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研究生： Getinet Asrat Mengesha
Getient Asrat Mengesha
論文名稱： 以液態電漿氧化技術改善純鋁抗腐蝕與附著強度之研究
Research of the corrosion resistance and adhesion strength improvement on pure aluminum by plasma electrolytic oxidation technique
指導教授： 朱瑾
Jinn P. Chu
李志偉
Jyh-Wei Lee
口試委員: 朱瑾
Jinn P. Chu
李志偉
Jyh-Wei Lee
駱碧秀
Bih-Show Lou
葛明德
Ming-Der Ger
郭俞麟
Yu-Lin Kuo
學位類別： 博士
Doctor
系所名稱： 工程學院 - 材料科學與工程系
Department of Materials Science and Engineering
論文出版年： 2020
畢業學年度： 108
語文別： 英文
論文頁數： 130
中文關鍵詞： 電漿電解氧化 、純鋁 、Si3N4奈米顆粒 、硼砂 、耐蝕性 、附著強度 、摩擦係數
外文關鍵詞： Plasma electrolytic oxidation, pure aluminum, Si3N4 nanoparticle, borax, corrosion resistance, adhesion strength, coefficient of friction
相關次數： 點閱：339  下載：0 
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    • 摘要
    鋁已廣泛用於工業和日常生活中。鋁最常見的用途是建造運輸工具（因更輕的重量使得移動交通工具只需更少的力，從而提高了燃油效率）、電纜應用（低密度使其成為長距離輸電線的最佳選擇）、消費品（智能手機、平板電腦、筆記型電腦和平板電視）以及建築材料（高鐵、地鐵，輪船和火箭的建造）。然而，由於鋁在腐蝕環境中有較差的耐腐蝕性能和較低的表面硬度，因而限制其應用範圍。因此已有許多方法來控制鋁的損壞速率，其中電漿電解氧化（PEO）是最有前途的方法。 PEO是一種電漿輔助陽極氧化製程，可以將鋁的表面轉化為陶瓷層，從而防止腐蝕性介質接觸基材。因此可以降低其腐蝕速率。此外，在PEO製程使用適當的電解質可以產生高度保護性的鍍層。由於鋁具有可貴的性質，因此已有許多人投入PEO的研究，以提升其腐蝕保護力及表面硬化能力。本研究中有系統的研究純鋁的PEO技術及其產生的氧化層特性。透過漸進式的研究，有效地提高了純鋁的耐腐蝕性能和氧化層附著強度。
    在第一個研究中，固定電源頻率，使用兩種不同的鹼性電解質，並改變添加Si3N4奈米粒子的濃度（0、0.5和1.5 gL-1）和不同的電源佔空比（25％，50％和80％）。藉由在3.5 wt%的NaCl溶液中的動電位極化試驗研究PEO氧化層的抗腐蝕性能。由結果顯示，隨著Si3N4奈米顆粒的濃度和佔空比的增加，PEO生長的氧化層重量、厚度和表面粗糙度增加。使用Na2B4O7.10H2O的電解質所生長的氧化物比其他添加Si3N4奈米顆粒生長的PEO氧化層具有優異的耐腐蝕性和低表面粗糙度。然而，在電解液中添加Si3N4奈米顆粒並不能改善PEO薄膜的腐蝕性能，這是因為無法形成緻密的微結構使然。
    在第二個研究，改變電解質添加硼砂（Na2B4O7.10H2O）的濃度(0、1.5、3、4.5和6 gL-1)，並固定佔空比、固定陽極和陰極電流的雙極脈衝模式電源來對純Al進行PEO處理。本研究使用動電位極化試驗和電化學阻抗分析來探討氧化層在3.5 wt% NaCl溶液的耐腐蝕性。我們發現，隨著硼砂濃度的增加，PEO生長氧化膜的表面平均孔徑和孔隙率降低。當電解液中含有高濃度硼砂時，可以形成緻密結構的氧化膜。，使得PEO生成的氧化層耐蝕性增加。藉由使用含有6 gL-1硼砂的電解液來對純鋁做PEO處理可使其耐蝕性得到極大的提升，達23058倍，這是因為氧化層是緻密的γ-Al2O3相且具有較少的缺陷所致。
    在第三個研究中，使用不同的佔空比（25％，50％和80％）和固定頻率，在矽酸鈉基電解液添加不同濃度的Si3N4（0-2.5 gL-1）奈米顆粒。由結果顯示，PEO崩潰電壓隨著Si3N4奈米顆粒濃度的增加而降低，並且隨著佔空比的增加而降低。隨著添加Si3N4奈米顆粒濃度的增加，PEO生長的氧化層厚度，表面粗糙度和附著強度也隨之增加。若是使用固定Si3N4添加濃度（2.5 gL-1）的電解液來做PEO處理，其生成氧化物的表面粗糙度，厚度和摩擦係數隨著佔空比的降低而降低。另一方面，當佔空比從80％降低到25％時，附著強度和耐磨性也有增加的趨勢。使用2.5 gL-1 Si3N4奈米顆粒電解液，佔空比為25％的PEO製程所生長的氧化層，具有最佳的附著強度，14.85 N及較低的摩擦係數。最後我們可以結論，於PEO電解質中添入硼砂和Si3N4奈米顆粒會影響純鋁生成氧化層的耐腐蝕性和附著強度。

    Abstract
    Aluminum has been widely used in industry and daily life. The most common use of aluminum is to construct transportation, electrical, consumer goods and construction materials. However, the application of aluminum material is still limited due to its intrinsically poor corrosion performance in the corrosive environments and low surface hardness. Therefore, various methods have been explored to control the degradation rate of aluminum, of which plasma electrolytic oxidation (PEO) is the most promising method. PEO is a plasma-assisted anodising process that can convert the surface of aluminum into a ceramic layer, thus preventing the corrosive medium contacting the substrate; therefore, the degradation rate can be reduced. Furthermore, highly protective coatings can be produced when appropriate electrolytes are used in the PEO process.
