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| DC 欄位 | 值 | 語言 |
|---|---|---|
| dc.contributor.advisor | 王玉麟 | |
| dc.contributor.author | Shih-Yung Chen | en |
| dc.contributor.author | 陳師詠 | zh_TW |
| dc.date.accessioned | 2021-06-17T00:55:22Z | - |
| dc.date.available | 2013-10-21 | |
| dc.date.copyright | 2011-10-21 | |
| dc.date.issued | 2011 | |
| dc.date.submitted | 2011-09-26 | |
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| dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/66750 | - |
| dc.description.abstract | 由於陽極氧化鋁薄膜是由排列整齊且高深寬比的氧化鋁奈米管所組成的孔洞狀材料，因此被廣泛的運用於成長奈米材料的底板。然而，對於氧化鋁奈米管的生長行為卻沒有被清楚地研究。在此篇研究中，我們利用微影的技術成功得成長出單根孤立的陽極氧化鋁奈米管，並且我們還發現其不斷地分岔進而形成一個樹枝狀的結構，此樹枝狀結構最後形成一個外觀為半球狀的孔洞結構。若仔細觀察此孔洞結構，其孔洞隨著時間演化成不同的形狀。我們也發現應力會影響孔洞狀氧化鋁的成長速率，並且應力亦會改變孔洞的形狀。此研究可以幫助我們了解陽極氧化鋁奈米管的成長機制，並且提供我們許多創新的想法，藉以改變氧化鋁孔洞的形狀以製作出不同結構的奈米材料。 | zh_TW |
| dc.description.abstract | Porous anodic aluminum oxide (AAO) membranes have been widely used as templates for growing nanomaterials because of their ordered nanochannel arrays with high aspect ratio and uniform pore diameter. However, the intrinsic growth behavior of an individual AAO nanochannel has never been carefully studied for the lack means to fabricate a single isolated anodic alumina nanochannel (SIAAN). In this study, we develop a lithographic method to fabricate a SIAAN, which grows into a porous hemispherical structure with its pores exhibiting fascinating morphological evolution during anodization. We also discover the mechanical stress affects the growth rate and pore morphology of AAO porous structure. This study helps reveal the growth mechanism of arrayed AAO nanochannels grown on a flat aluminum surface and provides insights to help pave the way to alter the geometry of nanochannels on AAO templates for the fabrication of advanced nanocomposite materials. | en |
| dc.description.provenance | Made available in DSpace on 2021-06-17T00:55:22Z (GMT). No. of bitstreams: 1 ntu-100-D95222024-1.pdf: 4089025 bytes, checksum: 66ee003ec022f3970d3e53466ecc18ca (MD5) Previous issue date: 2011 | en |
| dc.description.tableofcontents | Chapter 1 Introduction 1
1.1 Anodic aluminum oxide (AAO)………………………………………….1 1.2 Application of AAO film……………………………………………...…5 1.3 Mechanism of the growth of AAO…………………………………….…8 1.4 Two-step anodization……………………………………………..…….12 1.5 Mechanical stress model for self-organized formation………………....13 1.6 Porosity analysis of AAO………………………………………….……16 1.7 Focused ion beam (FIB) bombardment…………………………………25 1.7.1 Imaging…………………………………………………….26 1.7.2 Milling……………………………………………………..27 1.7.3 Deposition…………………………………………...…….29 Chapter 2 Morphological Evolution of Porous Nanostructures Grown from a Single Isolated Anodic Alumina Nanochannel 34 2.1 Motivation………………………………………………………………34 2.2 Experimental method…………………………………………………...34 2.2.1 Fabrication of polished aluminum substrate………………….34 2.2.2 Porous structure grown from a SIAAN……………………….35 2.3 Results and discussions…………………………………………………37 2.3.1 An array of porous structure evolved from SIAAN……………….37 2.3.2 Morphologies of the porous structure derived from a SIAAN…….40 2.3.3 Effect of spontaneous etching in porous nanostructure…………....44 2.3.4 Clarification of evolution from SIAAN-derived porous structure…47 2.3.5 Details for the fabrication of SIAAN……………………………...49 2.3.6 Stress on the oxide film……………………………………………50 2.3.7 Upward elongation of the hemispherical growth front……………52 2.3.8 Stress induced oxide dissolution model………………..………….53 2.3.9 Similarity in structure evolution between SIAAN-derived structure and honeycomb coral…………………………………………...……...58 Chapter 3 Comparison between SIAAN-derived porous structure and arrayed AAO nanochannels fabricated by one-step anodization 63 3.1 Motivation……………………………………………………………..63 3.2 Experimental process………………………………………………….63 3.2.1 Arrayed AAO nanochannels fabricated by one-step anodization...63 3.2.2 Arrayed AAO nanochannels fabricated by two-step anodization...63 3.3 Results and discussion………………………………………………...64 3.3.1 Comparison between arrayed AAO nanochannels by one-step anodization and SIAAN-derived porous structure……………..64 3.3.2 Comparison between arrayed AAO nanochannels by two-step anodization and SIAAN-derived porous structure……………..66 Chapter 4 Monte Carol model 68 4.1 Motivation……….