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完整後設資料紀錄
DC 欄位 | 值 | 語言 |
---|---|---|
dc.contributor.advisor | 林招松(Chao-Sung Lin) | |
dc.contributor.author | Daniel Mao-Teh Chen | en |
dc.contributor.author | 陳懋德 | zh_TW |
dc.date.accessioned | 2021-06-13T01:12:08Z | - |
dc.date.available | 2007-07-26 | |
dc.date.copyright | 2007-07-26 | |
dc.date.issued | 2007 | |
dc.date.submitted | 2007-07-18 | |
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Johansson, Y. Jeong and T. Albrektsson. The electrochemical oxide growth behavior on titanium in acid and alkaline electrolytes. Medical Engineering & Physics, 23, 329, 2001. 74. M. Pourbaix. Atlas of Electrochemical Equilibria in Aquaeous Solutions, 2nd ed., NACE, Houston, Texas, 1974. 75. J. H. Liu. The hydroxylapatite layer on titanium plate via micro-oxidation and hydrothermal treatment. Master thesis, National Taiwan University, 2005. | |
dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/29610 | - |
dc.description.abstract | 以微弧氧化法於鈦上所生成之具有多孔性,且富含鈣、磷的氧化鈦陽極膜,具備了可轉變成氫氧基磷酸鈣的成份,且可提昇其在植入生物體內的表現。然而此氧化鈦層具有部份內部缺陷,易導致陽極膜與基材的附著性大幅降低。本研究以定電流的方式,在適當的電解液中對於商用純鈦板進行陽極處理,並進行陽極膜的分析。當陽極電壓較高時,陽極膜將具有較高的鈣、磷含量,但較差的附著性。人工體液的浸泡可以於陽極膜上仿生地生成一主要由磷酸鈣鹽類所組成的沉積層。既有的存在於陽極膜中之鈣、磷成份提供了人工體液內沉積反應的成核位置。因此,搭配人工體液的浸泡,可提高從較低電壓所生成的陽極膜之鈣、磷含量。同時,本研究發現於人工體液浸泡之前,先針對陽極膜進行熱鹼處理,可降低於浸泡人工體液時的反應時間。此結果推論為因熱鹼處理所導致的陽極膜表面改質,在浸泡於人工體液的情況下,會在試片與溶液表面生成一酸鹼值較高,且富含磷酸根離子的區域。在此厚度極低的區域中,人工體液的析出反應可因此被加速。本研究所指出的最佳化製程為對於鈦板進行較低電壓的陽極微弧氧化後,依序進行熱鹼處理及人工體液的浸泡。 | zh_TW |
dc.description.abstract | Anodic oxidation of titanium in the solution containing calcium and phosphorus compounds can prepare a calcium- and phosphorus- containing oxide film. However, during the galvanostatic anodizing process, a porous inner layer formed prior to sparks and a crater-containing overlay formed with sparks resulted in decrease the adhesion of the anodic film. Calcium and phosphorus were predominantly incorporated in the porous overlay, in which the amorphous region contained more calcium and phosphorus than the crystalline region regardless of the anodizing voltages. Moreover, the ratio of amorphous to crystalline regions in the porous overlay changed insignificantly with anodizing voltage. Therefore, higher anodizing voltage can enhance the calcium and phosphorus contents in the anodic film, yet leads to the adhesion decrease problem. Simulated body fluid (SBF) is an unstable solution with some supersaturated calcium phosphate salts. Pure titanium plates and anodized titanium plates were immersed in SBF, and a layer mainly containing calcium and phosphorus was precipitated on them. The chemical properties of both pure titanium and the anodic film were herein enhanced. The time-consuming SBF precipitation process can be adjusted by alkali- and heat-treatment (AHT) before SBF immersion. Both the AHTed titanium and the anodic film resulted in forming a high-pH zone in the SBF medium, and further accelerated the precipitation process in SBF. Properties of the multi-layer structure on titanium were determined by SEM, cross-sectional TEM, EDS, XRD and the adhesion test in this study. | en |
