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系統識別號 U0002-0301200708535000
中文論文名稱 銦錫氧化物微電極電化學行為研究以及對阿黴素之偵測
英文論文名稱 The electrochemical behavior of indium tin oxide microelectrode and it’s application for doxorubicin detection.
校院名稱 淡江大學
系所名稱(中) 化學學系碩士班
系所名稱(英) Department of Chemistry
學年度 95
學期 1
出版年 96
研究生中文姓名 葉秀炫
研究生英文姓名 Hsiu-Hsuan Yeh
學號 693170051
學位類別 碩士
語文別 中文
口試日期 2006-12-13
論文頁數 85頁
口試委員 指導教授-林孟山
委員-陳壽椿
委員-傅明仁
委員-蔡東湖
中文關鍵字 銦錫氧化物  微電極  阿黴素 
英文關鍵字 Indium Tin Oxide  Microelectrode  Doxorubicin 
學科別分類 學科別自然科學化學
中文摘要 本研究的主要目的是利用黃光微影之大量製程技術將銦錫氧化物(indium tin oxide, ITO)導電玻璃製成微電極,並探討ITO微電極的電化學行為,並且用來偵測抗癌藥物-阿黴素。在過去並未有人利用黃光微影技術將ITO電極製成各式電極,尤其是微電極並且以此探討微電極對於阿黴素的分析研究,所以實驗中開發微機電系統技術,將ITO電極蝕刻成直徑50 的微電極,研究ITO微電極電化學行為,並且探討ITO微電極對於阿黴素的電化學行為。
ITO微電極製造方式是以轉速2000 rpm將正光阻劑AZ P4620均勻塗佈在ITO玻璃表面,用光源波長365 nm曝光機將微電極圖案曝光至正型光阻劑上,以35 %鹽酸蝕刻三分鐘即可在ITO電極表面蝕刻出微電極,再以負型光阻劑SU-8 2025封裝電極,即完成電極製備,取10支ITO微電極重複量測1 mM K3Fe(CN)6,相對標準偏差值為4.12 %。電化學實驗選擇以微差脈衝伏安法 (Differential Pulse Voltammetry)進行抗癌藥物阿黴素的偵測,阿黴素還原電位為-530 mV (vs. Ag/AgCl),在溶液環境為0.1 M、pH8磷酸緩衝溶液,內含0.01 M的氯化鉀條件下,脈衝振幅大小25 mV、脈衝時間25 msec、脈衝周期為200 msec、取樣時間17 msec,線性範圍可達25 μM (R=0.998),靈敏度為1.899×10-4 A/M,本系統的偵測極限 (S/N=3)為15.5 nM,重複操作的相對標準偏差為2.987 % (n=15)。
目前一片七公分見方的ITO玻璃可以製造出16支ITO微電,相對於傳統製造微電極技術,電極面積大小更為精準,製作效率更高,期望在未來增加電極面積使用率,降低成本,未來可將此微型ITO微電極用於小樣品分析技術上的研究。
英文摘要 In history, many kinds of microelectrode were produced and discussed. In this study, we used the photolithographic technique to develop a new type of indium tin oxide (ITO) microelectrode with 50 μm diameter, and the electrochemical behavior of ITO microelectrode was investigated. Finally, this ITO microelectrode was used to detect the anticancer drug- Doxorubicin.
In the photolithographic process, positive photo resist AZ P4620 was spin coated on ITO electrode at 2000 rpm. The patterns of microelectrode were exposed to positive photo resist. Then the ITO electrode was immersed into a 35 % HCl solution for 180 seconds, the unmasked ITO can be etched away and ITO microelectrode patterns were accomplished. Subsequently, the ITO microelectrodes were insulated and packaged by negative photo resist SU-8 to maintain and restrict at a constant area of working electrode the conducting wire, which affect the working electrode.
Doxorubicin was measured by Differential Pulse Voltammetry at the optimum condition at buffer solution: 0.1 M, pH8 phosphate buffer containing 0.01 M potassium chloride. The response peak potential is at -530 mV (vs. Ag/AgCl). In differential pulse Voltammetry optimal study, pulse amplitude is 25 mV; pulse width is 25 msec; pulse period is 200 msec; sample width is 17 msec. According to optimum operation conditions, the analytical performances of the ITO microelectrode are listed in the following contents. The linear range of Doxorubicin is obtained up to 25 μM (R=0.998), and the obtained sensitivity is 1.899×10-4 A/M. The estimated detection limited is 15.5 nM (S/N=3). The relative standard deviation of fifteen repetitive detections is 2.987 %.
論文目次 目錄(Contents)
第一章 緖論……………………………………………………………1
1-1 微電極 (Microelectrode)……………………………………………1
1-1-1 微電極的發展及特性……………………………………………1
1-1-2 微電極幾何形狀及材料…………………………………………4
1-1-3 微電極製作方法…………………………………………………5
1-1-4 微機電系統………………………………………………………9
1-2 銦錫氧化物 (Indium tin oxide)………………………………………11
1-2-1 導電玻璃的製造方法…………………………………………13
1-2-2 導電玻璃蝕刻方法……………………………………………15
1-2-3 導電玻璃的應用………………………………………………17
1-3 抗癌藥物…………………………………………………………18
1-3-1 抗癌藥物的使用與發展………………………………………18
1-3-2 抗癌藥物的分類………………………………………………19
1-3-3 抗癌藥物-阿黴素 (doxorubicin)…………………………………21
1-3-4 阿黴素的毒害機制……………………………………………23
1-3-5 阿黴素的抗癌機制……………………………………………27
1-3-6 阿黴素偵測方法………………………………………………29
1-4 研究目的…………………………………………………………31

