在本論文中，利用奈米壓痕技術去探討殘留應力對於塊狀金屬玻璃潛變之影響，為了在塊狀金屬玻璃中產生殘留應力，所使用的方法是將塊狀金屬玻璃彎曲限制在金屬圈中，而被彎曲的塊狀金屬玻璃試片其上半部就會存在張應力而下半部就會存在壓應力，經過奈米壓痕潛變測試後可得知，在張應力存在部分其潛變應變速率會明顯大於壓應力的部分，此現象可經由殘留應力對試片結構影響來解釋。

研究也針對鋯銅非晶薄膜、鋯奈米晶薄膜和鋯銅/鋯多層膜進行奈米壓痕潛變的研究，在研究中發現了潛變速率會因為施加應力的改變而發生了交叉現象，跟鋯銅非晶薄膜比起來鋯奈米晶薄膜擁有較高的應力靈敏度，這是因為鋯奈米晶薄膜擁有差排在不同滑移系統下的變形機制和晶界滑移的變形機制，而相對於單層薄膜，鋯銅/鋯多層膜表現出較高的潛變應變速率這是因為眾多界面的貢獻所造成。

最後，利用物理濺鍍製備鋯銅非晶薄膜/鋯奈米晶薄膜的多層膜試片(每層500 nm厚)，並且利用聚焦離子束去加工製備出擁有傾斜界面的奈米柱，這些傾斜界面奈米柱可以去探討壓縮應力方向與界面之間在不同的角度關係下的現象，實驗的結果與分子動力學的模擬和Tsai-Hill模型去針對楊氏模數和降伏應力做比較，可得知鋯銅非晶薄膜/鋯奈米晶薄膜的界面剪切模數和界面強度分別是25 GPa和1.0 GPa，透過分子動力學的模擬可了解奈米柱在彈性-塑性的變形現象和模式，實驗的結果與模擬的計算結果相當吻合。


關鍵字：金屬玻璃、多層膜、機械性質、潛變、界面

In this research, the effect of residual stresses on the time-dependent deformation of a bulk metallic glass is investigated by the nanoindentation technique. In order to induce residual stresses, a beam sample was elastically bent and constrained in a steel ring. The upper side of the beam experiences the tensile residual stress, the lower side the compressive residual stress, and the central line nearly nil stress. Afterward, nanoindentation creep tests are performed on this stressed sample at room temperature. The creep rate is apparently higher on the tensile side, and remains lower and nearly fixed on the compressive side. The behavior can be explained by the joint influence of the residual stress and indention loading.

We also attempt to investigate the nanoindentaion time-dependent relaxation tests were performed on the amorphous ZrCu, nanocrystalline Zr and multilayer ZrCu/Zr thin films aiming to explore the different time-dependent behaviors of these materials under the similar load level at room temperature. There appears an interesting crossing phenomenon of the creep rate as a function of applied stress. In comparison with the ZrCu thin films, the Zr film shows higher load/stress sensitivity for the creep response, suggesting the operating of dislocation creep along various slip systems and some minor grain-boundary-sliding creep mechanism. Multilayered ZrCu/Zr thin films also exhibit higher creep response due to the presence of numerous interfaces.

Eventually, an amorphous-ZrCu/crystalline-Zr nanolaminate (500 nm each layer) was initially synthesized using sputter deposition and, then, fabricated into micropillar samples using focus ion beam machining with the amorphous-crystalline (a-c) interfaces inclined to the pillar axis. These pillars were, subsequently, tested in compression in order to study the response of a-c interfaces to the applied shear stress, and further compared with the one that tested with their a-c interfaces normal to the compressive direction. Comparison was made on the experimental, MD and Tsai-Hill data on modulus and yield strength as a function of the angle φ with respect to the loading axis. The extracted interface shear modulus and interface strength for the current ZrCu/Zr is about 25 GPa and 1.0 GPa, respectively. Molecular dynamic simulations are also carried out to reveal the elastic-plastic behavior and, in particular, the deformation mode, of the pillars. The computed results are in excellent agreement with the experimental observations.


