的MoS2¬材料，再利用Bottom-up方式製程出GQDs來修飾1T相與2H相的MoS2。我們利用UV-vis , Raman spectroscopy, XRD, XPS等四種測量方式確認我們做出來的樣品為實驗所需。第二部分是利用常見的薄膜製程技術：化學氣相沉積法(CVD)長出WSe2薄膜，再用GQDs修飾WSe2。WSe2是用Raman spectroscopy, PL, AFM等量測技術來確認材料成分與長晶後的薄膜厚度。將兩種TMDCs材料與GQDs合成複合材料後，再用電化學的三電極系統研究兩樣複合材料之產氫效率。
第一部分的研究結果發現：1T相的MoS2產氫效果會比2H相來的好，且有經過GQDs修飾過的材料，也會提升其產氫效率。第二部分因為CVD是我們實驗室是新的技術，目前長晶技術還尚未成熟，從Raman spectroscopy, PL, AFM的量測數據可以得知我們還無法長出少層數之樣品，但已經確定可以從前驅物的粉末製造出WSe2的薄膜，要將WSe2長成少層甚至單層數的樣品是指日可待，不久的未來就可以把少層或單層數的WSe2經過GQDs修飾後去探討其複合材料之產氫效果。

Recently, two-dimensional transition metal dichalcogenides (TMDs) materials have been widely studied for their superior catalytic performance in hydrogen evolution reaction (HER). There are articles discussing enhanced HER efficiency due to metal ion doping. There are also articles about changing the structures of TMD material to increase the number of catalytic sites for improving HER efficiency. Nowadays, simple bottom-up method has become a mature technique to prepare graphene quantum dots (GQDs) or graphene oxide (GO) by tuning the carbonization degree of citric acid. In this thesis, we studied the HER activity of GQDs decorated molybdenum disulfide (MoS2) and tungsten diselenide (WSe2¬) composites.
The thesis is divided into two parts. The first part is about the preparation of 1T and 2H MoS2 by ion intercalation method and the decoration of MoS2 sample with GQDs. We have used UV-vis to measure the visible and ultraviolet light absorption rate of the materials, Raman spectroscopy and XRD to identify the crystal structures and XPS measurements to probe the valence states of the sample. The second part is about the preparation of WSe2 films by chemical vapor deposition (CVD) method and the decoration of WSe2 film with GQDs. Raman spectroscopy and photoluminescence were employed to characterize the samples. Atomic force microscopy (AFM) was used to observe the morphology of the samples and to measure their thickness. The HER catalytic activity of the samples was evaluated by using a three-electrode system.
The results of our measurements show that 1T-MoS2 has better HER efficiency than 2H-MoS2. With GQDs decorated on MoS2, the HER efficiency can be improved. The 1T-MoS2@GQDs composites has the best HER efficiency.

摘要 I
Abstract II
致謝 III
目錄 IV
第一章 序論--1
1-1 研究動機--1
1-2 研究目的--2
第二章 文獻回顧--3
2-1 二維過渡金屬二硫族化合物(TMDCs)材料介紹--3
2-2 二硫化鉬(MoS2)材料介紹--4
2-3 石墨烯量子點(GQDs)材料介紹--5
2-4 二硒化鎢(WSe2)材料介紹--5
第三章 實驗方法與原理--6
3-1 電化學(Electrochemical)--6
3-1-1 電化學產氫(Hydrogen Evolution Reaction；HER)--6
3-1-2 線性伏安法(Linear Sweep Voltammetry；LSV)--8
3-1-3 電化學阻抗頻譜(Electrochemical Impedance Spectroscopy；EIS)--10
3-2 拉曼光譜(Raman Spectroscopy)--12
3-3 紫外-可見光光譜(Ultraviolet–visible spectroscopy；UV-vis)--14
3-4 X光射線繞射(X-ray Diffraction；XRD)--15
3-5 X光射線光電子能譜學(X-ray Photoelectron Spectroscopy；XPS )--16
3-6 原子力顯微鏡(Atomic Force Mictroscopy；AFM )--16
3-7 光致發光光譜(Photoluminescence Spectrum；PL)--17
第一部分：石墨烯量子點修飾二硫化鉬--18
第四章 樣品製備與實驗流程--19
4-1 樣品製備--19
4-1-1 二硫化鉬製備--19
4-1-2 石墨烯量子點製備--21
4-2 實驗藥劑--23
4-3 實驗流程--24
4-4 樣品製備步驟--25
4-4-1 MoS2製備步驟--25
4-4-2 GQDs製備步驟--25
4-4-3 MoS2@GQDs製備步驟--27
第五章 數據分析與討論--28
5-1 紫外-可見光光譜(Ultraviolet-visible Spectroscopy)--28
5-2 X光射線繞射(X-ray Diffraction)--30
5-3 拉曼光譜分析(Raman Spectroscopy)--32
5-4 X光射線光電子能譜學(X-ray Photoelectron Spectroscopy)--34
5-5 電化學分析(The Electrochemical Analysis)--37
第六章 結論與展望--43

第二部分：石墨烯量子點修飾二硒化鎢--44
第四章 樣品製備與實驗流程--45
4-1 樣品製備--45
4-1-1 二硒化鎢製備--45
4-1-2 石墨烯量子點製備--47
4-2 實驗藥劑--49
4-3 實驗流程--50
4-4 樣品製備步驟--51
4-4-1 WSe2製備步驟--51
4-4-2 GQDs製備步驟--52
第五章 數據分析與討論--53
5-1 拉曼光譜分析(Raman Spectroscopy)--53
5-2 光致發光光譜分析(Photoluminescence Spectroscopy)--56
5-3 原子力顯微鏡(Atomic Force Microscopy)--58
第六章 結論與展望--59
參考文獻--60

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