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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 林新智(Hsin-Chih Lin) | |
| dc.contributor.author | Ying-Chu Chen | en |
| dc.contributor.author | 陳映竹 | zh_TW |
| dc.date.accessioned | 2023-03-19T22:26:24Z | - |
| dc.date.copyright | 2022-09-02 | |
| dc.date.issued | 2022 | |
| dc.date.submitted | 2022-08-31 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/84802 | - |
| dc.description.abstract | 鋁基複合材料(AMC)泛指以鋁合金作為基底而製成的複合材料。其中，陶瓷材料如碳化矽顆粒常被作為AMC的添加相，以製備出具有可調節(tailorable)性能的材料。近十年，關於AMC的文獻數量逐年攀升，AMC也被應用在許多場合當中。有文獻指出，AMC的腐蝕速率比鋁合金高，且孔蝕也是一大隱憂。然而，目前關於AMC腐蝕保護的文獻並不多，也尚未找到適合且有效的腐蝕保護方法。本研究利用原子層沉積(ALD)技術，沉積氧化鉿(HfO2)、氧化鋯(ZrO2)、氧化鈦(TiO2)以及氧化鋁(Al2O3)薄膜於鋁基碳化矽顆粒複合材料上。利用穿透式電子顯微鏡觀察薄膜在AMC上的形貌及均勻性，再以動電位極化法及交流阻抗譜，分析四種薄膜對於AMC在1.5%氯化鈉水溶液中的腐蝕保護性。結果顯示四種薄膜皆有效使得腐蝕電流密度下降，其中以氧化鉿的效果最為顯著。本研究也利用ALD技術沉積了50、100、150及200個循環的氧化鉿薄膜，以探討薄膜的厚度效應。腐蝕電流及阻抗頻譜的結果顯示，氧化鉿薄膜的腐蝕保護性大致上隨著厚度上升而提高，但是呈現趨近飽和的趨勢。這暗示不需要再將厚度提升就能達到十分優異的腐蝕保護性，以減少金錢及時間成本的耗費。 為了探究腐蝕形貌的變化，我們將AMC裸材以及有氧化鉿薄膜保護的AMC (HfO2/AMC) 放入1.5%氯化鈉水溶液中浸泡4小時及8小時後取出，觀察二次電子影像以及元素分布圖。結果顯示浸泡8小時的AMC裸材上出現蝕孔，而HfO2/AMC上產生裂紋。AMC裸材上的蝕孔分布範圍小且深，HfO2/AMC的裂紋則是廣而淺，顯示HfO2薄膜有效降低孔蝕的嚴重程度或延後孔蝕的發生。 本研究是第一個將ALD技術應用於AMC腐蝕保護上的研究。研究成果顯示ALD薄膜能均勻地沉積在AMC上，並且對AMC的抗腐蝕性有非常顯著的提升，以及減緩孔蝕的發生。 | zh_TW |
| dc.description.abstract | Aluminum matrix composites (AMCs) have been used in various applications and the number of journal articles regarding AMCs has been rising yearly. It has been reported that AMCs reinforced with silicon carbide (SiC) particles have a higher corrosion rate than aluminum alloys and are prone to pitting corrosion. However, there has been little study on the corrosion protection of AMCs, and no effective method has been proposed yet. In this work, we revealed that atomic layer deposition (ALD) is a feasible method to provide corrosion protection to AMCs reinforced with SiC particles. Thin films of HfO2, ZrO2, TiO2, and Al2O3 were deposited using ALD on AMC reinforced with 20 vol.% SiC particles. Observation of transmission electron microscope (TEM) images showed that these thin films were grown on AMC well and uniformly. Their corrosion protection properties were measured using potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS). Analysis showed that HfO2, ZrO2, TiO2, and Al2O3 thin films of 200 cycles provided enhanced corrosion protection to AMC from 1.5% NaCl (aq) solution, with HfO2 providing the highest level of protection. The effect of film thickness on corrosion protection properties was also investigated using AMC covered with HfO2 films of 50, 100, 150, and 200 cycles. Analysis of current density and impedance revealed that corrosion resistance generally increased with increasing film thickness but showed a sign of saturation, indicating that a further increase in film thickness will be unnecessary. To investigate the differences between the corrosion behavior of bare AMC and thin film-protected AMC, bare AMC and AMC covered with HfO2 films of 200 cycles (HfO2/AMC) were immersed in 1.5% NaCl (aq) solution for 4 and 8 hours. After immersion, their corrosion morphologies and corrosion products were compared and contrasted. Scanning electron microscope (SEM) images and elemental mappings from electron probe microanalyzer (EPMA) showed that corrosion pits were found on bare AMC after 8 hours of immersion but only cracks were observed on HfO2/AMC. The corrosion pits on bare AMC were local and deep, while the corrosion cracks on HfO2/AMC propagated outwardly and appeared in a much larger region. This indicates that HfO2 films can lessen the severity or delay the occurrence of pitting corrosion. This is the first reported instance of using oxide thin films fabricated by ALD for the corrosion protection of aluminum matrix composites. We reported improved corrosion resistance and showed the differences in corrosion morphologies between bare AMC and AMC covered with HfO2 thin films. | en |
