一維奈米材料由於其在奈米尺度下擁有優異之物理及化學特性逐漸受到大家重視。具備奈米雙晶結構的銅金屬除擁有高機械強度、良好導電率和抗腐蝕特性外，同時也具備高抗電遷移特性，因此奈米雙晶銅被認為是下一世代的積體電路元件中內連接導線的候選材料之一。本論文涵蓋三部分以奈米雙晶銅奈米線為基礎所延伸的研究：第一部分為奈米雙晶銅線的成長機制，第二部分為雙晶結構修飾表面的原子擴散行為，最後一部分則為雙晶結構輔助磊晶式成長銅銀核殼層結構。本研究主要的發現如下，藉由調控陽極氧化鋁的厚度和孔徑，可製備出不同成長方向的奈米銅線。其中具有（111）成長方向的銅奈米線具有高密度奈米雙晶結構（雙晶間距小於5奈米），而具有（110）成長方向的銅奈米線則具有準單晶結構。另外，雙晶晶界與表面的三接點（Triple junction）處可有效阻擋原子表面擴散，透過臨場式穿透式電子顯微鏡的觀察，發現雙晶晶界與電子流方向呈垂直方向的結構比非垂直夾角的結構更能有效地抑制電遷移。在此，我們使用擴散係數（Diffusivity）和電遷移有效電荷（Effective charge for EM）的特性乘積值去評估上述兩種雙晶結構抑制電遷移的能力。本實驗也根據分子靜力學模擬，計算原子在雙晶/表面三接點的凹處（concave）和凸處（convex）的能態，結果顯示出在凹處的能態比起凸處更加穩定，此結果與實驗所觀察的原子遷移在凹處與凸處接點之延遲時間結果相符。最後一部分，我們透過伽凡尼置換反應製備銅銀核殼結構，儘管銅和銀之間存在著高達12.6%的晶格失配（Lattice mismatch），依然可製備出具有磊晶層的銀殼層，本研究提出雙晶輔助成長與差排緩解機制，解釋銀殼層為何能具備平坦形貌與雙晶結構，此結果顯示出透過奈米雙晶結構能製備磊晶式成長的雙金屬核殼層結構，將可應用在許多光電元件。

One-dimensional materials have attracted considerable attention due to their outstanding physical and chemical properties. Cu metallization with high-density nanoscale twin boundaries (nt-Cu) exhibit high mechanical strength, good conductivity and corrosion resistance and delayed electromigration-induced (EM-induced) mass transport. Thus, nt-Cu nanowires (nt-CuNWs) is considered as a promising material for the next-generation interconnect technology. This thesis covers three aspects of nt-CuNWs, including (1) growth mechanism of nt-CuNWs; (2) atomic diffusion on twin-modified surface; (3) twin-mediated epitaxial growth of Cu/Ag core-shell structure. The major findings are summarized below. The crystallographic orientation of CuNWs can be manipulated by adjusting the thickness and pore size of anodic aluminum oxide (AAO) membranes. The (111)-oriented CuNWs exhibit very dense twin boundaries (average twin spacing ~ 5 nm), while the (110)-oriented CuNWs reveal quasi-single crystalline structure. The triple junctions where twin boundaries meet the CuNW surface serve as obstacles to atomic surface diffusion. The nt-CuNWs with twin boundaries in perpendicular to the CuNW surface is more effective in suppressing EM-induced atomic diffusion than those with twin boundaries inclined to the surface according to in-situ transmission electron microscope (TEM) observations. A characteristic product, DZ*, where D is diffusivity and Z* effective charge of EM, is determined for both types of nt-CuNWs. Moreover, the energy states of triple junctions with concave and convex configurations are calculated based on molecular statics simulations. We found that the former is more energetically stable than the latter, which is consistent with the delayed times measured at these two specific sites. Finally, we demonstrate the epitaxial growth of Ag on CuNWs through galvanic replacement reaction by forming a Cu/Ag core-shell structure despite a large lattice mismatch exists between Cu and Ag (~ 12.6 %). A twin-mediated growth mechanism is proposed to explain the formation of conformal morphology and relieving of misfit dislocations at Ag/Cu interface. The results suggest that a nanotwinning structure enables the heterogeneously epitaxial growth of bimetallic core-shell structure, which are critical for many optoelectronic materials.

