臺灣博碩士論文加值系統

本研究的主要目的分為二部分。第一部分是利用微波電漿氣相化學沉積法之技術製作摻硼鑽石薄膜電極，探討製程參數對電化學行為的影響；第二部分是將摻硼鑽石電極結合微差脈衝剝除法偵測環境毒物-鉈(I)。
摻硼鑽石薄膜電極製備在微波功率1500W、氣體總壓55torr、氫氣流速300sccm、甲烷流速12sccm、B(OCH3)3流速0.8sccm下，並施加-135V直流偏壓成核15分鐘、成長300分鐘即完成電極製備，此摻硼鑽石薄膜電極對1mM K3Fe(CN)6在循環伏安法的可逆性標準偏差值為4.73% (n=10)，鑽石純度平均為94% (n=10)。
第二部分將自製的摻硼鑽石電極作為工作電極，並使用微差脈衝剝除伏安法(Differential Pulse Stripping Voltammetry)進行偵測環境毒物-鉈(I)，在沉積電位-1200mV下，沉積時間150秒，緩衝溶液條件為0.05M、pH4磷酸緩衝溶液，脈衝振幅50mV，脈衝時間25ms，取樣時間17ms，其線性範圍為50nM-10μΜ (R=0.998)，靈敏度4.65μA/μM，偵測極限(S/N=3)為6.72nM，在連續偵測1μM鉈(I)20次的相對標準偏差為3.95%，而利用此系統量測池塘水
及淡水河水的回收率(1μΜ Tl+)分別為97.3%及99.7%。

The boron-doped diamond (BDD) electrode has attractive intensive attention recently. There are two parts in this study. The first one, we used the microwave plasma enhanced chemical vapor deposition (MPECVD) prepared the boron-doped diamond electrode, and study the various factors influence of the diamond quality and electrochemical behavior, including C/H ratio、B/C ratio and growth time.
Subsequently the boron-doped electrode was used to measure thallium. Thallium was measure by difference pulse stripping voltammetry(DPSV) at the optimum condition of buffer solution：0.05、pH4 phosphate buffer.
The measure peak current at 810mV (vs. /AgCl) for deposition potential at -1200mV、deposition time 150 sec. The differential pulse optimal condition, including the pulse amplitude 50mV、pulse width 25ms、sampling time 17ms.According the optimum conditions, the linear range of thallium is between 0.05μM to 10μM(R=0.998), and sensitivity is 4.65μA/μM. The estimated detection limit(S/N=3) is 6.72nM.The relative standard deviation of twenty repetitive detection is 3.95%.Typical recovery rates are 97.3 and 99.7 from the spikes of 1μM Thallium samples from pond water and Tamsui River,respectively.