…………………………………………………….68 4.2 Key assumptions of Monte Carlo model………………………………68 4.3 Results and discussion…………………………………………………69 4.3.1 Morphological transition………………………………………...69 4.3.2 Statistical result of Monte Carol model………………………….71 Chapter 5 Growth of AAO on curved aluminum surfaces 76 5.1 Motivation…………………………………….……………………….76 5.2 Experimental process………………………………………………….76 5.2.1 Growth of AAO on curved aluminum surfaces…………………76 5.2.2 Concaves bombarded by FIB…………………………………....78 5.3 Results and Discussions……………………………………………….79 Chapter 6 Conclusions 82 References 85 Appendix 97 List of publications…………………………………………………………………. 97 List of figures 1.1 Schematic of anodization………………………………………………………….2 1.2 Schematic of porous anodic aluminum oxide nanochannels………………...……2 1.3 SEM micrographs of the bottom view of anodic alumina layers. Anodization was conducted in 0.3 M (1.7 wt %) sulfuric acid at 10 °C at 25 V (a), 0.3 M (2.7 wt %) oxalic acid at 1 °C at 40 V (b), and 10 wt % phosphoric acid at 3 °C at 160 V (c). Pore opening was carried out in 5 wt % phosphoric acid at 30 °C for 30 min (a), 35 °C for 30 min (b), and 45 °C for 30 min (c)……………………………..………3 1.4 Interpore distance d in self-organized porous alumina versus anodic voltage Ua for sulfuric, oxalic, and phosphoric acid solutions. The solid line represents the relation d=-1.7+2.8Ua…………………………………………………………..………..4 1.5 Disordered pore arrangements of anodic alumina layers (bottom view) anodized in 10 wt % phosphoric acid at 120 V. Pores were opened in 5 wt % phosphoric acid at 45 °C for 30 min………………………………………………………….….…..5 1.6 Schematic diagram of the AAO template-assisted fabrication of C-PCBSD Nanorods…………………………………………………………………..…….6 1.7 SEM images of (a) a bare AAO template and C-PCBSD nanorods under (b) low-magnification and (c) high-magnification…………………………………7 1.8 (a) Schematic representation of the nanostructured device architecture used in this study. (b) J-V characteristics of the as-fabricated devices. (c) Degradation profiles of unencapsulated devices stored at either 30 ºC in ambient air……………….……..8 1.9 Four stages of formation of AAO nanochannels…………………………………..9 1.10 Schematic diagrams of voltage versus time and current versus time in galvanostatic and potentiostatic modes………………………………………………..………..10 1.11 The elementary processes involved in porous oxide growth: A, oxide dissolution by the proton-assisted electric field enhanced mechanism: B, movement of oxygen anions and aluminium cations through the barrier oxide by the field-stimulated mechanism; C. oxide growth at both internal and external oxide interfaces as a result of ionic species movement. The vector orientations and coordinates used are also shown…………………………………………………………………..........……11 1.12 Schematic diagram of two-step anodization for the preparation of anodic porous alumina with straight holes………………………………………………..……..12 1.13 Expansion of aluminum during anodic oxidation. On the left the level of the unoxidized metal surface is depicted……………………………………….……14 1.14 Transmission electron micrographs of self-ordered porous alumina fabricated at (a) 25 V in 1.7 wt % H2SO4, (b) 40 V in 2.7 wt % (COOH)2, and (c) 195 V in 1 wt % H3PO4……………………………………………………………………….……18 1.15 The plan and sectional views of a pore and adjacent cell for films formed in each of the major acids: a, sulphuric acid; b, oxalic acid; c, phosphoric acid; d, chromic acid. The cell comprises acid anion-contaminated film material adjacent to the pore and relatively pure alumina remote from it: ( ) acid anion contaimnated film material; ( ), relatively pure alumina……………………………………………….………20 1.16 The dependence of the pore radius on the electrolyte pH value as given by equation (3) compared with the experimental data. ▲, (COOH) 2 triethanolamine: ●, (COOH)2NaOH: ■, (COOH)2………………………………………………..……22 1.17 Scanning electron micrographs from phosphoric acid samples anodized for 24 h (A) and 48 h (B) in 1 wt % H3PO4 at 195 V, resulting in 500 nm interpore distance. C and D: Numerical image treatment of A and B, respectively, showing the domain size in false colors……………………………………………………………..