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研究生:賴炎暉
研究生(外文):Yen-Huei Lai
論文名稱:以微米壓縮量測不同金屬玻璃微米柱之尺寸效應
論文名稱(外文):Effects of Sample Size on Various Metallic Glass Micropillars in Microcompression
指導教授:黃志青黃志青引用關係
指導教授(外文):Chih-Ching Huang
學位類別:博士
校院名稱:國立中山大學
系所名稱:材料與光電科學學系研究所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2009
畢業學年度:98
語文別:英文
論文頁數:204
中文關鍵詞:玻璃微米壓縮測試尺寸效應
外文關鍵詞:microcompression testssample size effectmetallic glass
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在過去的幾十年中,塊狀金屬玻璃已經引起廣泛注意,由於它具備了許多優異的特
性,例如良好的抗腐蝕能力、大的彈性能、高的強度以及硬度等等。然而,由於微機電
系統以及其他微米尺度元件的出現,微米尺度下金屬玻璃的基本機械性質變得越來越重
要。因此,本研究論文中,才會使用單軸微米壓縮測試技術在金屬玻璃上做分析。
不同尺寸大小之Mg65Cu25Gd10 與Zr63.8Ni16.2Cu15Al5 金屬玻璃微米柱已經成功地藉
由聚焦離子束來製備,接著以不同應變速率在室溫下進行微米壓縮測試。其結果發現,
鎂基與鋯基金屬玻璃具有明顯的尺寸效應,也就是說當材料的尺寸變小時,其強度是呈
現上升。而強度的上升也可以藉由Weibull 方程式來做說明及統計,鎂基與鋯基金屬玻
璃之Weibull modulus 分別估算為35 與60。在鋯基金屬玻璃中測得較高Weibull modulus
也符合這個成分的金屬玻璃比較具有延性之特性。
此外,藉由高溫微米壓縮系統研究微米尺度下Au49Ag5.5Pd2.3Cu26.9Si16.3 金屬玻璃在
室溫到其玻璃轉化溫度之變型行為。對於1 μm 尺寸之金基金屬玻璃微米柱而言,發現
在玻璃轉化溫度附近有一個明顯的轉變,其變形機制由不均勻的變形到均勻的變形。結
果發現,這個明顯的轉變大約發生在應變速率1 x 10-2 s-1 以及溫度393 K 下。
而對於3.8 μm 尺寸之金基金屬玻璃微米柱而言,進一步利用高溫微米壓縮測試來
研究金基金屬玻璃在溫度395.9-401.2 K 下的均勻變形行為。其結果發現,微米尺度下
金基金屬玻璃之強度隨溫度上升而下降;隨應變速率下降而下降。而塑性變形行為可以
利用金屬玻璃之變形模型來做分析。其結果發現,變形時之活化能以及尺寸大小都可利
用此變形模型推算出來,且經比較發現結果符合其理論。
Over the past decades, bulk metallic glasses (BMGs) have attracted extensive interests
because of their unique properties such as good corrosion resistance, large elastic limit, as
well as high strength and hardness. However, with the advent of micro-electro-mechanical
systems (MEMS) and other microscaled devices, the fundamental properties of
micrometer-sized BMGs have become increasingly more important. Thus, in this study, a
methodology for performing uniaxial compression tests on BMGs having micron-sized
dimensions is presented.
Micropillar with diameters of 3.8, 1 and 0.7 μm are fabricated successfully from the
Mg65Cu25Gd10 and Zr63.8Ni16.2Cu15Al5 BMGs using focus ion beam, and then tested in
microcompression at room temperature and strain rates from 1 x 10-4 to 1 x 10-2 s-1.
Microcompression tests on the Mg- and Zr-based BMG pillar samples have shown an
obvious sample size effect, with the yield strength increasing with decreasing sample
diameter. The strength increase can be rationalized by the Weibull statistics for brittle
materials, and the Weibull moduli of the Mg- and Zr-based BMGs are estimated to be about
35 and 60, respectively. The higher Weibull modulus of the Zr-based BMG is consistent with
the more ductile nature of this system.