第二章 實驗…………………………………………………………32
2-1 儀器與設備………………………………………………………32
2-2 藥品………………………………………………………………33
2-3 ITO微電極蝕刻及封裝製程………………………………………34
2-4 ITO微電極製備最佳條件探討……………………………………34
2-5 阿黴素氧化還原機制……………………………………………35
2-6 ITO微電極偵測阿黴素最佳化條件探討…………………………35
2-7 微差脈衝伏安法最佳條件探討…………………………………36
2-8 分析特性…………………………………………………………37

第三章 結果與討論…………………………………………………38
3-1 ITO微電極蝕刻及封裝製程………………………………………38
3-1-1 ITO電極清潔……………………………………………………38
3-1-2 ITO微電極正光阻劑黃光微影…………………………………39
3-1-3 ITO微電極負光阻劑製程………………………………………40
3-2 ITO微電極製備最佳條件探討……………………………………41
3-2-1 蝕刻液的選擇…………………………………………………41
3-2-2 鹽酸溶液濃度探討……………………………………………42
3-2-3 封裝ITO微電極材料選擇………………………………………42
3-2-4 負型光阻劑曝光時間探討……………………………………43
3-2-5 ITO微電極電化學特性…………………………………………44
3-3 阿黴素氧化還原機制……………………………………………45
3-4 ITO微電極偵測阿黴素最佳化條件探討…………………………45
3-4-1 溶液環境pH值最佳化探討……………………………………46
3-4-2 緩衝溶液種類探討 ……………………………………………46
3-4-3 緩衝溶液濃度探討……………………………………………47
3-4-4 電解質濃度探討………………………………………………47
3-5 微差脈衝伏安法最佳條件探討…………………………………48
3-5-1 脈衝振幅大小的探討…………………………………………48
3-5-2 脈衝時間的探討………………………………………………49
3-5-3 脈衝週期的探討………………………………………………50
3-5-4 取樣時間的探討………………………………………………50
3-6 ITO微電極對於阿黴素的分析特性………………………………51
3-7 結論………………………………………………………………51
參考資料………………………………………………………………79

圖表目錄
圖1:AutoCAD繪圖軟體繪製出ITO微電極光罩的圖形。……………53
圖2:曝光顯影後AZ P4620的微電極顯微鏡照片。…………………53
圖3:蝕刻ITO微電極流程圖。………………………………………54
圖4:AutoCAD繪圖軟體繪製出固定ITO微電極面積圖形。…………55
圖5:以SU-8 2025封裝電極面積後的顯微鏡影像。………………55
圖6:以負光阻劑固定電極面積流程圖。……………………………56
圖7:ITO微電極連接裝置示意圖。…………………………………57
圖8:測試不同酸液對ITO玻璃蝕刻的影響。………………………57
圖9:鹽酸溶液濃度探討。……………………………………………58
圖10:封裝ITO微電極材料選擇。……………………………………59
圖11:負型光阻劑曝光時間探討。…………………………………60
圖12:曝光時間對負型光阻劑交聯程度的探討。…………………61
圖13:ITO微電極電化學特性。………………………………………62
圖14:ITO微電極穩定性探討。………………………………………63
圖15:阿黴素循環伏安圖譜。………………………………………64
圖16:阿黴素循環伏安圖譜(除氧20分鐘)。………………………65
圖17:阿黴素微差脈衝伏安法真實訊號。…………………………66
圖18:溶液環境pH值最佳化。………………………………………67
圖19:緩衝溶液種類探討。…………………………………………68
圖20:緩衝溶液濃度探討。…………………………………………69
圖21:電解質濃度探討。……………………………………………70
圖22:微差脈衝伏安法電位變化圖。………………………………71
圖23:脈衝振幅大小的探討。………………………………………72
圖24:脈衝時間的探討。……………………………………………73
圖25:脈衝週期的探討。……………………………………………74
圖26:取樣時間的探討。……………………………………………75
圖27:阿黴素濃度校正曲線。………………………………………76
圖28:ITO微電極偵測阿黴素穩定性探討。…………………………77
表1:ITO微電極正光阻劑黃光微影參數。…………………………54
表2:SU-8 2025負光阻劑製程參數。………………………………56
表3:ITO微電極對於阿黴素的分析特性。…………………………78

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