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研究生：	陳敏華 Chen, Min-Hua
論文名稱：	研究三氯乙烯電化學行為與其微加工感測器之製備 On the electrochemical behaviors and the microfabricated sensor of trichloroethylene
指導教授：	周澤川 Chou, Tse-Chuan
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2004
畢業學年度：	92
語文別：	中文
論文頁數：	262
中文關鍵詞：	感測器、電化學、三氯乙烯、微加工
外文關鍵詞：	sensor, microfabricated, trichloroethylene, electrochemistry
相關次數：	點閱：47 下載：2
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　　三氯乙烯是工業上一種常用的有機溶劑及去污劑，但是它亦是土壤及地下水中污染的來源。根據醫學的研究指出，三氯乙烯是一種具有致癌性的物質。因此，如何在廢水中監控三氯乙烯濃度是項很重要的指標。本研究中，先探討三氯乙烯在鉛及電鍍鉛電極的電化學還原反應行為，再依據所得之結果設計具有感測性能佳、靈敏度高、應答時間快、重覆使用性次數多及穩定性長的三氯乙烯感測器。
　　在有機電解液系統中，以電聚合的方法可以合成含有共軛性質的聚氯乙炔，並在紫外光-可見光譜有一最大吸收峰在波長315nm，核磁共振光譜及氣相層析圖譜顯示電解後主要產物為氯乙炔，差式掃描熱量分析法得到相變化溫度在325 ˚C。
　　以鉛片為工作電極感測三氯乙烯，工作電極最佳的製備條件為：1.0 M HNO3水溶液前處理30分鐘；三氯乙烯最佳感測條件為：有機電解質濃度0.025 M TBAT，感測電位-2.10 V (vs. Ag/Ag+ with 0.1 M TBAP in AN)，攪拌速率250 rpm。在此條件下，三氯乙烯感測器之靈敏度為7.15 μA/cm2-ppm，應答時間10秒，且電極壽命至少四個月。另外，在此研究偵測範圍內，即三氯乙烯濃度為50至250 ppm間，可以得到三氯乙烯濃度(CL)與其感測應答電流(id)之關係為id=7.15CL，及在質傳控制下的反應速率常數為4.86810-3 (cm-s)-1。
　　以電鍍鉛修飾碳片為工作電極感測三氯乙烯，工作電極最佳的製備條件為：電鍍電流密度10 mA/cm2，電鍍溫度25 ˚C及電鍍時間2小時；三氯乙烯最佳感測條件為：有機電解質濃度0.01 M TBAT，感測電位-2.10 V (vs. Ag/Ag+ with 0.1 M TBAP in AN)，攪拌速率100 rpm。在此條件下，三氯乙烯感測器之靈敏度為7.06 μA/cm2-ppm，應答時間15秒，且電極壽命至少二個月。另外，在此研究偵測範圍內，即三氯乙烯濃度為100至700 ppm間，可以得到三氯乙烯濃度(CL)與其感測應答電流(id)之關係為id=7.06CL，及在質傳控制下的反應速率常數為4.8110-3 (cm-s)-1。
　　以電鍍鉛修飾鉛箔為工作電極感測三氯乙烯，工作電極最佳的製備條件為：0.1 M HNO3水溶液前處理60分鐘，電鍍電流密度20 mA/cm2，電鍍溫度30 ˚C及電鍍時間2小時；三氯乙烯最佳感測條件為：有機電解質濃度0.01 M TBAT，感測電位-2.10 V (vs. Ag/Ag+ with 0.1 M TBAP in AN)，攪拌速率155 rpm。在此條件下，三氯乙烯感測器之靈敏度為1.06 μA/cm2-ppm，應答時間20秒，且電極壽命至少二個月。另外，在此研究偵測範圍內，即三氯乙烯濃度為50至700 ppm間，可以得到三氯乙烯濃度(CL)與其感測應答電流(id)之關係為id=1.06CL，及在質傳控制下的反應速率常數為7.21710-4 (cm-s)-1。
　　以電鍍鉛修飾Pt-Ti薄膜為工作電極感測三氯乙烯，Pt-Ti薄膜基材的濺鍍條件為：310-3 Torr的濺鍍壓力，20分鐘的濺鍍時間及30 Watt的濺鍍功率；工作電極最佳的製備條件為：電鍍電流密度18.75 mA/cm2，電鍍時間2小時在室溫下；三氯乙烯最佳感測條件為：0.1 M TBAT有機電解質溶液，感測電位-2.10 V (vs. Ag/Ag+ with 0.1 M TBAP in AN)，攪拌速率為250 rpm。此條件下，三氯乙烯感測器之靈敏度為2.86 μA/cm2-ppm，應答時間為15秒，重覆使用性至少15次及電極壽命至少六個月。另外，在此研究偵測範圍內，即三氯乙烯濃度為100至700 ppm間，可以得到三氯乙烯濃度(CL)與其感測應答電流(id)之關係為id=2.86CL，及在質傳控制下的反應速率常數為2.43410-3 (cm-s)-1。
　　由以上所有的實驗結果得知，當使用電鍍鉛修飾Pt-Ti薄膜電極於感測三氯乙烯時，皆具有良好的感測性能，不論在靈敏度、應答時間、電極重覆使用性與電極穩定度上均可得到良好的感測結果。除此之外，應用此電極對三氯乙烯感測器的設計是最具實用性的，因為它可以配合微加工的技術將整個感測器微小化。因此，在未來商業化產品的應用中，以電鍍鉛修飾Pt-Ti薄膜電極是最具有發展潛力。

　　Trichloroethylene (TCE) is a widely used organic solvent and degreasing agent in industry. However, the contamination of soil and groundwater with persistent organic pollutants is a matter of increasing concern such as TCE. There are many investigations implying the TCE is a carcinogenic material which causes serious health problems. Furthermore, how to control the concentration of TCE is a very important goal. In this study, the electrochemical reduction behaviors of TCE by using a Pb and an electrodeposited Pb modified electrodes in organic electrolyte were developed. Based on the data, a new amperometric TCE sensor can be designed with high performance, good sensitivity, short response time, nice reusability and long stability to monitor the concentration of TCE.