….23 1.18 Average domain size as a function of the anodization time during anodization in 1 wt % H3PO4 at 195V. The domain size is obtained by numerical picture treatment. First the domain size increases due to self-ordering, but after a critical time shown by the dashed line the domain size decreases again. Current transient during of the same sample, showing first a current decrease typical for self-ordering, and then after a critical time the current increases………………………………………....25 1.19 Block diagram and real FIB…………………………………………………….26 1.20 The principle of FIB (a) imaging, (b) milling and (c) deposition………………30 1.21 Schematic diagram of a single cell of the patterning lattice……………………31 1.22 AFM images of the barrier layer, with f = (a) 0, (b) 2%, (c) 6%, (d) 22%, (e) 28%, and (f) a self-organized structure; f is the degree of mismatch. The insets show the 2D power spectra of corresponding areas. Arrows in (b) and (d) indicate the point defects…………………………………………………………………………….32 1.23 (a) Pores of nanochannels are reduced in size under FIB exposure. (b) Pore size distributions of arrays exposed to different FIB doses……………………….…..33 2.1 Schematic diagram illustrating dendritic branching (green area) from single isolated anodic alumina nanochannel (SIAAN)…………………………………...…….36 2.2 Morphological SEM images of (b) array of isolated alumina and (c) individual isolated alumina (1 hour anodization)……………………………………..……37 2.3 Diagram of average radius of porous structure versus anodization time……..….38 2.4 Top-view SEM images of (a) hemispherical porous structure after removal of barrier alumina layer by acid etching for 200 minutes. (b) High-magnification image of (a). (c) Etching time: 130 minutes. Inset shows division of the pore………………………………………………………………………...……39 2.5 Comparison between (a) budding phase of a nanoporous structure evolving from a SIAAN and (b) fully developed hemispherical structure after removal of barrier layer……….…………………………………………………………………….40 2.6 Cross-sectional TEM images showing the growth of dendritic structure grown from a single isolated anodic alumina nanochannel (SIAAN) after (a) 1 hour, (b) 24 hours and (c) 48 hours of anodization (green arrows indicate the protecting layer). The morphological transition of dendritic porous structure is classified into four phases, which are (1) highly ramified twig-like pores, (2) dendritic structure consisted of stem-like pores (analogous to (6)), (3) straight nanochannels decorated by diminishing stem-like pores (analogous to (5)), and (4) straight nanochannels with kinks. The pore morphology near the growth front also changes from (4) straight nanochannels with many kinks to (5) straight nanochannels decorated by some stem-like pores and then to (6) dendritic structure consisted of stem-like pores…………………………………….……………………………………….43 2.7 Cross-sectional TEM images showing the effect of spontaneous etching on the pore morphology of porous structures formed by (a) 24 hours and (b) 48 hours anodization. a(1) shows highly ramified twig-like pores and a(2) shows the stem-like pores. Such pores formed in the similar region have been etched into b(1) bead-like pores and b(2) wider stem-like pores after additional 24 hours of immersion in oxalic acid………………………………………………………..46 2.8 Dendritic structure evolved from three nanochannels, as indicated in the red rectangle…………………………………………………………………….……..50 2.9 (a) SEM image of isolated alumina after clashing to neighboring. (b) Cracks of the protecting layer after clashment of the isoalted alumina………………………….51 2.10 Diagrams of normalized growth front versus polar angle after 24 and 48 hours anodization time……………………………………...……………………...……53 2.11 Comparison between experimental data ( ) obtained by anodization of SIAAN-derived porous structure of 24 hours anodization and fitting curve by equation 2.12 (red line)………………………………….………………….…..57 2.12 Top-view image of a SIAAN-derived porous structure (a) and a honeycomb coral (c) taken by SEM and camera. High-magnification images also shown in (b) and (d). ……..……………………………………………………………………….59 2.13 Anatomy of a coral polyp………………………………………………….……61 2.14 A single polyp (a) dividing into two (b) and then form a colony (c). The growth time are 6 month, one year and two years, respectively…………………….