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研究生:向西蘭
研究生(外文):S.L.HSIAN
論文名稱:電解沉積HA/ZrO2生醫陶瓷鍍層於純鈦上之研究
論文名稱(外文):Electrolytic HA/ZrO2 Bioceramic Coatings on pure Ti
指導教授:顏秀崗顏秀崗引用關係
指導教授(外文):S.K.Yen
學位類別:碩士
校院名稱:國立中興大學
系所名稱:材料工程學研究所
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2003
畢業學年度:91
語文別:中文
論文頁數:151
中文關鍵詞:電解沉積氫氧基磷灰石ZrO2純鈦導骨作用
外文關鍵詞:electrolytic depositionhydroxyapatiteZrO2Tiosteoconduction
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為了要改進氫氧基磷灰石(HA)在植入合金上之附著力,本研究使用純Ti(ASTM F67 Grade 1)當基材在硝酸氧化鋯水溶液(ZrO(NO3)2)中先電解沉積氫氧化鋯(Zr(OH)4)膠體,然後再於磷酸鈣混合水溶液(Ca(NO3)2.4H2O+NH4H2PO4 )中沉積氫氧基磷灰石(HA)陶瓷鍍層,藉由控制不同的電化學參數濃度和溫度,獲得在純鈦基材上沉積HA/ZrO2複合鍍層的最佳條件,將HA/ZrO2複合鍍層試片經燒結後藉由XRD、SEM/EDS、循環極化試驗、刮痕試驗、浸泡試驗及細胞培養等分析方法,針對表面型態、抗蝕性、導骨作用(Osteoconduction)等作有系統的分析與探討。由人工模擬體液之循環極化測試結果顯示,HA/ZrO2複合鍍層較單層HA具有較佳的抗蝕效果;由超音波震盪與刮痕試驗測試結果得知,HA/ZrO2複合鍍層其附著力較單層HA為佳,有效提高鍍層之附著力;從浸泡試驗的結果得知,浸泡於模擬體液中之單層HA及HA/ZrO2複合鍍層結構均很穩定。從細胞培養之SEM觀察顯示,HA鍍層及HA/ZrO2複合鍍層之細胞貼附生長攤平的能力較基材及ZrO2鍍層良好且快速,得以證明氫氧基磷灰石(HA)具有骨引導的能力。
In order to improve the adhesion of HA on implant alloy, electrolytic hydroxyapatite HA/ZrO2 double layer coatings on pure Ti were conducted in ZrO(NO3)3 aqueous solution and subsequently mixing Ca(NO3)2.4H2O and NH4H2PO4 aqueous solution. By controlling the electrochemical parameters, concentration and temperature, the optimum conditions of HA/ZrO2 coated specimens were obtained. After annealing, the HA/ZrO2 coated specimens were characterized by XRD, SEM/EDS and cyclic polarization tests, scratch tests, immersion tests and cell culture. The HA/ZrO2 coated specimens showed the better corrosion resistance than the HA coated or uncoated. The adhesion strength of HA coatings on Ti were dramatically improved by the intermediate ZrO2 coating. Also, SEM observations of cell culture revealed the better extension of osteosacoma on HA/ZrO2 or HA coated specimens than on ZrO2 coated or uncoated. This indicates that HA coatings exhibited the better osteocondution.