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dc.description.tableofcontents | Abstract I
Figure Caption VII Table Caption X Chapter 1 Introduction 1 1.1 About Titanium 1 1.2 Need of Research Theme 3 Chapter 2 Literature Review 4 2.1 Properties of Human Bones 4 2.2 Properties of Titanium 5 2.3 Properties of Calcium Phosphate 7 2.4 Popular Applications of Calcium Phosphate 8 2.5 Properties and Effects of Simulated Body Fluid 10 2.6 Technologies of Calcium Phosphate Coating 13 2.6.1 Plasma Spraying 13 2.6.2 Alkali- and Heat-treatment 14 2.6.3 Electrochemical Deposition 15 2.6.4 Electrophoretic Deposition 16 2.6.5 Micro-arc Discharging Oxidation 17 2.6.6 Simulated Body Fluid Immersion 20 Chapter 3 Materials and Methods 24 3.1 Designs for Experiments 24 3.2 Experimental Processes 25 3.2.1 Specimen Cleaning 25 3.2.2 Electrolyte for Anodic Oxidation 25 3.2.3 Anodic Oxidation 26 3.2.4 Alkali- and Heat-treatment 26 3.2.5 Simulated Body Fluid Immersion 27 3.2.6 Adhesion Test Specimen Preparation 27 3.3 Specimen Analysis 28 3.3.1 Transmission Electron Microscopy Characterization 28 3.3.2 Scanning Electron Microscope Characterization 28 3.3.3 X-ray Diffraction Analysis 29 3.3.4 Anodic Film Adhesion Test 29 3.3.5 Surface Roughness Measurement 30 Chapter 4 Results 33 4.1 Anodic Oxidation 33 4.1.1 Anodizing Voltage Response 33 4.1.2 Surface Morphology Evolution and Composition of Anodic Oxidation 34 4.1.3 Crystallinity Analysis of Anodic Films 36 4.1.4 Cross-sectional Observation of Anodic Films 36 4.1.5 Adhesion Test and Fracture Surface Morphology 36 4.2 Treatments of the Anodic Film 38 4.2.1 SBF Immersion of Titanium 38 4.2.2 Alkali- and Heat-Treatment for Titanium 39 4.2.3 Alkali- and Heat-Treatment of Anodic Film 40 4.2.4 SBF Immersion of Anodic Film 40 4.2.5 SBF Immersion of AHTed Titanium and Anodic Film 41 4.2.6 Crystallinity Analysis of SBF Immersed Anodic Film 42 4.2.7 Adhesion Test and Fracture Surface Morphology 42 Chapter 5 Discussion 55 5.1 Anodic Oxidation 55 5.1.1 Properties of Anodic Films 55 5.1.2 Crystallinity of Anodic Film 57 5.1.3 Cross-sectional Observation of Anodic Film 57 5.1.4 Decrease of Adhesion with Anodizing Voltage 59 5.2 Treatments of the Anodic Film 61 5.2.1 SBF Immersion of Titanium 61 5.2.2 Alkali- and Heat-Treatment 62 5.2.3 SBF Immersion of Anodic Film 64 5.2.4 SBF Immersion of AHTed Titanium and Anodic Film 66 5.2.5 Enhanced Adhesion Properties 67 5.3 The Multi-Layer Structure 68 Chapter 6 Conclusion 72 Reference 73 Appendix – Pourbaix Diagram of Titanium, Calcium and Phosphorus 81 Figure Caption FIGURE 2.1. THE INTERFACE BETWEEN BONE TISSUES AND DIFFERENT IMPLANTED MATERIALS. 