為了解決在多層膜結構下，受應力導致延界面脫層的現象，在本研究中，嘗試利用漸進區的產生以試圖消除多層膜之陡變界面。我們利用磁控濺鍍系統製備出以下三種不同型態的非晶質鋯銅/奈米晶純銅的多層膜結構：一、界面無漸進層「ZCC-G0」，二、界面處具有五十奈米厚漸進層「ZCC-G50」，三、界面處具有一百奈米厚漸進層「ZCC-G100」。在漸進結構中，可以觀察到非晶質母相中有奈米晶純銅析出，其組成成分變化、析出之奈米晶尺寸、奈米晶體積分率，以及試片橫截面的楊氏模數變化均呈現了梯度變化的特性。為了瞭解漸進區對整體試片機械性質的貢獻，我們利用奈米刮痕測試、奈米拉伸測試，以及奈米撓曲測試進行以下研究。

在奈米刮痕測試中，我們首次利用破裂韌性隨外加正向力的變化的關係，來判斷界面脫層的發生時機並找出其脫層力，而此種方法並不會因負載率的變化而導致不同結果。在鋯銅與銅的多層膜結構中，試片ZCC-G0於正向力達到1460毫牛頓時會發生界面脫層現象。而其餘兩種結構，ZCC-G50與ZCC-G100則無明顯脫層情形發生。

在奈米拉伸實驗中，我們透過聚焦離子束將試片加工為奈米尺度的拉伸試片，利用奈米壓痕系統配備一圓錐頭，在刮痕模式下對試片進行拉伸側試。唯因薄膜厚度之限制，使奈米壓痕系統之鑽石頭無法帶動拉伸試片移動，導致實驗無法成功，但此測試手法卻對未來進行奈米尺度拉伸實驗帶來許多可能。

在奈米撓曲實驗中，我們利用聚焦離子束系統將試片製為倒凸型結構，以利在測試過程中使外加力集中於介面處。在ZCC-G0的測試結果，其界面撓曲破裂應力為1.9 ± 0.1 GPa、撓曲應變約為11 ± 1%。而具有漸進結構的ZCC-G50與ZCC-G100試片，其界面撓曲破裂應力為2.8 ± 0.1 GPa、撓曲應變約為18 ± 1%。此一結果展現出當多層膜結構中具有漸進結構時，會對整體機械性質，不論是在撓曲破裂應力、撓曲應變帶，以及撓曲模數上帶來超過百分之五十的大幅強化，並展現類似韌性材料的變形行為。

In this study, to solve the delamination behavior along the interface, graded regions were fabricated to erase the sharp interface. Three kinds of the amorphous ZrCu/ nanocrystalline Cu multilayered structures, namely, without graded region (ZCC-G0), with 50 nm graded region (ZCC-G50) and with 100 nm graded region (ZCC-G100), are manufactured by the magnetron co-sputter system. In the graded region, there are Cu nanoparticles distributed in the amorphous matrix. The graded region possesses the gradient nature in terms of composition, nanocrystalline phase size, nanocrystalline volume fraction, and cross sectional modulus distribution from the amorphous ZrCu to the nanocrystalline Cu. To figure out the mechanical properties enhancement by the graded region, nano-scratch, nano-tension, and nano-bending tests were applied in this study.

For the nano-scratch testing, we first used the variation of fracture toughness as a function of normal force to determine the delamination point. And this method is considered not to be influenced by the loading rate. ZrCu/Cu interface delaminated when the applied normal force reached to 1460 μN for ZCC-G0, and no obvious interface delaminated behavior could be found for both ZCC-G50 and ZCC-G100.

For thenano-tension testing, nano-scaled tension samples are designed and fabricated by focus ion beam. The nano-scaled tension tes is performed by the nanoindentation system equipped a conical tip with scratch mode. Although this test failed due to the limitation of the film thickness, the tip could not drag the tension sample successfully, but it brings many possible ways for the nano-scaled tensile testing with scratch mode.