第一章 緒論
1- 1前言…………………………………………………………………1
1-2研究動機與目的 …………………………………………‥………2
第二章 文獻回顧………………………………………………7
2-1生醫材料之簡介 ……………………………………………………7
2-1-1 生醫材料之基本要求……………………………….………7
2-1-2 生醫材料之分類及應用……………………………….……9
2-2 鈦及鈦合金 …………………………………….…………………14
2-3氧化鋯陶瓷…………………………………………………………16
2-4氫氧基磷灰石………………………………………………………17
2-5極化…………………………………………………………………19
2-5-1活性極化………………………………………………………19
2-5-2濃度極化……………………………………………………20
2-5-3電阻極化……………………………………………………23
2-6生醫陶瓷的披覆法 ………………………………………….……23
2-6-1熱均壓………………………………………………………23
2-6-2電漿噴塗……………………………………………………23
2-6-3離子束濺射沉積……………………………………………24
2-6-4溶膠-凝膠沉積 ……………………………………….……24
2-6-5射頻磁控濺射………………………………………………24
2-6-6電化學沉積…………………………………………………24
2-7電解沉積氧化鋯之反應機構 ……………………………………25
2-8電解沉積氫氧基磷灰石(HA)之反應機構 ………………………26
2-9電化學交流阻抗實驗 ……………………………………………27
2-9-1 交流阻抗之原理 …………………………………………27
2-9-2交流阻抗之應用……………………………………………33
第三章 實驗步驟與方法 ……………………………………35
3-1 試片準備與前處理 ………………………………………………37
3-2 電解液之調配 ……………………………………………………39
3-2-1 硝酸氧鋯電解液之調配……………………………………39
3-2-2 氫氧基磷灰石電解液之調配………………………………39
3-3陰極極………………………………………………………………39
3-4電解沉積……………………………………………………………40
3-4-1 最佳沉積電位………………………………………………40
3-4-2 最佳沉積時間………………………………………..….…41
3-5 陰乾與燒結 …………………………………………………….…41
3-6 X光繞射(XRD)分析…………………………………………….…41
3-7 SEM/EDS表面型態分析 …………………………………………42
3-8 電化學動態極化測試 ……………………………………………42
3-9 電化學交流阻抗測試 ……………………………………………44
3-10 浸泡試驗…………………………………………………………44
3-11 橫切面(Cross-Section)成份分佈分析……………………………45
3-12 刮痕試驗…………………………………………………….…....45
3-13 超音波震盪測試………………………………………………….46
3-14生物評估(in vitro)………………………………………….……46
3-14-1細胞培養 ………………………………….………………46
3-14-2老鼠頭蓋骨器官培養 ……………….……………………49
第四章 結果與討論 …………………………………………50
4-1 陰極極化 …………………………………………………………51
4-1-1 硝酸氧化鋯水溶液之陰極極化實驗………………………51
4-1-2 磷酸鈣電解液之陰極極化實驗……………………………53
4-2 電解沉積製程之參數探討 ………………………………………55
4-2-1 單層ZrO2 …………………………………………………55
4-2-2 單層HA ……………………………………………………57
4-2-3 HA/ZrO2複合鍍層 …………………………………………58
4-3陰乾與燒結…………………………………………………………60
4-4 X光繞射分析………………………………………………………61
4-4-1 ZrO2鍍層之SEM表面微結構觀察 ………………………61
4-4-2 HA鍍層之SEM表面微結構觀察…………………………62
4-5動態極化測試………………………………………………………64
4-6電化學交流阻抗測試………………………………………………67
4-7橫切面(Cross-Section)成份分佈分析 …………………………69
4-8附著力測試…………………………………………………………71
4-8-1 刮痕測試……………………………………………………71
4-8-2 超音波震盪測試……………………………………………72
4-9浸泡試驗……………………………………………………………73
4-9-1 HA鍍層於模擬體液中之浸泡試驗 ………………………74
4-9-2 ZrO2/HA複合鍍層於模擬體液中之浸泡試驗……………75
4-10細胞附著型態之觀察 ……………………………………………76
4-10-1 細胞專用培養皿上細胞附著型態之SEM觀察 …….….76
4-10-2 Ti基材上細胞附著型態之SEM觀察 ……………………76
4-10-3 ZrO2鍍層上細胞附著型態之SEM觀察…………………77
4-10-4 HA鍍層上細胞附著型態之SEM觀察 …………………77
4-10-5 HA/ZrO2複合鍍層上細胞附著型態之SEM觀察………78
4-10-6 HA/ZrO2複合鍍層器官培養之相位差顯微鏡觀察………79
第五章 結論 …………………………………………………80
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