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| dc.description.tableofcontents | CONTENTS 誌謝 i 中文摘要 ii ABSTRACT iii CONTENTS v LIST OF FIGURES viii LIST OF TABLES xv Chapter 1 Introduction 1 Chapter 2 Literature Review 4 2.1 Properties of Aluminum Matrix Composites (AMCs) 4 2.1.1 Mechanical and Physical Properties 4 2.1.2 Corrosion Behavior and Properties 6 2.1.3 Corrosion Protection of AMCs 10 2.2 Atomic Layer Deposition (ALD) 11 2.2.1 Process and Mechanism 11 2.2.2 Conformality of ALD 13 2.2.3 Growth Rate 15 2.2.4 Plasma-Enhanced ALD 17 2.2.5 Corrosion Protection of Metal Materials by ALD Thin Films 20 Chapter 3 Experimental Methods 24 3.1 AMC Sample Preparation 24 3.2 ALD Thin Film Deposition 25 3.3 Microstructure Observation and Composition Analysis 30 3.3.1 Scanning Electron Microscope (SEM) 30 3.3.2 X-Ray Diffractometer (XRD) 30 3.3.3 Electron Probe Microanalyzer (EPMA) 31 3.3.4 X-Ray Photoelectron Spectroscopy (XPS) 32 3.3.5 Transmission Electron Microscope (TEM) 32 3.4 Corrosion Property Measurement 33 3.4.1 Open Circuit Potential (OCP) 35 3.4.2 Electrochemical Impedance Spectroscopy (EIS) 35 3.4.3 Potentiodynamic Polarization (PDP) 36 3.4.4 Immersion Test 37 3.4.5 Salt Spray Test 38 3.5 Surface Property 38 3.5.1 Contact Angle System 38 Chapter 4 Results and Discussion 40 4.1. Characterization of AMC 40 4.1.1 Microstructure 40 4.1.2 Crystal Structure 41 4.2 Characterization of ALD Thin Films 43 4.2.1 Microstructure 43 4.2.2 Crystal Structure 51 4.2.3 Valence State and Composition 54 4.2.4 Hydrophilicity 58 4.3 Corrosion Behavior and Properties 63 4.3.1 Corrosion Rate 63 4.3.2 Electrochemical Impedance 68 4.3.3 Corrosion Morphology 74 4.3.4 Corrosion Behavior and Products 76 4.3.5 Salt Spray Test 84 Chapter 5 Conclusions 86 Reference 88 LIST OF FIGURES Fig. 1-1. Number of articles regarding AMCs published in academic journals between 1980 and 2020 according to Web of Science. 2 Fig. 2-1. The electrochemical series and standard reduction potentials [42]. 7 Fig. 2-2. Pourbaix diagram for aluminum at 25℃ [9]. 8 Fig. 2-3. Schematic diagram of one cycle of an ALD process for Al2O3 deposition [16]. 13 Fig. 2-4. Schematic diagrams of a 3D structure with (a) non-conformal coating and (b) conformal coating [17]. 14 Fig. 2-5. SEM image of a DRAM trench with an aspect ratio of 1:60. The trench was covered with Al2O3 film deposited by ALD and showed close to 100% conformality [18]. 15 Fig. 2-6. Growth rates of ALD thin film as a function of growth temperature [19]. 16 Fig. 2-7. Growth rates of HfO2 films deposited by thermal ALD and PE-ALD as a function of growth temperature [19]. 19 Fig. 2-8. The (a) capacitance and (b) leakage current density of MOS capacitors with HfO2 films deposited by thermal ALD and PE-ALD [19]. 20 Fig. 2-9. (a) Polarization curves and (b) Bode plot of HfO2, ZrO2, TiO2, ZnO, and Al2O3 films deposited by ALD on copper [25]. 22 Fig. 2-10. (a) Polarization curves and (b) Bode plot of Al2O3 films of varying thickness on copper with impedance shown as closed squares and phase angle shown as open circles [25]. 22 Fig. 2-11. (a) Impedance spectrum and (b) phase angle spectrum of HZO films of varying thickness on Mg-Ca alloy [15]. 23 Fig. 3-1. The as-received AMC sample, which was reinforced by SiC particles. 25 Fig. 3-2. The ALD system used in this study (Fiji, Cambridge Nanotech). 26 Fig. 3-3. Schematic diagram showing the process of growing HfO2, ZrO2, and TiO2 films by PE-ALD. 26 Fig. 3-4. Schematic diagram showing the process of growing Al2O3 films by PE-ALD. 27 Fig. 3-5. Schematic representation of (a) typical XRD and (b) GIXRD [26]. 