Keywords: Metallic glasses, Multilayer, Mechanical properties, Creep, Interface

論文審定書 i
致謝 ii
中文摘要 iv
Abstract v
Content vii
List of tables xi
List of figures xii
Chapter 1 Introduction 1
1.1 Amorphous alloys 1
1.2 The evolution of amorphous alloys and bulk metallic glasses (BMGs) 2
1.3 The development of thin film metallic glasses (TFMGs) 3
1.4 Motivation 5
Chapter 2 Background and literature review 8
2.1 The evolution of fabrication methods 8
2.2 The characters and forming conditions of amorphous alloys 8
2.2.1 Glass forming ability 8
2.2.2 The empirical rules for forming amorphous alloys 11
2.3 Sputtering deposition process 12
2.3.1 Introduction of sputtering 12
2.3.2 Nucleation and growth of sputter-deposited films 13
2.3.3 Amorphous film growth 13
2.4 The characterization of amorphous alloys 13
2.4.1 Mechanical properties 14
2.4.2 Magnetic properties 14
2.4.3 Chemical properties 14
2.5 The deformation mechanisms of metallic glasses 15
2.6 Thin film materials 16
2.6.1 Mechanical properties of multilayer thin films 16
2.6.2 Applications of thin film metallic glasses 18
2.7 Nanoindentaion creep tests 19
2.8 Microscale mechanical properties 21
2.8.1 Introduction to microcompression tests 22
2.8.2 Microscale mechanical properties on monolithic amorphous micropillars 26
2.8.3 Microscale mechanical properties on multilayer micropillars 27
2.9 Focused ion beam (FIB) 29
2.9.1 Introduction to FIB 29
2.9.2 Ion induced damage 30
2.10 Nanoscale tensile tests 31
Chapter 3 Experimental procedures 34
3.1 Raw materials 34
3.2 Substrate preparation 34
3.3 Sample preparation by sputtering 35
3.4 Materials characterization 36
3.4.1 X-ray diffraction (XRD) 36
3.4.2 SEM and EDS analyses 36
3.5 Nanoindention tests 36
3.6 Nanoindention creep tests 37
3.7 Microcompression tests 37
3.7.1 Perparation for microcompression samples 37
3.7.2 Microcompression tests using nanoindentation system 38
3.8 Simulation 38
Chapter 4 Results and discussions 40
4.1 Effect of residual stresses on nanoindentation creep behavior of Zr-based BMG 40
4.1.1 Sample preparations 40
4.1.2 The parameters of nanoindentaion creep 40
4.1.3 Bending properties of ZrAlTiCuNi BMG beam sample 41
4.1.4 Time-dependent deformation behavior of bent ZrAlTiCuNi BMG beam sample 41
4.2 Nanoindentation creep behavior of amorphous ZrCu, nanocrystalline Zr and multilayers thin films 46
4.2.1 Sample preparations 46
4.2.2 The parameters of nanoindentaion creep 46
4.2.3 EDS and XRD analyses 47
4.2.4 Mechanical properties of amorphous ZrCu and nanocrystalline Zr 47
4.2.5 Time-dependent deformation behavior of amorphous ZrCu and nanocrystalline Zr 48
4.2.6 Time-dependent deformation behavior of ZrCu/Zr multilayer composites 52
4.3 Mechanical properties of amorphous ZrCu/crystalline Zr multilayers with inclined interfaces 54
4.3.1 Experimetal observations 54
4.3.2 Simulation findings 56
4.3.3 Comparison with Tsai-Hill composite model 57
4.3.4 On the interface strength 59
4.4 Extended elastic region in nanocrystalline metals under nano-tension testing 59
4.4.1 XRD analyses 59
4.4.2 Nano-tension tests 60
4.4.3 MD simulation results 62
4.4.4 Ga+ damage during FIB 64
Chapter 5 Conclusions 66
References 68-76
Tables 77-79
Figures 80-154

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