…..61 2.15 Cross-sectional images of a SIAAN-derived porous structure (a) and honeycomb coral (b) taken by TEM and camera, respectively………………………………62 3.1 Cross-sectional TEM images of arrayed AAO nanochannels of (a) one-step anodization and (b) shows nanochannels with segments in the initial phase of the anodization……………………………………………………………………..65 3.2 Cross-sectional TEM images of arrayed AAO nanochannels of two-step anodization. b and c show the initial and final morphologies of nanochannels, respectively…………………………………………………………………….67 4.1 2-dimentional Monte Carlo simulated results with different ratio (σgb) of growth probability to branching probability of line cells. (a) Definitions of growth and branching of line cells. (b) For σgb =3. (c) For σgb =0.01, simulated growth behavior of single isolated anodic alumina nanochannel. (d) For σgb =0.01, occurrence of negative feedback effect to attenuate roughened surface when fast evolving cell branches in large angle α to become slower and slower evolving cell branches in small angle β to become faster………...…………………….....……71 4.2 Diagram of number (N) of nanochannels versus radius (R) of real object. N increases linearly with R…………………………………………………..……..73 4.3 Diagram of number (N) of line cells versus radius (R) of simulated object. N increases linearly with R. The curve is obtained according to average excluded distance of 0.73 cell length………………………………………………..……..74 4.4 Variation of number of channels as a function of (R/d), R: radius of semicircular structure and d: interchannel distance. Experimental curve (square) and simulated curve of σgb=0.01 (triangle) are highly correlated. Simulated results of σgb=1 (circle), σgb=3 (diamond) and σgb=10 (inverted triangle)…………..…….…..…75 5.1 Schematic diagram illustrating the fabrication of AAO film (green area) on curved aluminum surface……………………………………………………..….……..78 5.2 Top view SEM image (a) of an array of concaves bombarded by focused-ion beam. (b) Cross-sectional SEM image of a concave………………………….…….…79 5.3 shows the growth front of AAO film on arrayed (a) and individual (b) curved surfaces………………………………………………………………………….80 5.4 Cross-sectional TEM images of AAO nanostructures on curved aluminum surfaces. (a) Only the curved area allows the growth of AAO nanostructure. (b) AAO nanostructures grown on the curved surface. (b) High-magnification image of the dendritic nanostructure on top of the curved surface……………………...…….81 List of tables 1. Current effficiency for oxide formation in 0.3 M oxalic acid at 1 °C……………15 2. Alumina layer thickness compared to the consumed aluminum layer using 20 wt. % H2SO4 at 1 °C…………………………………………………………………….16 3. Results of structural property of self-organized AAO analyzed from TEM images in Figure 1.14………………………………………………………………….…….16 4. Typical implantation depth and sputtering yield for Ga+ ions in silicon (Si), silicon dioxide (SiO2), aluminium (Al), at normal incidence. The figures in this table were obtained using TRIM Monte Carlo simulations…………………………………..28 5. The relation between FIB beam current and the milling spot size……………...…29 | |
| dc.language.iso | en | |
| dc.subject | 陽極氧化鋁 | zh_TW |
| dc.subject | 孔洞結構 | zh_TW |
| dc.subject | 奈米管 | zh_TW |
| dc.subject | 應力 | zh_TW |
| dc.subject | 樹枝狀結構 | zh_TW |
| dc.subject | Anodic alumina oxide | en |
| dc.subject | porous structure | en |
| dc.subject | nanochannels | en |
| dc.subject | stress | en |
| dc.subject | dendritic structure | en |
| dc.title | 單根陽極氧化鋁奈米管之成長及其孔洞結構之演化 | zh_TW |
| dc.title | Morphological Evolution of Porous Nanostructures
Grown from a Single Isolated Anodic Alumina Nanochannel | en |
| dc.type | Thesis | |
| dc.date.schoolyear | 100-1 | |
| dc.description.degree | 博士 | |
| dc.contributor.oralexamcommittee | 林景泉,宋克嘉,王偉華,劉志毅,劉定宇 | |
| dc.subject.keyword | 陽極氧化鋁,孔洞結構,奈米管,應力,樹枝狀結構, | zh_TW |
| dc.subject.keyword | Anodic alumina oxide,porous structure,nanochannels,stress,dendritic structure, | en |
| dc.relation.page | 97 | |
| dc.rights.note | 有償授權 | |
| dc.date.accepted | 2011-09-28 | |
| dc.contributor.author-college | 理學院 | zh_TW |
| dc.contributor.author-dept | 物理研究所 | zh_TW |
| 顯示於系所單位： | 物理學系 | |
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