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研究生: 翁賜齡
Weng, Si-Ling
論文名稱: 以氧化鋯薄膜增強多孔鈦的機械性質與生物表現性
Development of zirconia film coating on porous-titanium for mechanical properties and biocompatibility enhancement
指導教授: 廖峻德
Liao, Jiunn-Der
共同指導: 劉浩志
Liu, Bernard HaoChih
王士豪
Wang, Shyh-Hau
學位類別: 碩士
Master
系所名稱: 工學院 - 材料科學及工程學系
Department of Materials Science and Engineering
論文出版年: 2017
畢業學年度: 106
語文別: 中文
論文頁數: 60
中文關鍵詞: 多孔氧化鋯薄膜塗層承載力生物材
外文關鍵詞: titanium, porous, zirconia, thin-film coating, load-bearable, biomaterial
相關次數: 點閱:199下載:4
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  • 多孔鈦在生醫材料界已發展多年,相關應用與製程也不可計數,近來植入材發展漸漸走向複合材料,不僅要有一定的機械性質,能誘導骨細胞生長,對生物體也要不具毒性。有鑑於此本實驗應用溶膠凝膠法在多孔鈦上製備氧化鋯薄膜作為研究方向而努力。
    本實驗採用傳統粉末冶金製備多孔鈦,在造孔劑移除方面使用水熱法取代傳統的燒結或超音波震盪移除。利用溶膠凝膠法在試片結構覆蓋具生物惰性的氧化鋯薄膜並進行力學性質和生物測試。於化性方面以XRD與XPS及EDS對試片做成份分析,物性方面以分析表面形貌的SEM與AFM和測量孔隙率之阿基米得原理及壓縮測試來分析試片。力學性質上抗壓強度期望能達到ISO 5833 (Implant for surgery)規範人體植入材最低強度的70 MPa,表面硬度與剛性需與人骨硬度相符合。生物相容性測試方面化依據ISO 10993 (醫療器材生物相容性評估)進行降解產物測試,並且於試片上培養纖維母細胞(L929)並同時進行細胞毒性(LDH)和細胞活性測試(MTS)。
    從XRD分析及晶格常數計算發現多孔鈦最合適燒結溫度是1000℃。孔隙率經由阿基米德法量測實際值與預期值並無太大差異。XPS與SEM的表面元素分析(EDS)中都能偵測到試片中含有鋯的訊號,確認氧化鋯覆蓋於試片表面。多孔試片Z-P-Ti_35~55的抗壓強度符合ISO 5833規範人體植入材最低強度70MPa,另外微觀觀測上有鍍膜的試片比沒有鍍膜的試片無論在剛性、微硬度和表面粗糙度都有顯著提升,顯示氧化鋯著實提升試片的機械性質表現。降解產物測試中不論在極端或生物模擬溶液下鋯離子濃度皆保持一定。經MTS和LDH細胞毒性測試孔隙率越高的試片其細胞生長性與存活率越高,死亡率則沒有變化。
    綜合以上結論,造孔劑添加55%鍍有氧化鋯薄膜的多孔鈦試片因為符合ISO規範強度且有相對高的孔細率與細胞存活率,適合作為未來臨床應用的參數。

    Porous titanium (Ti)-based scaffolds are a promising approach for achieving stiffness reduction. To be used as a biomaterial, porous Ti scaffolds (P-Ti) must have suitable wear and corrosion resistance and the generation of either metallic wear debris or Ti ion release should be insignificant throughout a large timescale. The present study combines a porous structure appropriate for cell ingrowth with a physically and chemically stable thin-film coating to create a load-bearing bio-inspired scaffold. The as-designed zirconia-coated P-Ti (Z-P-Ti) was made via a hydrothermal process, followed by a sol-gel method. Mechanical tests were conducted primarily on P-Ti, and chemical stability tests were conducted on Z-P-Ti. The biocompatibility test results correlated with cell mitigation into Z-P-Ti were compared with those for reference surfaces. The results show that Z-P-Ti is load-bearable with an increased surface hardness and roughness. L929 cell morphology and viability assessed using the live/dead cell staining protocol show a significant enhancement of cell affinity on the surface of Z-P-Ti. The combination of porous Ti, a load-bearable structure, and biocompatible zirconia coating makes the designed biomaterial promising for many applications, such as vertebral discs.

    摘要 I Extended Abstract II 目錄 XI 圖目錄 XIII 表目錄 XV 第一章、緒論 1 1.1簡介 1 研究動機 3 第二章、文獻回顧 4 2.1多孔鈦製程 4 2.2造孔劑選用 4 2.3孔隙率變數 6 2.4表面粗糙度 9 2.5氧化鋯塗層 12 2.6溶膠凝膠法 14 研究目的 16 第三章、理論基礎 17 3.1 粉末冶金(Powder Metallurgy) 17 3.2 真空燒結(Vacuum sintering) 17 3.3水熱法(Hydrothermal method) 18 3.4 MTS量測原理 20 3.5 LDH量測原理 21 第四章、實驗材料與方法 23 4.1實驗藥品 23 4.2多孔鈦製作 23 4.3 孔隙率測定 (Porosity measurement) 25 4.4表面形貌與元素分析 25 4.5試片機械性質 26 4.6生物性測試與法規ISO 10993 27 4.7 MTS與LDH細胞毒性實驗 28 第五章、試片成分分析與機械性質表現 29 5.1 XRD分析 29 5.2孔隙率分析 33 5.3 XPS分析 34 5.4壓應力測試 35 5.5 SEM顯微圖與EDX元素分析 36 5.6微硬度測試及剛性測量 38 5.7表面粗糙度(Ra) 40 第五章總結 42 第六章、模擬溶液降解與體外細胞毒性測試 43 6.1降解實驗 43 6.2細胞培養 44 6.3 MTS測試結果 45 6.4 LDH測試結果 46 第六章總結 48 結論 49 未來展望 51 參考文獻 52

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