臺灣博碩士論文加值系統

本實驗利用磁控濺鍍系統，以單晶矽(100)為基底，控制其他參數不變，通過改變V靶材不同的射頻功率，共鍍製備了CoCrFeMnNiVx (x = 0, 0.07, 0.3, 0.7, 1.1) 高熵合金薄膜，並討論了V的加入對該薄膜成分、結構與機械性質的影響。XRD的結果表明，當x=0, 0.07時，薄膜為單一的fcc結構；x = 0.3, 0.7, 1.1時，X-Ray繞射峰變寬，通過TEM結果得知，這是因為隨著V的含量增加，薄膜的結構趨於非晶態。TEM結果也表明，當x = 0, 0.07時，薄膜中存在大量雙晶，同時APT的結果表明，這兩個參數下的V原子完全嵌入晶格中，沒有產生析出物，這種微結構使得薄膜的機械性質顯著提升。利用奈米壓痕試驗，檢測了薄膜的微硬度和楊氏模數，可發現V的加入可使薄膜的微硬度有所提升，由約6.8 GPa提高至8.7 GPa。在x = 0.07時，楊氏模數達到最大值206.4 GPa，更高含量的V會使楊氏模數下降，這是由於薄膜中非晶相的產生，導致抵抗變形能力的降低，符合TEM的結果。薄膜的屈服強度、極限抗壓強度、壓縮延性及斷裂韌性由In-situ奈米壓痕試驗機經奈米柱壓縮試驗檢測。該壓縮應力-應變曲線表明，當V的含量為x = 0.07時，屈服強度可達為3.8 GPa，極限抗壓強度可達約4.9 GPa，並保持了約13%的壓縮延性。同時，x ≥ 0.3時，在壓縮後的奈米柱上發現剪切帶，且對應的應力-應變曲線呈現鋸齒流變，這些現象均表明非晶態的產生。觀察壓縮後的奈米柱的TEM結果得知，薄膜中產生的奈米雙晶在壓縮過程中有效緩衝了塑性形變，使薄膜的機械性質有大幅提升。

In the present work, CoCrFeMnNiVx (x = 0, 0.07, 0.3, 0.7, 1.1) high entropy alloy films were fabricated by magnetron co-sputtering. For low contents of V, typical face-centered cubic (fcc) peaks were identified in X-ray diffraction patterns. With the increasing V content, the diffraction peaks became broadening and the formation of amorphous phase was promoted. TEM observations showed abundant nanotwins in films with low V contents and the transition from fcc to amorphous structure with the increasing V content. The 3D APT reconstruction results revealed no precipitate in the as-deposited films (x = 0, 0.07). Mechanical properties of the films were studied using nanoindentation and micro-pillar compression tests. The films exhibited high hardness ranging from 6.8 to 8.7 GPa. The serrated flow associated with shear banding showed in the stress-strain curves for films with x ≥ 0.3. When x = 0.07, excellent yield strength of ~3.8 GPa and ultimate compressive strength of ~4.9 GPa were achieved with little sacrifice in ductility. The presence of nanotwins contributed to the strain hardening effect.

口試委員會審定書 #
ACKNOWLEDGEMENT i
中文摘要 ii
ABSTRACT iii
CONTENTS iv
LIST OF FIGURES vii
LIST OF TABLES xii
Chapter 1 Introduction 1
Chapter 2 Literature Review 5
2.1 High Entropy Alloys 5
2.1.1 Definitions of HEAs 5
2.1.2 Phase Formation Rules 7
2.1.3 Four Core Effects 8
2.1.4 Mechanical Properties of High-Entropy Alloys 10
2.2 High Entropy Alloy Films 12
2.2.1 Processing of High Entropy Alloy Films 12
2.2.2 Microstructure of High Entropy Alloy Films 13
2.2.3 Mechanical Properties of High Entropy Alloy Films 17
2.3 Introduction of CoCrFeMnNi 19
2.3.1 Microstructure and Mechanical Properties of CoCrFeMnNi 20
2.3.2 Heat Treatment to CoCrFeMnNi HEA 21
2.3.3 Al addition to CoCrFeMnNi HEA 22
2.3.4 Mo addition to CoCrFeMnNi HEA 24
2.3.5 Ti and C addition to CoCrFeMnNi HEA 25
2.3.6 V addition to CoCrFeMnNi HEA 26
2.3.7 CoCrFeMnNi HEAF 28
Chapter 3 Experimental Procedure 30
3.1 Target and Substrate Preparation 30
3.2 Deposition Process 31
3.3 Analysis Equipment 32
3.3.1 X-ray diffraction 32
3.3.2 SEM Observation 32
3.3.3 TEM Observation 33
3.3.4 3D APT reconstruction 33
3.3.5 Nanoindenter 33
3.3.6 Picoindenter 34
Chapter 4 Results and Discussion 36
4.1 Microstructure 36
4.1.1 Chemical Compositions 36
4.1.2 XRD Results 37
4.1.3 TEM Observations 38
4.1.4 3D APT Reconstructions 41
4.1.5 TKD Observations 41
4.2 Mechanical Properties 42
4.2.1 Nanoindentaion 42
4.2.2 Picoindentation 44
Chapter 5 Conclusions 50
References 51

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