    Motivated by the valuable properties of aluminum, corrosion protection and surface hardening provided by the PEO technique, considerable efforts have been devoted towards the development of surface engineering on aluminum based on PEO protection.
    In this study, PEO processes on pure aluminum and the resulting coating characteristics were systematically studied. Through this progressive study, the corrosion performance and the adhesion strength of the pure aluminum were effectively improved.
    In the first study, by using two different alkaline electrolytes with different addition concentrations of Si3N4 nanoparticles (0, 0.5 and 1.5 gL-1) and different duty cycles (25%, 50% and 80%) at a fixed frequency. The corrosion properties of PEO coatings were investigated by the potentiodynamic polarization test in 3.5 wt.% NaCl solutions. It showed that the weight gains, layer thickness and surface roughness of the PEO grown oxide increased with increasing concentrations of Si3N4 nanoparticles and duty cycles. The PEO grown oxide using the Na2B4O7.10H2O contained electrolyte showed an excellent corrosion resistance and low surface roughness than other PEO coatings grown with Si3N4 nanoparticle additives. However, the corrosion performance of PEO coatings was not improved by the addition of Si3N4 nanoparticle in the electrolytic solutions possibly due to its detrimental effect to the formation of dense microstructure.
    In the second study, PEO treatment was conducted on pure Al using a power supply under a bipolar pulsed mode with constant duty cycle, fixed anodic and cathodic currents. The effect of different concentrations of borax (Na₂B₄O₇∙10H₂O), i.e., 0, 1.5, 3, 4.5 and 6 gL-1 in the electrolyte on the corrosion resistance of PEO grown oxide coatings in 3.5 wt.% NaCl solution was comprehensively studied by a potentiodynamic polarization test and electrochemical impedance spectroscopy method. We found that the average pore size and porosity on the PEO grown oxide coating decreased with increasing borax concentration. The dense microstructure of oxide coating can be seen when the borax concentration in the electrolyte was high. The corrosion resistance of PEO coating increased with increasing borax content. The corrosion resistance of pure Al was greatly improved up to 23058 times higher by the formation of a PEO layer treated in the electrolyte containing 6 gL-1 borax due to its ability to grow a dense -Al2O3 phase with less defects.