　　A novel conjugated polyacetylene chloride containing a chloric side chain which is synthesized from the TCE with an organic electrolyte by electropolymerization method. UV-Vis spectrum of the monomer shows an absorption maximum (λmax) around 315 nm due to the π-conjugation which exists in the monomer. The 1H NMR and GC-Mass spectra show that the main product is an acetylene chloride. Additionally, the phase transition temperature of polyacetylene chloride at 325 ˚C was examined by differential scanning calorimeter (DSC).
　　An amperometric TCE sensor by using a Pb electrode in an organic electrolyte was developed. The optimal pretreating and sensing conditions were found to be 1.0 M pretreatment HNO3 concentration, 30 min pretreatment time, -2.10 V (vs. Ag/Ag+ with 0.1 M tetrabutylammonium perchlorate (TBAP) in AN) sensing potential, 250 rpm agitation rate in a 0.025 M tetrabutylammonium tetrafluoroborate (TBAT) organic electrolyte. The response time and the sensitivity were 10 s and 7.15 μA/cm2-ppm, respectively. Additionally, at least 4 months stability for the prepared working electrode was also obtained. The correlation of the sensing response current, id, and TCE concentration, CL, is id=7.15CL in the range from 50 to 250 ppm TCE. The rate constant of (TCE) at mass-transfer control was found to be 4.86810-3 (cm-s)-1.
　　The TCE sensor by using an electrodeposited a Pb modified graphite electrode in an organic electrolyte was studied. The best electrodeposition conditions of the prepared working electrode were 20 mA/cm2 electrodeposition current density, 25 ˚C electrodeposition temperature and 2 hrs. Additionally, the optimal sensing conditions were -2.10 V sensing potential (vs. Ag/Ag+ with 0.1 M tetrabutylammonium perchlorate (TBAP) in acetonitrile (AN) solution), 100 rpm agitation rate, and at 25 ˚C with 0.01 M tetrabutylammonium tetrafluoroborate (TBAT) electrolyte concentration in AN solution were obtained in this system. Under the optimal sensing conditions, the results indicated that the sensitivity and response time were 7.06 μA/cm2-ppm and 15 s (90% response time), respectively. 　　　　　Furthermore, the stability is at least 60 days for prepared electrode. Additionally, the correlation of sensing response current, id, and trichloroethylene (TCE) concentration, CL, is id=7.06CL in the range from 100 to 700 ppm TCE. The rate constant of (TCE) at mass-transfer control was found to be 4.8110-3 (cm-s)-1.
