利用後硒化製程在絕緣基板上控制二硒化鎢層狀成長之研究

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研究生：	吳姵禛 Wu, Pei-Chen
論文名稱：	利用後硒化製程在絕緣基板上控制二硒化鎢層狀成長之研究 Layered growth of WSe2 thin films on insulating substrate by post selenization
指導教授：	賴志煌 Lai, Chih-Huang
口試委員:	廖建能 Liao, Chien-Neng 朱旭山 Chu, Hsu-Shen 闕郁倫 Chueh, Yu-Lun 曾院介 Tseng, Yuan-Chieh
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：	2020
畢業學年度：	108
語文別：	中文
論文頁數：	114
中文關鍵詞：	二硒化鎢、硒化、層狀成長、方向性堆疊、記憶體、磊晶
外文關鍵詞：	WSe2, selenization, layered growth, texture control, memory, epitaxy
相關次數：	點閱：2 下載：0
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層狀TMDC材料由於高電子流動性、高電流開關比、可調變能隙以及高化學反應活性接觸點，所以層狀TMDC材料被的研發被認為是一種可以驅使積體電路中電晶體數目不斷增加的方法之一。WSe2在大氣中相對穩定。在不須添加氧化物做為保護層，就可以清楚的暸解在不同製程手法下，材料本身基礎的特性。在過去十年,TMDC層狀尺寸化成長技術一直都是很大的挑戰。從絕緣基板到藍寶石基板、前驅物的選擇從金屬到金屬氧化，化學氣相沉積製程中所使用的硒源和時間梯度控制，以及最後TMDC的轉印技術都是控制TMDC是否可以尺寸化因素之一。
為了有效成長WSe2膜層，並且了解WSe2的成長機制，本論文致力於使用低溫、短時間以及不需要使用毒性氣體(H2Se)的製程使層狀WSe2膜層尺寸化。本論文首先嘗試在(111)方向性的Pt/Ta/SiO2/Si 基板利用後硒化製程成長大尺寸且均勻地層狀WSe2膜層。其次使用非晶質SiO2/Si基板，運用具有相變化的金屬鎢做為前驅層，在使用相同的硒化條件，了解WSe2的成長機制。最後，透過硒化條件的控制，使表面形貌發生改變，進而造成親水性與疏水性的變化。
本論文提出的方法在不需要使用金屬氧化物(WO3)以及有毒氣體(H2Se)的前提下，不僅可以大尺寸均勻的成長WSe2、也可以藉由不同相的前驅層金屬鎢控制WSe2膜的堆疊方向，同時藉由硒化條件改變可以調整WSe2表面形貌進而增加WSe2的應用性。現階段，此製程不論在大尺寸均勻合成或是表面改質上都可具有可調變性，相信在未來將具有一定的潛力。

Increasing the number of transistors in integrated circuits is vital to the continued development of modern technological devices. Layered transition metal dichalcogenides (TMDCs) have been proposed for this purpose due to their high electron mobility, high current-switching ratio, variable energy gap, and high chemical reactivity. Relatively stable WSe2 film is employed in this dissertation, on which a protective layer of oxide does not need to be deposited, allowing the characteristics of WSe2 to be accurately assessed without interference. In the past 10 years, layered TMDC dimension growth is a big challenge. The factors that affect the layered TMDC dimension include a substrate, precursor, the selenium source and the reaction temperature gradient using in the process. This dissertation aims to utilize the low reaction temperature, short reaction time and non-toxic gas source to synthesis the layered WSe2 in order to understand the WSe2 growth mechanism. At first, in the dissertation, the big dimension growth of layered WSe2 films on (111)-directional Pt/Ta/SiO2/Si substrates using the selenization process. Secondly, the WSe2 with a different texture on the amorphous SiO2/Si substrates using the selenization process with different tungsten phase precursors in order to understand the WSe2 growth mechanism. Finally, through an optimized selenization temperature gradient modified WSe2 surface with different wettability. With this approach to growth the big dimension WSe2 film, the structure of WSe2 with different texture and morphology can be obtained by the precursor tungsten with different phases. At the current stage, the post selenization shows potential for large dimension layered WSe2 synthesis in the future.

致謝 I
Abstract  II
中文摘要III
Contents  IV
List of Figures  VI
Chapter 1 General Introduction  1
1 Context and objectives  1
2 Organization of this thesis  4
Chapter 2 Background  5
1 Introduction to TMDCs  5
1.1 TMDC crystals  6
1.2 The electron band structure for bulk and monolayer WSe2 7
1.3 2H–1T phase transformation  9
2 Fabrication of TMDCs  12
2.1 Bottom-up techniques  12
2.2 Top-down method 14
2.3 Low-temperature synthesis methods 17
3 Application of WSe2  20
3.1 The use of van der Waals forces 20
3.2 The use of dangling bonds  23
Chapter 3 Experimental Design and Analysis  26
1 Sample preparation  26
1.1 Tungsten fabrication 26
1.2 Two-step selenization 27
1.3 Film transfer method 28
2 Structural characterization  29
2.1 X-ray diffraction (XRD)  29
2.2 2D X-ray diffraction (2D-XRD)  30
2.3 Raman spectroscopy 31
2.4 Atomic force microscopy (AFM)  32
2.5 Scanning electron microscopy (SEM)  33
2.6 Transmission electron microscopy (TEM) 34
2.7 X-ray photoelectron spectroscopy (XPS)  35
2.8 Resistivity switching measurement system  36
Chapter 4 Epitaxial Growth of WSe2 via the Self-Assembly of PtSe2  37
1 Introduction of the epitaxial technique 37
2 Experimental design 38
3 Results and discussion  40
3.1 Scalable epitaxial WSe2 film  40
3.2 The uniformity of WSe2 as analyzed by Raman mapping  48
3.3 Se2 flakes with different thicknesses after exfoliation  51
3.4 Electrical performance of the WSe2 film  55
3.5 Summary  58
Chapter 5 Mechanisms Underlying the Growth Process of WSe2  59
1 Purpose  59
2 Experimental design 59
3 Mechanism discussion  59
3.1 Substrate effect  59
3.2 The role of PtSe2  62
3.3 The influence of Pt thickness  68
4 Summary  73
Chapter 6 Stacking of WSe2 in Lateral and Vertical Directions through the
Controlled Selenization of Tungsten Films74
1 Purpose  74
2 Experimental details76
3 Results and discussion 77
3.1 Characterization of WSe2  77
3.2 Tungsten phase transformation  78
3.3 The growth mechanisms of WSe2  81
3.4 Summary  86
Chapter 7 Controlling Wettability by Changing WSe2 Surface Roughness  87
1 Introduction 87
2 Experimental details 88
3 Results and discussion  89
3.1 Texture control for WSe2 film.  89
3.2 WSe2 growth mechanisms  93
3.3 Creation of a hydrophobic surface  99
4 Summary  102
Chapter 8 Conclusion and Suggestions for Future Work  103
1 Conclusion  103
2 Suggestions for future work  104
                                

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