20 FIGURE 2.2. PHOSPHATE IONS IN DIFFERENT PH ENVIRONMENT. 21 FIGURE 2.3. SCHEMATIC REPRESENTATION OF A CHARGED PARTICLE IN THE SOLUTION. 21 FIGURE 2.4. CROSS-SECTIONAL TEM MICROGRAPH OF A PLATE ANODIZED TO 100V. 22 FIGURE 2.5. CROSS-SECTIONAL TEM MICROGRAPH OF A PLATE ANODIZED TO 150V. 22 FIGURE 2.6. CROSS-SECTIONAL TEM MICROGRAPH OF A PLATE ANODIZED TO 300V. 23 FIGURE 2.7. (A) A HIGHER MAGNIFICATION VIEW NEAR THE SURFACE OF ANODIC FILM SHOWN IN FIGURE 4.11, AND (B) AND (C) ARE THE SAD PATTERNS ASSOCIATED WITH THE AREAS MARKED BY THE ARROW AND DOUBLE ARROWS IN (A), RESPECTIVELY. 23 FIGURE 3.1. THE FLOW CHART OF THIS STUDY 31 FIGURE 3.2. A SCHEMATIC REPRESENTATION OF THE ANODIC OXIDATION DEVICES. 32 FIGURE 3.3. A SCHEMATIC REPRESENTATION OF THE ADHESION TEST SPECIMEN. 32 FIGURE 4.1. ANODIZING VOLTAGE AS A FUNCTION OF ANODIZING TIME DURING GALVANOSTATIC ANODIZING. 44 FIGURE 4.2. ANODIZING VOLTAGE AS A FUNCTION OF ANODIZING TIME DURING GALVANOSTATIC ANODIZING IN THE ELECTROLYTE ADDED ADDITIONAL HYDROXYLAPATITE POWDER. 44 FIGURE 4.3. SURFACE MORPHOLOGY OF (A) TITANIUM PLATE ANODIZED TO (B) 50V, (C) 100V AND (D) 150V, RESPECTIVELY. 45 FIGURE 4.4. SURFACE MORPHOLOGY OF TITANIUM PLATE ANODIZED TO (A) 200V, (B) 250V, (C) 300V AND (D) 350V, RESPECTIVELY. 45 FIGURE 4.5. CA AND P CONTENTS OF THE ANODIC FILM AROUND THE EDGE OF A CRATER AS A FUNCTION OF ANODIZING VOLTAGE. 46 FIGURE 4.6. CA AND P CONTENTS OF THE ANODIC FILM AROUND THE EDGE OF A CRATER AS A FUNCTION OF ANODIZING VOLTAGE IN THE ELECTROLYTE ADD ADDITIONAL HYDROXYLAPATITE POWDER. 46 FIGURE 4.7. SURFACE ROUGHNESS OF THE ANODIC FILM AS A FUNCTION OF THE ANODIZING VOLTAGE. 47 FIGURE 4.8. XRD PATTERNS OF A PLATE ANODIZED TO (A) 50, (B) 100, (C) 150, (D) 200, (E) 250, (F) 300, AND (G) 350V. 47 FIGURE 4.9. THICKNESS OF THE INNER PORE-CONTAINING LAYER AND THE ENTIRE ANODIC FILM AS A FUNCTION OF THE ANODIZING VOLTAGE. 48 FIGURE 4.10. THE ADHESIVE STRENGTH OF THE ANODIC FILM AS A FUNCTION OF THE ANODIZING VOLTAGE. 48 FIGURE 4.11. SURFACE MORPHOLOGY OF (A) SUBSTRATE SIDE AND (B) EPOXY SIDE OF THE SPECIMEN ANODIZED TO 200 V AFTER ADHESION TEST, AND (C) AND (D) ARE THEIR CORRESPONDING EDS SPECTRUMS. 49 FIGURE 4.12. SURFACE MORPHOLOGY OF (A) SUBSTRATE SIDE AND (B) EPOXY SIDE OF THE SPECIMEN ANODIZED TO 250 V AFTER ADHESION TEST. 49 FIGURE 4.13. SURFACE MORPHOLOGY OF THE TITANIUM SPECIMEN IMMERSED IN SBF FOR (A) 1 DAY, (B) 7 DAYS AND (C) 14 DAYS. 50 FIGURE 4.14. SURFACE MORPHOLOGY OF THE TITANIUM PLATE PERFORMED WITH AHT FOR (A) 1 H, (B) 24 HRS AND (C) A POROUS STRUCTURE ON THE 24-HRS-AHT SPECIMEN. 