　　Electrochemical detection of trichloroethylene with an electrodeposited Pb modified was designed. The optimal conditions for the preparation of the electrodeposited Pb modified electrode were obtained which 0.1 M pretreatment HNO3 concentration, 60 min pretreatment time, 20 mA/cm2 electrodeposition current density, 30 ˚C electrodeposition temperature and 2 hrs. The optimal sensing conditions such as -2.10 V sensing potential (vs. Ag/Ag+ with 0.1 M tetrabutylammonium perchlorate (TBAP) in acetonitrile (AN) solution), 155 rpm agitation rate, and at room temperature with 0.01 M tetrabutylammonium tetrafluoroborate (TBAT) electrolyte concentration in AN solution were obtained in this system. Under the optimal sensing conditions, the results indicated that the sensitivity and the response time were 1.06 μA/cm2-ppm and 20 s (90% response time), respectively. Furthermore, the stability is at least 60 days for prepared electrode. Additionally, the correlation of sensing response current, id, and trichloroethylene (TCE) concentration, CL, is id=1.06CL in the range from 50 to 700 ppm TCE. The rate constant of (TCE) at mass-transfer control was found to be 7.21710-4 (cm-s)-1.
　　A novel electrochemical TCE sensor using an electrodeposited Pb modified Pt-Ti thin film electrode was successfully developed and well characterized. The prepared conditions of the electrodeposited Pt-Ti thin film working electrode were obtained as 310-3 torr sputtering pressure, 20 min sputtering deposition time ,30 watts sputtering power, 18.75 mA/cm2 and 2 hrs under room temperature. Optimal sensing conditions were found to be -2.10 V (vs. Ag/Ag+ with 0.1 M tetrabutylammonium perchlorate (TBAP) in acetonitrile (AN) solution) sensing potential, 250 rpm agitation rate. At room temperature, the sensitivity and response time was 2.86μA/cm2-ppm and 15 s (90% response time), respectively. Furthermore, the prepared electrode had over 15 cycles of reusability, and the stability is least 180 days. Additionally, the correlation of sensing response current, id, and trichloroethylene (TCE) concentration, CL, is id=2.86CL in the range from 100 to 700 ppm TCE. The rate constant of (TCE) at mass-transfer control was found to be 2.43410-3 (cm-s)-1.
　　In this study, the framework of the TCE sensor with an electrodeposited Pb modified Pt-Ti thin film electrode can be obtained excellent sensing performances such as the sensitivity, the response time, the reusability and the stability. Additionally, the electrodeposited Pb modified Pt-Ti thin film electrode can be combined with microfabrication technique for the design of TCE sensor. Therefore, the electrochemical TCE sensor using an electrodeposited Pb modified Pt-Ti thin film electrode in TBAT organic electrolyte showed promising features for commercial application.