第一章 緒論
1-1鑽石簡介………………………………………………………….1
1-1-1鑽石和碳之結構………………………………………..…….1
1-2鑽石合成方式及理論……………………………………….……2
1-2-1鑽石合成方式………………………………………………2
1-2-2鑽石薄膜之合成理論……………………………………...3
1-2-3影響鑽石薄膜純度之因素………………………………...6
1-3鑽石薄膜的應用……………………………………………….....8
1-3-1鑽石在光化學的應用………………………………………8
1-3-2鑽石電極在電化學上之應用……………………………..10
1-4鉈………………………………………………………………..17
1-4-1鉈的分佈與應用………………………………………….17
1-4-2鉈的毒理效應及治療…………………………………….18
1-4-3偵測鉈(I)的方法………………………………………….21
1-4-3-1電化學方法…………………………………………21
1-4-3-2光譜法………………………………………………26
1-4-3-3質譜法……………………………………………….27
1-4-3-4中子活化法………………………………………….28
1-5剝除伏安法……………………………………………………...28
1-6研究目的………………………………………………………...30
第二章 實驗部分
2-1實驗儀器………………………………………………………...31
2-1-1摻硼鑽石薄膜之鍍膜設備…………………………………31
2-1-2量測鉈(I)之電化學儀器…………………………………...31
2-2.藥品...……………………………………………………………33
2-3 鍍膜系統……………………………………………………….32
2-3-1鍍膜系統……………………………………………………32
2-3-2鍍膜步驟…………………………………………………...33
2-3-3拉曼光譜儀………………………………………………...34
2-4摻硼鑽石薄膜電極組成之探討………………………………..38
2-4-1碳氫比(C/H ratio)之探討………………………………….38
2-4-2硼碳比(B/C ratio)之探討………………………………….38
2-4-3成長時間之探討…………………………………………...38
2-5利用鑽石電極偵測鉈(I)………………………………………...39
2-5-1鑽石電極之製備……………………………………………..39
2-5-2實驗條件設計……………………………………………….39
2-5-2-1沉積電位之探討………………………………………..39
2-5-2-2溶液酸鹼值之探討……………………………………..39
2-5-2-3沉積時間之探討………………………………………...39
2-5-2-4緩衝溶液種類之探討…………………………………..39
2-5-2-5緩衝溶液濃度之探討…………………………………...40
2-5-2-6脈衝振幅大小之探討…………………………………..40
2-5-2-7脈衝時間之探討………………………………………..40
2-5-2-8取樣時間之探討……………………………………….40
2-5-2-9分析特性之探討……………………………………….40
第三章 結果與討論
3-1鑽石薄膜組成探討……………………………………………...41
3-1-1碳氫比(C/H ratio)之探討…………………………………41
3-1-2硼碳比(B/C ratio)之探討…………………………………43
3-1-3成長時間之探討………………………………………….46
3-1-4製程穏定性之探討………………………………………46
3-2偵測鉈(I)最佳化探討………………………………………….49
3-2-1偵測機制及CV之探討………………………………….49
3-2-2沉積電位之探討………………………………………….52
3-2-3沉積時間之探討………………………………………….53
3-2-4溶液酸鹼值之探討……………………………………….54
3-2-5緩衝溶液種類之探討…………………………………….55
3-2-6緩衝溶液濃度之探討…………………………………….56
3-2-7脈衝振幅大小之探討…………………………………….58
3-2-8脈衝時間之探討………………………………………….59
3-2-9取樣時間之探討………………………………………….60
3-3分析特性之探討………………………………………………..62
3-4結論……………………………………………………………..62
參考資料………………………………………………………………67

圖表目錄

圖(一)碳氫比之探討，探討碳氫比對1mM K3Fe(CN)6在pH3、0.1M
KCl之循環伏安圖………………………………………..........42
圖(二)碳氫比對電化學可逆性及鑽石薄膜純度之影響……………...43
圖(三)硼碳比之探討，探討不同的硼碳比對於鑽石顆粒、厚度及電
阻值的影響……………………………………………………..45
圖(四)硼碳比之探討，探討不同的硼碳比對於鑽石純度之影響……45
圖(五)成長時間探討，探討不同成長時間的鑽石薄膜在電子顯微鏡下放大10萬倍的形態圖(morphology)………………………………….47
圖(六)製程穏定性之探討……………………………………………..48
圖(七)循環伏安圖……………………………………………..49
圖(八)連續添加循環伏安圖………………………….50
圖(九)掃描速率的探討………………..51
圖(十)微差脈衝伏安圖…………………………………..……52
圖(十一)電位沉積之探討………………..…………..……..53
圖(十二)沉積時間之探討……………………………..……..54
圖(十三) pH值探討………….…………………..……………55
圖(十四)緩衝溶液種類探討……..……………………………………56
圖(十五)緩衝溶液濃度探討…………………………………………..57
圖(十六)微差脈衝伏安法電位變化圖………………………………..58
圖(十七)脈衝振幅大小之探討………………………………………..59
圖(十八)脈衝時間之探討……………………………………………..60
圖(十九)取樣時間探討………………………………………………..62
圖(二十)不同沉積時間的校正曲線……………………….....…...65
圖(二十一)摻硼鑽石電極對於偵測鉈(I)的校正曲線圖…....…….66
圖(二十二)操作系統穏定性之探討…………………………….…...66

表(一)摻硼鑽石電極偵測鉈(I)的操作化最佳條件………………...67
表(二)分析特性表……………………………….…………………...67
表(三)干擾物探討…………………………………………………....68
表(四)鉈(I)偵測方法比較…………………………………………….69

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