臺灣博碩士論文加值系統

　　鈦及鈦合金具有優秀的機械性能，常用於航太材料及生醫植入物。而鈦金屬容易在表面自然形成氧化鈦薄膜，鈦的氧化膜具良好的化學穩定性，可保護底層合金不被外在環境因素腐蝕。為了得到更好的表面性質，本研究在生醫級純鈦上鍍製了TiV薄膜，再進行氧化後處理，以獲得富鈦及富釩氧化物的氧化層，藉由釩氧化物獨特且多樣的結構性質改善薄膜的磨潤性，本研藉由將鈦釩合金薄膜進行高溫退火氧化及雷射紋理氧化，以獲得不同表面形貌之鈦釩氧化層，進而分析其機械性質、抗腐蝕性能、生物抗菌性及相容性。
　　在本研究中，利用陰極電弧系統沉積搭配鈦釩合金靶材鍍製在生醫級純鈦試片鍍製出均勻且附著良好之TiV薄膜，TiV薄膜再進行高溫退火氧化，分別以500℃、600℃、700℃進行高溫退火氧化，以及由脈衝雷射在TiV掃描進行雷射紋理氧化，分別以100kHz、300kHz、500kHz等不同頻率的脈衝雷射，藉由雷射的高能量及特性，在TiV薄膜表面上形成規律的表面微結構。再分析藉由兩種不同的氧化方式所獲得的氧化層的機械性質、抗腐蝕性、生物相容性及抗菌性。
薄膜的表面微結構及成份分析採用場發射掃描式電子顯微鏡（Field-Emission Scanning Electron Microscope, FE-SEM）和能量分散式光譜分析儀（Energy Dispersive Spectrometer, EDS）對鍍層的微觀結構以及成份分佈進行了分析，以X光繞射儀（X-Ray Diffraction, XRD）觀察氧化物結晶像。薄膜的機械性質以維氏硬度測量經不同方式氧化後的薄膜硬度變化，而磨耗試驗則以球對盤式的磨耗形式搭配鉻鋼球進行測試，以測得試片的磨潤性變化。以恆電位儀進行電化學腐蝕試驗，以5%重量濃度百分比的氯化鈉(NaCl)溶液做為腐蝕液，分析TiV薄膜氧化後的抗腐蝕性。抗菌試驗則以Syto9熒光染料進行抗菌性分析，測定金黃色葡萄球菌在試片上的細菌存活率。
　　本研究是以物理氣相沉積沉積TiV薄膜，再進行高溫退火氧化與雷射紋理氧化來形成不同表面微結構的含氧化鈦及氧化釩之表面，藉由氧化鈦及氧化釩的特性，以及經不同氧化方式所得的表面形貌。其中以在100kHz的雷射紋理氧化後的TiV薄膜，其經雷射處理後獲的超疏水性薄膜提升抗沾黏的效果，以及其表層所含的氧化釩提升了磨潤性，而藉由雷射熱影響大幅提升薄膜的微小硬度。而經由表層氧化物的生成及氧化後的表面形貌，更進一步提升抗菌性及生物相容性。

　　Thanks to its excellent corrosion resistance, good mechanical properties and biocompatibility, itanium has been widely used as aerospace materials and biomaterials.
A passive oxide film formed on titanium surface is responsible for its high corrosion resistance
　　TiO2, a wide band-gap semiconductor, is known as a photocatalyst which has various remarkable features including self-cleaning, anti-bacteria, and anti-corrosion. The bactericidal activity of TiO2 thin films is very important in regards to its practical applications, Besides TiO2, vanadium oxides have been investigated extensively due to their distinctive structure versatility, especially with respect to potential applications in tribological, biomedical and electrochemical devices.
　　In this study, a cathodic-arc deposition method was successfully developed to produce a crack-free, spatially homogeneous Ti-V coating on pure titanium. After deposition, the Ti-V alloy coatings were annealed to form a composite structure of titanium oxides and vanadium oxides by thermal oxidation at high temperature up to 500 oC~700 oC And laser texturing oxidation at high frequency pulse laser up to 100kHz~500kHz.
　　The surface morphologies, crystal structures and bonding states of the deposited coatings were identified by field emission scanning electron microscope (FE-SEM), Glancing Incidence X-ray diffraction (GAXRD),To evaluate the antibacterial ability, Staphylococcus aureus (S. A., Gram-positive bacteria) were tested. Bacteria were tested by a fluorescence staining method (Syto9) and bacterial viability agar tests. The in vitro cytotoxicity was tested followed by the standard of ISO 10995-5:2009. Cell viability and proliferation of human skin fibroblast cells cultured on these films were also determined by using the MTT assay.
　　Ball-on-disc wear tests were conducted to evaluate the tribological properties of the coatings. The result showed that an appropriate thermal oxidation and laser texturing oxidation of Ti-V coatings improved both the antibacterial ability and biocompatibility with good tribological performance.