31 Fig. 3-6. Schematic diagram showing the operating principle of WDS [43]. 32 Fig. 3-7. The three-electrode electrochemical cell used in this study. 34 Fig. 3-8. A typical cyclic PDP curve. Tafel extrapolation is done as shown with dotted lines for icorr [27]. 37 Fig. 3-9. Schematic diagram showing the relations between contact angle and surface hydrophobicity [28]. 39 Fig. 4-1. Secondary electron image of AMC showing its surface morphology. 41 Fig. 4-2. (a) Secondary electron image of AMC and its corresponding elemental mappings showing the distribution of (b) Al, (c) Si, (d) O, (e) Mg, and (f) C. 41 Fig. 4-3 XRD pattern of AMC. 42 Fig. 4-4. (a) TEM bright field image, (b) HRTEM image, (c) and (d) FFT patterns of HfO2/AMC. (c) and (d) correspond to region I and II in (b) respectively. 44 Fig. 4-5. TEM elemental mappings of HfO2/AMC showing the distribution of (a) Hf, (b) O, (c) Pt, (d) Al, (e) Si, and (f) C. 45 Fig. 4-6. (a) TEM bright field image, (b) HRTEM image, (c) and (d) FFT patterns of ZrO2/AMC. (c) and (d) correspond to region I and II in (b) respectively. 46 Fig. 4-7. TEM elemental mappings of ZrO2/AMC showing the distribution of (a) Zr, (b) O, (c) Pt, (d) Al, (e) Si, and (f) C. 47 Fig. 4-8. (a) TEM bright field image, (b) HRTEM image, (c) and (d) FFT patterns of TiO2/AMC. (c) and (d) correspond to region I and II in (b) respectively. 48 Fig. 4-9. TEM elemental mappings of TiO2/AMC showing the distribution of (a) Ti, (b) O, (c) Pt, (d) Al, (e) Si, and (f) C. 49 Fig. 4-10. (a) TEM bright field image, (b) HRTEM image, (c) and (d) FFT patterns of Al2O3/AMC, corresponding to region I and II in (b) respectively. 27.73 nm might include the thickness of the oxide films naturally formed on aluminum alloys. 50 Fig. 4-11. TEM elemental mappings of Al2O3/AMC showing the distribution of (a) Al, (b) O, (c) Pt, (d) Si, and (e) C. 51 Fig. 4-12. GIXRD pattern of HfO2/AMC. XRD pattern of bare AMC is also shown. 53 Fig. 4-13. GIXRD pattern of ZrO2/AMC. XRD pattern of bare AMC is also shown. 53 Fig. 4-14. GIXRD pattern of TiO2/AMC. XRD pattern of bare AMC is also shown. 54 Fig. 4-15. GIXRD pattern of Al2O3/AMC. XRD pattern of bare AMC is also shown. 54 Fig. 4-16. High-resolution XPS scans of (a) HfO2, (b) ZrO2, (c) TiO2, and (d) Al2O3. 56 Fig. 4-17. Depth profiles of (a) HfO2, (b) ZrO2, (c) TiO2, and (d) Al2O3 from XPS. 58 Fig. 4-18. Images of water drop on the surface of (a) HfO2/AMC (b) ZrO2/AMC (c) TiO2/AMC (d) Al2O3/AMC, and (e) bare AMC. 60 Fig. 4-19. Contact angles on varying types of surface. 60 Fig. 4-20. Images of water drop on HfO2 films of (a) 50 nm (b) 100 nm (c) 150 nm, and (d) 200 nm on AMC. 62 Fig. 4-21. Contact angles on HfO2 of varying thickness on AMC. 62 Fig. 4-22. PDP curve of bare AMC. 65 Fig. 4-23. PDP curves of AMC covered with varying types of thin films and bare AMC. 65 Fig. 4-24. PDP curves of AMC covered with HfO2 films of varying thickness and bare AMC. 67 Fig. 4-25. Corrosion current density as a function of HfO2 thickness (characterized by number of cycles). 68 Fig. 4-26. (a) Nyquist plot of AMC covered with HfO2, ZrO2, TiO2, and Al2O3 thin films and (b) enlargement of the part marked with a blue rectangle in (a). 70 Fig. 4-27. Equivalent circuit used to model the results in Fig. 4-26. 70 Fig. 4-28. Bode plots showing the (a) impedance and (b) phase angle of AMC covered with HfO2, ZrO2, TiO2, and Al2O3 thin films. 71 Fig. 4-29. (a) Nyquist plot of AMC covered with HfO2 films of varying thickness and (b) enlargement of the part marked with a gray rectangle in (a). 73 Fig. 4-30. Bode plots showing the (a) impedance and (b) phase angle of AMC covered with HfO2 films of varying thickness. 