    In the third study, by using a sodium silicate-based electrolyte with different concentrations of Si3N4 (0 - 2.5gL-1) additives at different duty cycles (25%, 50% and 80%) and a fixed frequency. It showed that the breakdown voltage decreased with increasing concentration of Si3N4 nanoparticles and it also decreased with increasing duty cycles from 25% to 80%. The coating thickness, surface roughness and adhesion strength of PEO grown oxide layer increased with increasing Si3N4 nanoparticle concentration. For the PEO grown oxide with the same amount of Si3N4 concentration (2.5 gL-1) additive, the surface roughness, thickness and COF decreased with decreasing duty cycle. . On the other hand, an increasing tendency of adhesion strength and the best wear resistance was observed when the duty cycle decreased from 80 to 25%. The best adhesion strength of 14.85 N and lower coefficient of friction was found for the PEO grown coating fabricated with 2.5 gL-1 Si3N4 nanoparticle additive at a duty cycle of 25%. We can conclude that the corrosion resistance and the adhesion strength of pure aluminum were influenced by the added borax and Si3N4 nanoparticle additive in the PEO electrolyte.

    Table of Contents 摘要 i Abstract ii Acknowledgment iv List of Figures viii List of Tables xii List of Abbreviations xiii Chapter 1 1 1. Introduction 1 1.1. Background of study 1 1.2. Objective of the study 2 Chapter 2 3 2. Literature Review 3 2.1. Plasma electrolytic oxidation 3 2.1.1. Corrosion resistance 5 2.1.1.1. Potentiodynamic polarization 5 2.1.1.2. Electrochemical impedance spectroscopy (EIS) 7 2.1.1.3. Factors affecting the corrosion resistance 10 2.1.1.3.1. Effect of electrolyte on corrosion resistance 10 2.1.1.3.2. Effect of electrical variables on corrosion resistance 11 2.1.1.3.3. Effect of treatment time on corrosion resistance 12 2.1.1.3.4. Effects of substrate on corrosion resistance 12 2.1.2. Adhesion strength 12 2.1.2.1. Factors affecting the adhesion strength 13 2.1.2.1.1. Effects of substrate on adhesion strength 13 2.1.2.1.2. Effects of duration of coating time on adhesion strength 13 2.1.2.1.3. Effects of electrolyte on adhesion strength 14 2.1.2.1.4. Effect of electrical variables on adhesion strength 15 Chapter 3 16 3. Experimental Methods 16 3.1. The Scanning Electron Microscope (SEM) 16 3.2. X-ray diffraction (XRD) 17 3.3. Field emission electron probe micro analyzer (FE-EPMA) 19 3.4. Potentiostat 22 3.5. Scratch test 24 3.6. Surface profilometer 26 Chapter 4 28 4. Effects of processing parameters on the corrosion performance of plasma electrolytic oxidation grown oxide on commercially pure aluminum 28 4.1. Introduction 28 4.2. Experimental procedures 30 4.2.1. Preparation of the samples 30 4.2.2. Sample characterization 31 4.3. Results and discussion 31 4.3.1. Voltage –time response of PEO coatings 31 4.3.2. Phase and composition analysis 34 4.3.3. Microstructure analysis of PEO coatings 36 4.3.4. PEO Layer thickness and weight gain 40 4.3.5. Surface roughness 42 4.3.6. The anti-corrosion performance evaluation of PEO coatings 42 4.3.6.1. Potentiodynamic polarization tests 42 4.3.6.2. Electrochemical Impedance Spectroscopy (EIS) test 45 4.4. Conclusions 49 Chapter 5 50 5. Corrosion performance of plasma electrolytic oxidation grown oxide coating on pure aluminum: Effect of borax concentration 50 5.1. Introduction 50 5.2. Materials and Methods of PEO coatings 52 5.2.1. Preparation of the PEO coatings 52 5.2.2. Characterization of PEO coatings 52 5.3. Results and discussion 54 5.3.1. Voltage –time curve characteristics of coatings 54 5.3.2. Phase and chemical composition analysis 56 5.3.3 Surface morphology analysis of PEO coatings 57 5.3.4. Corrosion resistance evaluation 61 5.4. Conclusions 68 Chapter 6 69 6. Adhesion property evaluation of plasma electrolytic oxidation treatment on aluminum: effect of Si3N4 69 6.1. Introduction 69 6.2. Experimental details 70 6.2.1. Sample Preparation 70 6.2.2. Characterization of PEO coatings 71 6.3. Results and discussion 72 6.3.1. Voltage-time responses 72 6.3.2. Structural and composition analysis 74 6.3.3. PEO coatings microstructure analysis 75 6.3.4. Analysis of adhesion properties and wear resistance 82 6.4. Conclusions 86 Chapter 7 87 7. Conclusions and future work 87 7.1. Conclusions 87 7.2. Future work 89 References 90

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