中文摘要…………………………………………………………………i
英文摘要………………………………………………………………...ii
誌謝……………………………………………………………………. iii
目錄……………………………………………………………………..iv
表目錄…………………………………………………………………..vi
圖目錄………………………………………………………………….vii
第一章　緒論……………………………………………………………1
1.1 前言…………………….……………………………………….1
1.2 研究動機………………………………….…………………….2
1.3 研究目的…………………………………………………….….2
第二章 倫理背景與文獻回顧…………………………………………..3
2.1 鈦及鈦合金之特性……………………………………………..3
2.2 鈦及鈦合金在工業之應用………………………………….….5
2.2.1在航太材料上之應用…………………………………...5
2.3 鈦合金在生醫材料之應用.………………………………….…7
2.3.1 生醫材料的分類.……………………………..………...8
2.3.2 鈦及其氧化物在抗菌性上之應用…………………....10
2.3.3 鈦及其合金在生醫植入物上之應用……………….....13
2.4 薄膜沉積技術……………………………………….………...14
2.4.1 陰極電弧沉積（Cathodic Arc Evaporation, CAE）....15
2.5 薄膜成長機制………………………….……………………...17
2.6 鈦及鈦合金之長件表面處理回顧…………………………....21
2.6.1 鈦之陽極氧化處理………………………………........21
2.6.2 鈦之微弧氧化處理…………………………………....23
2.6.3 鈦之高溫退火氧化處理…………..………..................26
2.6.4 雷射紋理氧化處理………………………………........28
2.6.5 雷射紋理氧化對機械性質之影響……..……………..31
2.6.6 雷射紋理氧化對抗腐蝕性能的影響..………………..33
2.6.7 雷射紋理氧化對表面水接觸角之影響……………....35
第三章 研究方法………………………………………………………38
3.1 實驗流程…………………………………….………………...38
3.2 薄膜設計與製程…………………………………………........39
3.2.1 前處理與鍍膜步驟……………………………………39
3.2.2 TiV薄膜參數…………………………………………..41
3.3 TIV薄膜之氧化處理……………………….…………………42
3.3.1 高溫退火氧化………………………………………....42
3.3.2 雷射紋理氧化…………………………………………43
3.4 薄膜微結構分析………………………………………….…...44
3.4.1場發射掃描式電子顯微鏡分析(FE-SEM)…………….44
3.4.2 X光繞射分析儀(X-Ray Diffractometer, XRD)…….....45
3.5 薄膜機械性質分析…………………………………….……...47
3.5.1 微小維克氏硬度試驗機................................................47
3.5.2 磨耗試驗機……………..……………………………..48
3.6 水接觸角量測儀………………………………...…………….51
3.7 恆電位電流儀…….…………………………………………...50
3.7.1 塔佛極化曲線……………………………..…………..53
3.7.2 電化學阻抗頻譜法………………………..…………..55
3.8 生物實驗分析…………………………………………….…...57
3.8.1 Syto9 螢光抗菌性分析……………………………......57
3.8.2 ISO 10993-5 細胞毒性分析…………………………...58
第四章 結果與討論………………………………………………........59
4.1 試片表面結構與成份分析……………………………….…...59
4.1.1 試片表面形貌分析………………..…………………...59
4.1.2 試片表面微結構與成份分析………………………….62
4.1.3 試片斷面結構與成份分析…………………………….69
4.1.4 X光繞射儀分析……………………………...………73
4.2 機械性質分析………………………………………………...77
4.2.1 微小維克氏硬度分析………………………………….77
4.2.2 表面粗糙度分析……………………………...………..79
4.2.3 常溫磨耗試驗測試……………………………...……..80
4.3 表面水接觸角分析…………………….……………………...83
4.4 恆電位儀分析………………………………………………....85
4.4.1 塔佛極化曲線………………………………...………..85
4.4.2 電化學阻抗頻譜…………………………………….....87
4.5 生物實驗分析………………………………………….……...90
4.5.1 Styo9 螢光抗菌性分析……………………..…………90
4.5.2 ISO 10993-5 細胞毒性分析………………………...…92
第五章 結論……………………………………..…..…………………95
參考文獻………………………………………………………………..97
Extended Abstract……………………………………………………...107

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