73 Fig. 4-31. (a) Impedance and (b) phase angle at 0.01 Hz as a function of HfO2 film thickness. 74 Fig. 4-32. SEM images showing corrosion pits on different sites of AMC after 8 hours of immersion in 1.5% NaCl (aq) solution. 75 Fig. 4-33. SEM images showing the corrosion morphology of HfO2/AMC after 8 hours of immersion in 1.5% NaCl (aq) solution. (b) was taken from the region marked with a pink square in (a). (c) and (d) were taken from the region marked with a green and a blue rectangle in (b), respectively. 76 Fig. 4-34. (a) secondary electron image and (b)-(f) elemental mappings of bare AMC after 8 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) O, (c) Cl, (d) Al, (e) Si, and (f) Mg. 77 Fig. 4-35. (a) secondary electron image and (b)-(f) elemental mappings of bare AMC after 4 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) O, (c) Cl, (d) Al, (e) Si, and (f) C. 79 Fig. 4-36. (a) secondary electron image and (b)-(f) elemental mappings of a corrosion pit on bare AMC after 8 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) O, (c) Cl, (d) Al, (e) Si, and (f) C. 79 Fig. 4-37. (a) secondary electron image and (b)-(g) elemental mappings of HfO2/AMC after 4 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) Hf, (c) O, (d) Cl, (e) Al, (f) Si, and (g) C. 81 Fig. 4-38. (a) Secondary electron image and (b)-(g) elemental mappings of HfO2/AMC after 8 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) Hf, (c) O, (d) Cl, (e) Al, (f) Si, and (g) C. 82 Fig. 4-39. (a) Secondary electron image and (b)-(g) elemental mappings of HfO2/AMC after 8 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) Hf, (c) O, (d) Cl, (e) Al, (f) Si, and (g) C under a higher magnification. 83 Fig. 4-40. (a) Secondary electron image and (b)-(g) elemental mappings of another site on HfO2/AMC after 8 hours of immersion in 1.5% NaCl (aq) solution, showing the distribution of (b) Hf, (c) O, (d) Cl, (e) Al, (f) Si, and (g) C. 84 LIST OF TABLES Table 2-1. Properties of conventional packing materials and AMCs [5]. 5 Table 3-1. Deposition parameters of Al2O3 thin films. 28 Table 3-2. Deposition parameters of ZrO2 thin films. 28 Table 3-3. Deposition parameters of TiO2 thin films. 29 Table 3-4. Deposition parameters of HfO2 thin films. 29 Table 3-5. Gradings for salt spray tests. 38 Table 4-1. Corrosion potential and corrosion current density of AMC covered with varying types of thin films. 66 Table 4-2. Corrosion potential and corrosion current density of AMC covered with HfO2 films with varying thickness. ‘0 cycles’ represents bare AMC. 67 Table 4-3. Fitted equivalent circuit model parameters of AMC covered with varying types of thin films. 71 Table 4-4. Results from salt spray tests. 85 | |
| dc.language.iso | en | |
| dc.title | 以原子層沉積技術提升鋁基碳化矽複合材料之抗腐蝕性 | zh_TW |
| dc.title | Improvement of Corrosion Resistance of Aluminum Matrix Composites by Atomic Layer Deposition | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 110-2 | |
| dc.description.degree | 碩士 | |
| dc.contributor.oralexamcommittee | 林昆明(Kun-Ming Lin),楊木榮(Mu-Rong Yang),洪衛朋(Wei-Peng Hong) | |
| dc.subject.keyword | 原子層沉積,腐蝕保護,鋁基複合材料,極化曲線,交流阻抗譜, | zh_TW |
| dc.subject.keyword | atomic layer deposition,corrosion protection,aluminum matrix composites,potentiodynamic polarization,electrochemical impedance spectroscopy, | en |
| dc.relation.page | 94 | |
| dc.identifier.doi | 10.6342/NTU202202973 | |
| dc.rights.note | 同意授權(限校園內公開) | |
| dc.date.accepted | 2022-08-31 | |
| dc.contributor.author-college | 工學院 | zh_TW |
| dc.contributor.author-dept | 材料科學與工程學研究所 | zh_TW |
| dc.date.embargo-lift | 2022-09-02 | - |
| 顯示於系所單位： | 材料科學與工程學系 | |
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