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研究生:Nguyen Van Cuong
研究生(外文):Nguyen Van Cuong
論文名稱(外文):Study on the mechanical properties of nickel coating electrodeposited in electrolyte mixed with supercritical carbon dioxide
指導教授(外文):Chun-Ying Lee
口試委員:林景崎張六文林 招松黃榮堂
口試委員(外文):Jing-Chie LinLiuwen ChangChao-Sung LinJung-Tang Huang
外文關鍵詞:Electrodepositionsupercritical carbon dioxideinternal stressnano- crystalline nickelSc-CO2 chargingCO2 bubblepost Sc-CO2
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本論文研究在分別有、無混合超臨界二氧化碳的瓦特浴鍍液中進行各項控制參數下之鎳電鍍製程,由超臨界二氧化碳(Sc-CO2)輔助電鍍的試片分析與傳統電鍍試片進行機械性質比較,以研究超臨界二氧化碳在製程中所扮演之角色。探討不同微結構、結晶狀態電鍍層之內應內為本研究的重要研究任務之一。此外,發展所謂的後超臨界二氧化碳(post Sc-CO2)電鍍新製程技術也是本研究的重要貢獻。
實驗結果顯示,在超臨界二氧化碳電鍍的鎳鍍層比起傳統電鍍較有光亮平整和較高硬度的表面。然而,藉由穿透式電子顯微鏡(TEM)和原子力顯微鏡(AFM)的實驗中發現在超臨界二氧化碳電鍍鎳層中存在著奈米等級的針孔,而這些針孔就是在超臨界二氧化碳高壓環境下影響鍍層的內應力,這種結果造成了在超臨界二氧化碳電鍍鎳的試片內應力遠遠大過於傳統電鍍鎳的鍍層。研究中也發現了鎳鍍層的內應力與其晶粒尺寸和X光繞射量測之{200} /{111} 晶格優選方向峰值比值成反比關係。較小的晶粒尺寸,伴隨有較高{111}優選方位,導致高內應力的鍍層,反之亦然。本研究提出之理論模型考量晶粒尺寸和結晶的優選方向,其結果和不同實驗參數下製備的鍍層內應力量測結果有著相當的一致性。此外,在超臨界二氧化碳混和之電鍍液中加入了界面活性劑會提高鎳鍍層的內應力。然而,要有效的降低鍍層的內應力,可以藉由以下的四個方法來進行改善:提高電流密度、增加鍍液溫度、降低電鍍槽體壓力和在電鍍液中加入糖精(Saccharin)。
另外一方面,藉由後超臨界二氧化碳混合瓦特浴電鍍液之電鍍製程,可以獲得晶粒尺寸小於50 nm之鎳鍍層。後超臨界二氧化碳鎳鍍層具有大於650 Hv之硬度,但是比起超臨界二氧化碳電鍍鎳有明顯的下降且晶粒尺寸稍有變大,雖然如此,後超臨界環境下的電鍍層表面還是較光亮、平整,且在大氣中進行之後超臨界電鍍層,也在鍍層中量測碳原子的存在。顯然地,後超臨界二氧化碳電鍍鎳製程提供了一種新的超臨界電鍍方法,可以提供較大工件及連續電鍍在超臨界二氧化碳輔助下改善鍍層性質之可行性。最後,本論文提供如何進一步提高鎳鍍層的機械性質及促進新電鍍製程實用化之方法建議。