50 FIGURE 4.15. SURFACE MORPHOLOGY OF TITANIUM PLATE (A) ANODIZED TO 250V THEN (B) TREATED WITH AHT FOR 1 H. 51 FIGURE 4.16. SURFACE MORPHOLOGY OF THE 250V-ANODIZED SPECIMEN IMMERSED IN SBF FOR (A) 1 DAY, (B) 7 DAYS AND (C) 14 DAYS. 51 FIGURE 4.17. SURFACE MORPHOLOGY OF AS-POLISHED TITANIUM PLATE TREATED WITH AHT FOR 1 H THEN IMMERSED IN SBF FOR 1 DAY. 52 FIGURE 4.18. SURFACE MORPHOLOGY OF TITANIUM PLATE ANODIZED TO 250V, TREATED WITH AHT FOR 1 H THEN IMMERSED IN SBF FOR 1 DAY. 52 FIGURE 4.19. XRD PATTERNS OF (A) AS-RECEIVED TITANIUM PLATE, (B) SPECIMEN A5, (C) B2, (D) C1, (E) E1 AND (F) F2. 53 FIGURE 4.20. ADHESIVE STRENGTH OF THE SPECIMEN A5, D1, E1 AND F2. 53 FIGURE 4.21. SURFACE MORPHOLOGY OF (A) SUBSTRATE SIDE AND (B) EPOXY SIDE OF THE SPECIMEN F2 AFTER ADHESION TEST. 54 FIGURE 5.1. A SCHEMATIC REPRESENTATION OF THE ANODIC FILM FORMED AFTER SPARING. 55 FIGURE 5.2. THE XRD PATTERNS OF (A) AS-RECEIVED TRICALCIUM POWDER AND IT (B) AFTER IN AHT FOR 1 H. 55 FIGURE 5.3. SCHEMATIC DIAGRAM OF THE MECHANISM OF TITANIUM WITH AHT AND SBF. 55 FIGURE 5.4. SCHEMATIC DIAGRAM OF THE MECHANISM OF THE ANODIC FILM WITH AHT AND SBF. 55 Table Caption TABLE 2.1. MECHANICAL PROPERTIES OF COMMERCIAL PURE TITANIUM. 5 TABLE 2.2. DIFFERENT TYPES OF CALCIUM PHOSPHATE SALTS 7 TABLE 2.3. CHEMICAL COMPONENT OF HUMAN BONE, ENAMEL AND DENTINE 8 TABLE 2.4. NOMINAL CONCENTRATIONS OF BLOOD PLASMA AND SBF 10 TABLE 2.5. REACTIONS IN SBF 12 TABLE 2.6. CHEMICAL PROPERTIES OF HEPES 13 TABLE 2.7. COMPARISON OF ELECTROPLATING AND ELECTROPHORETIC DEPOSITION 16 TABLE 3.1. SPECIMENS IN THIS STUDY 24 TABLE 3.2. CHEMICALS FOR SBF PREPARATION 27 TABLE 4.1. ELEMENTAL COMPONENT OF THE LAYER ON EVERY SPECIMEN. 43 | |
dc.language.iso | en | |
dc.title | 含鈣磷之氧化鈦陽極膜於人工體液浸泡行為 | zh_TW |
dc.title | Simulated Body Fluid Immersion of Calcium- and Phosphorus-containing Anodic Titanium Oxide Film | en |
dc.type | Thesis | |
dc.date.schoolyear | 95-2 | |
dc.description.degree | 碩士 | |
dc.contributor.oralexamcommittee | 林峰輝,潘永寧,楊聰仁,楊哲人 | |
dc.subject.keyword | 陽極氧化法,微弧氧化法,鈦,鈣,磷,氫氧基磷酸鈣,人工體液,熱鹼處理, | zh_TW |
dc.subject.keyword | anodic oxidation,micro-arc oxidation,titanium,calcium,phosphorus,hydroxylapatite,simulated body fluid,alkali-and heat-treatment, | en |
dc.relation.page | 80 | |
dc.rights.note | 有償授權 | |
dc.date.accepted | 2007-07-20 | |
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 |
顯示於系所單位: | 材料科學與工程學系 |
文件中的檔案:
檔案 | 大小 | 格式 | |
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ntu-96-1.pdf 目前未授權公開取用 | 2.78 MB | Adobe PDF |
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