本研究以穿透式電子顯微鏡即時動態壓縮與壓痕技術分析微柱之機械性質。從研究結果得知，在即時動態壓縮過程中可以發現材料應力波傳遞與結構變化；在壓縮後，因內部結構產生缺陷與破壞而使材料產生彎曲與斷裂。氯化鈉、氧化鋁、鎳鋁和鎳鈦合金奈米柱經動態壓縮試驗得知楊氏模數分別為: 10.4-23.9 GPa、25.5-347.5 GPa、32.7-44.9 GPa、5.9-24.4 GPa。氯化鈉、氧化鋁、銅、鎳鋁和鎳鈦合金經奈米壓痕試驗得知維氏硬度值分別為: 196-260 MPa、14.0-20.2 GPa、1.1-1.2 GPa、2.9-4.5 GPa和7.4-7.7GPa。研究中發現氧化鋁在維克氏硬度測試後，材料內部結構透過高解析穿透式電子顯微鏡觀察出有位錯和差排環的現象產生。本文也使用分子動力學探討銅柱狀結構受壓縮後之力學特性與材料變形機制。研究結果可以看出，銅柱在壓縮過程中會有差排和應力波傳遞的現象，且銅柱的外徑會隨著壓縮的位移增加而增加。最後，透過理論探討與模擬分析，材料微柱的機械特性應建立重要性能與結構相關連的機制與理論。

In this study, the mechanical properties of micropillars were analyzed by in situ transmission electron microscopy compression and indentation. The results show that the stress wave propagation and structural variations of the material can be found during in situ compression. After compression process, because of the internal structure of the material defects and damage, the micropillar will be bended and broken. The Young's modulus of NaCl, Al2O3, NiAl and NiTi alloy micropillaby in situ compression test were 10.4-23.9 GPa, 25.5-347.5 GPa, 32.7-44.9 GPa and 5.9-24.4 GPa, respectively. Vickers hardness values of NaCl, Al2O3, Cu, NiAl and NiTi alloy were found to be 196-260 MPa, 14.0-20.2 GPa, 1.1-1.2 GPa, 2.9-4.5 GPa and 7.4-7.7GPa, respectively. In the study, it was found that the phenomenon of dislocation and dislocation loop appeared in the internal structure of the Al2O3 by high-resolution transmission electron microscopy after the Vickers hardness test. The mechanical behavior and deformation mechanism of Cu micropillar structures through molecular dynamics simulation after compressed were also investigated in this study. As can be seen from the research results, Cu pillars have dislocation and stress wave transmission phenomenon during the compression process, and the diameter of the Cu pillar has increased with the increase of the compression displacement. Finally, through theoretical exploration and simulation analysis, the mechanical properties of micropillar should establish the important properties and the mechanism of structures and theory.

摘要 i
Abstract ii
Acknowledgements iv
Contents v
List of table captions ix
List of figure captions x
Symbol table xiv
Chapter 1 Introduction 1
1.1 Microstructure materials 1
1.1.1 Mechanical properties of microstructure materials 1
1.2 Nanostructure materials 3
1.2.1 Mechanical properties of nanostructure materials 4
1.3 Motivation 5
1.4 Thesis organization 5
Chapter 2 Literature review 7
2.1 Literature review of in situ transmission electron microscope compression 7
2.2 Literature review of sodium chloride materials 9
2.3 Literature review of alumina materials 10
2.4 Literature review of single crystal copper materials 11
2.5 Literature review of nickel - aluminum alloy 12
2.6 Literature review of nickel - titanium alloy 13
Chapter 3 Experimental and molecular dynamics simulation method 14
3.1 Experimental architecture 14
3.1.1 . Preparation of the materials 15
3.1.2 . Cutting of pillar structures 15
3.1.3 Experimental procedures 15
3.2 Mechanical analysis of materials 20
3.3 Molecular dynamics simulation 24
3.4 Measurements devices 26
3.4.1 Vacuum arc melting furnace 26
3.4.2 Grinding and polishing machine 27
3.4.3 Atomic force microscope (AFM) 28
3.4.4 Double beam type focusing ion beam instrument (DB-FIB) 29
3.4.5 In situ nano indentation testing machine 30
3.4.6 Transmission electron microscope (TEM) 31
3.4.7 Raman 32
3.4.8 Nanoindentation 33
3.4.9 Vicker hardness 36
Chapter 4 NaCl substrate and pillar structures 38
4.1 Results and discussion 38
4.1.1 Surface morphology and local contact behavior 38
4.1.2 Mechanical properties and dynamic deformation 40
4.1.3 Nanoindentation 44
4.1.4 Vickers micro-hardness test 45
Chapter 5 Alumina (Al2O3) substrate and pillar structures 48
5.1 Results and discussion 48
5.1.1 Dynamic deformation of Al2O3 nanopillars during in situ TEM compression 48
5.1.2 Stress-displacement curves of Al2O3 nanopillars during in-situ TEM compression 53
5.1.3 Nanoindentation 54
5.1.4 Vickers micro-hardness test 56
5.1.5 Raman spectrum 57
5.1.6 FIB micrographs after the Vickers hardness measurement 58
5.1.7 HR-TEM micrographs after Vickers hardness 59
Chapter 6 Single-crystal Cu substrate and pillars structures 61
6.1 Results and discussion 61
6.1.1 Compression process and mechanical properties during molecular dynamics simulation 61
6.1.2 Dynamic deformation of single-crystal Cu pillars during in situ TEM compression 65
6.1.3 Stress-strain curves of single-crystal Cu nanopillars during in situ TEM compression 69
6.1.4 Nanoindentation 69
6.1.5 Vickers micro-hardness test 70
6.1.6 Comparison of the dynamic process and mechanical properties of single-crystal Cu nanopillars using experimental and simulation results 72



Chapter 7 NiAl alloys substrate and pillar structures 74
7.1 Results and discussion 74
7.1.1 Phase diagram and X-ray diffraction 74
7.1.2 Dynamic deformation of Ni30Al70 pillars utilizing in situ TEM compression test 76
7.1.3 Stress–strain curves of Ni30Al70 pillars 86
7.1.4 Nanoindentation 88
7.1.5 Vickers micro-hardness test 89
Chapter 8 NiTi alloys substrate and pillar structures 91
8.1 Results and discussion 91
8.1.1 Scanning electron microscope and X-ray diffraction 91
8.1.2 Dynamic deformation of NiTi pillars utilizing in situ TEM compression test 94
8.1.3 Load-displacement curves of NiTi nanopillars during in situ TEM compression 97
8.1.4 Stress-Strain curves of NiTi alloy nanopillars during in situ TEM compression 97
8.1.5 Nanoindentation test 100
8.1.6 Raman spectrum of NiTi alloy substrate 102
8.1.7 Vickers micro-hardness test 102
Chapter 9 Conclusions 105
References 108
Curriculum vitae 118
Publication list 118

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