The electrodeposition of nickel film, with and without the mixing of supercritical carbon dioxide (Sc-CO2) in the Watts bath electrolyte, was performed in this work under various plating conditions. The specimens from Sc-CO2 assisted plating were then analyzed and the results were compared with their conventional counterparts for the discussion of the underlined mechanisms. A thorough study on the internal stress in deposited nickel film, its controlled mechanism and the relationship between crystalline structure and internal stress, was one of the important tasks of this study. A proposed new electroplating technique so-called post Sc-CO2 was the other useful contribution.
As the results, the Ni films plated in Sc-CO2 had brighter, smoother surface, smaller grains and higher hardness than that plated in conventional electrolyte without Sc-CO2. However, there existed more nano-sized pinholes observed by SEM, TEM and AFM measurements on the Sc-CO2 specimens. This special appearance affected coating properties under such a high pressure condition through the Sc-CO2 charging. The result showed that the internal stress in the nickel film plated through the Sc-CO2 method was significantly higher than that in the conventional one. A relationship was found that the internal stress of the Ni coating was inversely proportional to its grain size and the Ni{200}/Ni{111} peak fraction in the measured X-ray diffraction pattern. The smaller grain size, accompanied with higher Ni{111} texture, resulted in higher internal stress of the coating, and vice versa. A proposed theoretical model, which took both the grain size and preferred crystalline orientation into account, correlated closely with experimental results in the internal stress of the coatings prepared using different processes. The presence of surfactant in the Sc-CO2 electrolyte increased the internal stress of Ni coating. However, a reduction of internal stress was made possible by varying four factors: the raising of current density, the increasing of plating temperature, the lowering of plating pressure, and the addition of saccharin into electrolyte.
On the other hand, by using the post Sc-CO2 mixed electrolyte, the obtained nickel coating had the grain size in the range less than 50nm. The micro hardness of post Sc-CO2 nickel film was greater than 650 Hv. Both the grain size and hardness of the post Sc-CO2 specimen fall between its conventional and real Sc-CO2 counterparts. Moreover, the post Sc-CO2 specimen had bright, smooth, and uniform surface. The incorporation of C in Ni electrodeposit was also detected in the post Sc-CO2 coating, which had been plated under the atmospheric condition. Apparently, this new plating method presents a promising alternative to solve the issues associated with the requirement of large autoclave for big work-piece and the adaption to continuous electroplating for using supercritical plating method.
Finally, this work investigated how to further enhance the mechanical properties of the nickel deposited films as well as the facilitation of the electrodeposition via this new electroplating method. Some useful suggestions for designing Sc-CO2 electroplating system and configuring plating condition were also addressed.

摘要 i
Abstract iii
Acknowledgements iv
Contents v
List of Tables viii
List of Figures ix
Chapter 1 Introduction 1
Chapter 2 Background 3
2.1 Introduction 3
2.2 Supercritical carbon dioxide 3
2.3 Nickel 5
2.4 Electrodeposition 8
2.4.1 Fundamentals and terminologies 8
2.4.2 Electrodeposition using electrolyte mixed with Sc-CO2 11
2.4.3 Periodic plating characteristics 11
2.5 Internal stress in coatings 13
2.6 Literature review 14
2.7 Motivation of this study 18
Chapter 3 Experimentation 20
3.1 Introduction 20
3.2 Experiment details 21
3.2.1 Materials 21
3.2.2 Apparatus 23
3.2.3 Analyses 27
3.2.4 Grain size and micro hardness measurements 27
3.2.5 Internal stress measurement 28
Chapter 4 Mechanical properties of nickel electrodeposits 31
4.1 Introduction 31
4.2 Surface morphology 31
4.3 Crystal texture and microhardness 32
4.4 Effect of Boric acid on surface morphology and crystal orientation 35
4.5 Presence of nano-sized pinholes in deposit 38
4.6 Defects on nickel coating 46
Chapter 5 Internal stress in nickel coatings 48
5.1 Introduction 48
5.2 Internal stress of coating 48
5.3 Determination of Sc-CO2 recharge effect 51
5.4 The effects of plating pressure and temperature 54
5.5 The effect of plating current density 56
5.6 The effect of additives in the electrolyte 59
5.7 Relationship between crystallite structure and internal stress 61
Chapter 6 The post Sc-CO2 electroplating- A new technique 68
6.1 Introduction 68
6.2 Appratus and process procedure 70
6.2.1 Plating system 70
6.2.2 Evaluation of CO2 diffusing/releasing from electrolyte 72
6.2.3 Electroplating procedure 75
6.3 Surface morphology of nickel coating 76
6.3.1 Effects of duration of post Sc-CO2 electrolyte exposure 76
6.3.2 Effects of electrodeposition time 78
6.3.3 Comparison between different plating methods 79
6.3.4 Effects of Saccharin 82
6.4 Crystal structure and hardness 83
6.5 Incorporation of carbon in nickel coating 88
Chapter 7 Conclusions 91
7.1 Conclusions 91
7.2 Suggestions for future works 92
List of publications 94
Literature references 95
Nomenclatures 101

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