中文摘要	I
Abstract	IV
誌謝	VIII
目錄	IX
表目錄	XV
圖目錄	XVI
符號說明	XXI
第一章 緒論	1
1前言	1
2三氯乙烯分析方法	2
3三氯乙烯感測器偵測方式	3
4有機化合物的氧化還原反應	6
5氯乙炔與共軛高分子簡介	7
5.1氯乙炔簡介	7
5.2共軛高分子簡介	7
5.2.1聚乙炔簡介	12
6電流式感測器	13
7研究動機與目的	13
7.1研究動機	13
7.2研究目的	14
第二章 理論分析	15
1鹵化物的電化學還原反應機構	15
2三氯乙烯電化學理論分析	16
2.1反應控制模式	16
2.2質傳控制模式	21
3鉛的電化學特性	23
4電鍍鉛的特性	24
4.1電鍍鉛之鍍液成份	24
5有機助電解質的選擇	24
第三章 實驗	27
1藥品及儀器設備	27
1.1藥品	27
1.2儀器設備	28
2實驗步驟	29
2.1三氯乙烯電解合成裝置及分析方法	29
2.2三氯乙烯感測器的裝置	32
2.3電鍍鉛修飾碳片電極的製備	33
2.4電鍍鉛修飾鉛箔電極	33
2.4.1基材的前處理	33
2.4.2電鍍鉛修飾鉛箔電極的製備	33
2.5微小化電極系統	34
2.5.1 Pt-Ti與Pb-Pt-Ti薄膜電極的製備	34
2.5.2電鍍鉛修飾薄膜電極的製備	35
2.6三氯乙烯的感測分析	36
2.7製備工作電極表面特性分析	38
第四章 三氯乙烯電化學反應行為之研究	39
1前言	39
2結果與討論	39
2.1三氯乙烯電化學反應	39
2.1.1線性伏安法求取三氯乙烯之還原反應	39
2.1.2助電解質種類對陰極電流的影響	45
2.1.3不同陰極電位對反應級數的影響	46
2.2氯乙炔特性分析	49
2.2.1氯乙炔pH值測定	49
2.2.2氯乙炔光譜分析	51
2.2.3氯乙炔之氣相-質譜分析	52
2.3聚氯乙炔特性分析	55
2.3.1聚氯乙炔之表面分析	55
2.3.2聚氯乙炔之熱分析	55
2.3.3聚氯乙炔之光譜分析	56
2.3反應機構的探討	62
3結論	62
第五章 應用鉛片電極感測三氯乙烯之研究	63
1前言	63
2結果與討論	63
2.1電極表面之特性分析	63
2.2極限電流的測定	64
2.3三氯乙烯感測應答測試與校正曲線	67
2.4感測攪拌速率對感測靈敏度的影響	67
2.5感測TBAT有機電解質濃度對感測靈敏度的影響	71
2.6製備電極之鉛片前處理硝酸濃度對感測靈敏度的影響	73
2.7製備電極之鉛片前處理時間對感測靈敏度的影響	73
2.8工作電極穩定性測試	80
2.9理論與實驗結果比較	80
3結論	84
第六章 應用電鍍鉛修飾碳片電極感測三氯乙烯之研究	85
1前言	85
2結果與討論	86
2.1電極表面之特性分析	86
2.2極限電流的測定與其施加電位的探討	86
2.3三氯乙烯感測應答測試與校正曲線	94
2.4感測攪拌速率對感測靈敏度與應答時間的影響	97
2.5感測TBAT有機電解質濃度對感測靈敏度與應答時間的影響	100
2.6製備電極之電鍍電流密度對感測靈敏度的影響	103
2.7製備電極電鍍溫度對感測靈敏度的影響	103
2.8製備電極電鍍時間對感測靈敏度與應答時間的影響	108
2.9工作電極穩定性測試	113
2.10實際廢水之感測應答測試	113
2.10.1工廠研發部門廢水之感測應答測試	113
2.10.2工廠化學機械研磨廢水之感測應答測試	114
2.10.3學校高分子合成廢水之感測應答測試	114
2.11理論與實驗結果比較	120
3結論	121
第七章 應用電鍍鉛修飾鉛箔電極感測三氯乙烯之研究	122
1前言	122
2結果與討論	123
2.1電極表面之特性分析	123
2.2極限電流的測定與其施加電位的探討	123
2.3三氯乙烯感測應答測試與校正曲線	132
2.4感測攪拌速率對感測靈敏度與應答時間的影響	135
2.5感測TBAT有機電解質濃度對感測靈敏度與應答時間的影響	138
2.6製備電極之鉛箔前處理硝酸濃度對感測靈敏度的影響	141
2.7製備電極之鉛箔前處理時間對感測靈敏度的影響	141
2.8製備電極之電鍍電流密度對感測靈敏度的影響	148
2.9製備電極之電鍍時間對感測靈敏度的影響	153
2.10製備電極之電鍍溫度對感測靈敏度的影響	157
2.11工作電極穩定度測試	157
2.12實際廢水之感測應答測試	163
2.13理論與實驗結果比較	165
3結論	166
第八章 應用薄膜電極感測三氯乙烯之研究	167
1前言	167
2結果與討論	167
2.1極限電流的測定	167
2.1.1 Pt-Ti薄膜電極之極限電流的測定	167
2.1.2 Pb-Pt-Ti薄膜電極之極限電流的測定	168
2.1.3電鍍鉛修飾Pt-Ti薄膜電極之極限電流的測定	169
2.2三氯乙烯感測應答測試與校正曲線	173
2.2.1 Pb-Pt-Ti薄膜電極之三氯乙烯感測應答測試	173
2.2.2電鍍鉛修飾Pt-Ti薄膜電極之三氯乙烯感測應答測試	178
2.2.3電鍍鉛修飾Pt-Ti薄膜電極之三氯乙烯濃度校正曲線	178
2.3感測攪拌速率對感測靈敏度的影響	181
2.4感測TBAT有機電解質濃度對感測靈敏度的影響	181
2.5工作電極重覆使用性測試	184
2.6工作電極穩定度測試	184
2.7實際廢水之感測應答測試	189
2.7.1工廠研發部門廢水之感測應答測試	189
2.7.2工廠化學機械研磨廢水之感測應答測試	189
2.7.3學校高分子合成廢水之感測應答測試	190
2.8理論與實驗結果比較	194
3結論	194
第九章 綜合討論、結論與未來工作建議	196
1綜合討論	196
2總結	201
3未來工作建議	201
參考文獻	202
附錄	209
自述	260
著作	261

                                    

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