Contents
Abstract I
摘要 III
誌謝 IV
Contents VI
List of Figures IX
List of Tables XXI
Chapter 1 Introduction 1
1.1. Introduction 1
1.2. Thesis guide 5
Chapter 2 Literature review 7
2.1. AAO membrane 7
2.1.1. AAO porous structure 7
2.1.2. Formation mechanism of AAO membrane 9
2.1.3. Two-step anodization 11
2.2 Template-assisted electrochemical deposition 12
2.2.1 Electrodeposition of nanotwinned metallic nanowires 13
2.2.2 Microstructure of coherent twin boundary (CTB) 18
2.3. Core-shell nanostructure 19
2.3.1. Galvanic replacement reaction 19
2.3.2. Kirkendall effect during galvanic replacement reaction 21
2.3.3. Copper/metal core-shell nanowires 24
2.4. Properties of nt-Cu 27
2.4.1. Mechanical property of nt-Cu 27
2.4.2. Thermal stability of nt-Cu 30
2.4.3. Abnormal growth in nt-Cu 33
2.4.4. Chemical stability of nt-Cu 36
2.4.5. Electrical property of nt-Cu 40
2.5. Surface diffusion of Cu 45
2.5.1. Surface diffusivity of Cu 45
2.5.2. EM physics 50
2.5.3. Effect of the twin-modified surface on Cu electromigration 52
2.6. Simulation of atomic surface diffusion 54
2.6.1. Embedded-atom method (EAM) functions for fcc metals 54
2.6.2. Surface relaxation 56
2.6.3. Ehrlich-Schwoebel (ES) barrier 58
2.6.4. Cu self-diffusion on surfaces 59
Chapter 3 Experimental section 67
3.1. Chemicals and apparatuses 67
3.2. Sample preparation 69
3.2.1. Fabrication of AAO template 69
3.2.2. Electrodeposition of CuNWs 70
3.2.3. Synthesis of Ag-coated CuNWs 70
3.2.4. TEM sample preparation 70
3.3. Characterization of microstructure 71
3.3.1. X-ray diffractometry (XRD) analysis 71
3.3.2. In situ TEM observation 72
3.3.3. Characterization of CuNWs and Ag-coated CuNWs 72
3.4. Electrical testing setup 72
3.5. Software 73
3.5.1. Construction of periodic crystal structure 73
3.5.2. MS simulation of the energy barrier of surface diffusion 73
Chapter 4 Fabrication and characterization of CuNWs with dense nanoscale CTBs. 75
4.1. AAO-templated electrodepositing of CuNWs 75
4.1.1. Effect of AAO process conditions on CuNW growth direction 77
4.1.2. Effect of the AAO thickness on growth orientation 80
4.2. Microstructure of CuNWs and mechanisms for nucleation and growth 84
4.3. Electrical property of nt-CuNWs 99
4.4. Summary 103
Chapter 5 In situ TEM investigation of atomic diffusion on twin modified surface 104
5.1. Current-induced surface diffusion on nt-CuNWs 105
5.2. Effect of CTB/surface triple junctions on Cu surface diffusion 113
5.3. Summary 118
Chapter 6 Twin-mediated epitaxial Ag growth on nt-CuNWs 119
6.1. Microstructure of Cu/Ag core-shell structures 120
6.2. Twin-mediate epitaxial growth mechanism 127
6.3. Electrical property of Cu/Ag core-shell nanowires 130
6.4. Summary 132
Chapter 7 Conclusions and outlook 133
7.1. Conclusions 133
7.2. Outlook 134
References 139

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