For the nano-bending testing, T-shaped cantilevers are designed and fabricated by focus ion beam to let the applied force concentrate on the interface region during testing. The nano-bending test is performed by an in-situ nanoindentation system. For the ZCC-G0 samples interface bending fracture stress is 1.9 ± 0.1 GPa, and the bending strain is about 11 ± 1%. The interface bending fracture stress, for the ZCC-G50 and ZCC-G100 samples is 2.8 ± 0.2 GPa, and the bending strain is about 18 ± 1%. These results demonstrated that multilayered thin films with graded structure would be inherited with a much higher interface strength/strain/modulus, with an overall improvement upgrade of more than 50% and a ductile failure manner.

論文審定書 i
誌謝 ii
中文摘要 v
Abstract vii
Contents ix
List of tables xiii
List of figures xiv
Chapter 1 Introduction 1
1-1 Amorphous alloys 1
1-2 The progress of bulk metallic glasses 2
1-3 The development of Zr-based metallic glasses 3
1-4 Motivation 4
Chapter 2 Background and literature review 7
2-1 Background of amorphous alloys 7
2-1-1 Supercooled liquid region (SCLR) 7
2-1-2 The empirical rule for forming amorphous alloys 7
2-1-3 Glass forming ability (GFA) 8
2-2 Sputtering deposition 10
2-2-1 Deposition rate with the system condition 11
2-2-2 Growth of sputter-deposited film 12
2-3 Mechanical properties of metallic glass composites 14
2-3-1 Secondary phase 15
2-3-2 Modulus mismatch 16
2-3-3 Rule of mixture 17
2-4 Amorphous/crystalline multilayered thin film 18
2-5 Mechanical properties measured by nanoindentation 20
2-5-1 Hardness and modulus 21
2-5-2 Modulus Mapping 23
2-5-3 Limitation of Modulus Mapping 26
2-5-4 Adhesion property measurement by scratch test 27
2-6 The feature of focus ion beam (FIB) 28
2-6-1 FIB imaging 30
2-6-2 FIB milling 31
2-6-3 FIB deposition 31
2-6-4 TEM sample preparation 32
2-7 Nano-scale mechanical property testing 33
2-7-1 Nano-tension testing 33
2-7-2 Micro-bending testing 35
Chapter 3 Experimental procedures 39
3-1 Materials 39
3-2 Sample preparation 40
3-2-1 Pretreatment for substrate 40
3-2-2 Preparation for thin films and multilayer thin films 40
3-3 Property measurements and analyses 41
3-3-1 X-ray diffraction 41
3-3-2 Cross-section-view TEM analysis 42
3-3-3 Cross-section-view qualitative and quantitative component analyses 42
3-3-4 Cross sectional modulus mapping 43
3-3-4-1 Sample preparation 43
3-3-4-2 Equipment for the modulus mapping 43
3-4 Scratch testing 43
3-4-1 Sample preparation 44
3-4-2 Scratch test equipment 44
3-5 Nano-tension testing 44
3-5-1 Sample preparation 44
3-5-2 Nano-tension test equipment 45
3-6 Nano-bending testing 46
3-6-1 Sample preparation 46
3-6-2 Nano-bending test equipment 46
Chapter 4 Results and discussions 48
4-1 Characterizations of ZrCu/Cu miltilayered thin films 48
4-1-1 XRD results 48
4-1-2 Microstructures confirmed by TEM analyses 48
4-1-3 Composition profile measured by STEM and EDS analyses 50
4-1-4 Graded region modulus mapping results 51
4-1-5 The formation of graded region 52
4-2 Scratch test results 53
4-2-1 ZrCu/Cu bilayered thin film results 54
4-2-2 Fracture toughness calculation in the scratch test 54
4-2-3 Monolithic ZnO thin film results comparison 56
4-2-4 Variety of KC in ZrCu/Cu bilayered structure 60
4-3 Nano-tension test results 61
4-4 Nano-bending test results 64
4-4-1 Interface strengthening mechanism 66
Chapter 5 Conclusions 70
Chapter 6 Future work 72
References 73
Tables 83
Figures 88

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