In additions, high temperature microcompression tests are performed to investigate the
deformation behavior of micron-sized Au49Ag5.5Pd2.3Cu26.9Si16.3 BMG pillar samples from
room to their glass transition temperature (~400 K). For the 1 μm Au-based BMG pillars, a
transition from inhomogeneous flow to homogeneous flow is clearly observed at or near the
glass transition temperature. Specifically, the flow transition temperature is about 393 K atthe strain rate of 1 x 10-2 s-1.
For the 3.8 μm Au-based BMG pillars, in order to investigate the homogeneous
deformation behavior, microcompression tests are performed at 395.9-401.2 K. The strength
is observed to decrease with increasing temperature and decreasing strain rate. Plastic flow
behavior can be described by a shear transition zone model. The activation energy and the
size of the basic flow unit are deduced and compared favorably with the theory.
Table of Content i
List of Tables v
List of Figures vii
Abstract xvi
中文摘要 xviii
Chapter 1 Introduction 1
1-1 Amorphous alloys 1
1-2 The evolution of Mg-, Zr- and Au-based amorphous alloys 2
1-3 The sample size effect on amorphous alloys 5
1-4 Motives of this research 7
Chapter 2 Background and Literature Review 10
2-1 The history of amorphous alloys 10
2-2 The systems of amorphous alloys 12
2-3 The indices for predicting glass forming ability (GFA) 13
2-4 The main empirical rules for the synthesis of amorphous alloys 16
2-5 Properties and behaviors of amorphous alloys 19
2-5-1 Mechanical properties 19
2-5-2 Deformation mechanisms 20
2-5-3 Characterization of shear bands 22
2-5-4 Deformation behavior 23
2-5-5 Deformation model 26
2-6 Introduction of microcompression tests 28
2-6-1 Microsample preparation 29
2-6-2 Force application and measurement 32
2-6-3 Parameters of microcompression tests 32
2-6-4 Microscale characterization of mechanical properties 35
Chapter 3 Experimental Procedures 39
3-1 Materials 39
3-2 Sample preparation 40
3-2-1 Preparation for Mg65Cu25Gd10 40
3-2-2 Preparation for Zr63.8Ni16.2Cu15Al5 41
3-2-3 Preparation for Au49Ag5.5Pd2.3Cu26.9Si16.3 43
3-3 Property measurements and analyses 44
3-3-1 XRD and SEM/EDS characterization of as-cast ingots 44
3-3-2 Thermal analysis using DSC 44
3-3-3 Microstructure analysis using TEM 45
3-4 Microcompression test 45
3-4-1 Microcompression sample fabrication using FIB 45
3-4-2 Microcompression test using nanoindentation system 46
3-4-3 Morphology of deformed pillar samples 46
3-4-4 Microstructures of deformed pillar samples 47
3-5 High temperature microcompression test 47
3-5-1 MTS Nanoindenter XP system 48
3-5-2 Hysitron Triboindenter system 48
3-6 Nanoindentation measurements 49
3-6-1 Elastic modulus and hardness 49
3-6-2 Abrasive wear 50
Chapter 4 Experimental Results 51
4-1 XRD and SEM/EDS analysis 51
4-2 DSC analysis 51
4-3 TEM analysis 52
4-4 Microcompression test 54
4-4-1 Results for Mg65Cu25Gd10 54
4-4-2 Results for Zr63.8Ni16.2Cu15Al5 56
4-4-3 TEM analysis of the microstructure in pillar sample 58
4-5 High temperature microcompression test 60
4-5-1 Results for Au49Ag5.5Pd2.3Cu26.9Si16.3 using MTS Nanoindenter 60
4-4-2 Results for Au49Ag5.5Pd2.3Cu26.9Si16.3 using Hysitron Triboindenter 62
4-6 Nanoindentation and nanoscratch test 63
4-6-1 Elastic modulus and hardness 64
4-6-2 Abrasive wear behavior 64
Chapter 5 Discussions 66
5-1 Room temperature microcompression test 66
5-1-1 Evolution of Young''s modulus 66
5-1-2 Effect of FIB damage 68
5-1-3 Weibull statistics 69
5-1-4 Sample size and strain rate effect 71
5-1-5 Strain burst phenomena 73
5-1-6 Strain burst speed 75
5-2 High temperature microcompression test 78
5-2-1 Effect of temperature on mechanical behavior 78
5-2-2 Homogeneous flow 80
Chapter 6 Conclusions 83
References 86
Tables 97
Figures 113
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