電化學沉積修飾電極於電化學感測器之應用｜國立清華大學博碩士論文庫

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研究生：	連健宏 Lien, Chien-Hung
論文名稱：	電化學沉積修飾電極於電化學感測器之應用 Modified Electrodes via Electrodeposition for Electrochemical Sensors
指導教授：	胡啟章 Hu, Chi-Chang 汪上曉 Wong, Shan-Hill
口試委員:	萬其超溫添進陳生明何佳安黃景帆
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：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	167
中文關鍵詞：	鉍薄膜電極、電鍍、複合電極、重金屬感測器、非酵素型葡萄糖感測器
外文關鍵詞：	Bismuth film electrode (BFE), Electrodeposition, Composite electrode, Heavy-metal sensor
相關次數：	點閱：1 下載：0
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由於日益嚴重的環境污染和健康照護問題，本研究致力於發展重金屬感測器及非酵素型-雙材料葡萄糖感測器.
首先,在重金屬離子感測器部分，主要著眼於篩選出影響Sn2+靈敏度的鉍薄膜電極關鍵因素。由實驗結果發現，鉍薄膜電極的最佳成晶面向比例(preferred orientation ratio)是主要關鍵因素，但是當最佳成晶面向比例高於0.11時，晶粒尺寸(grain size)大小和最佳成晶面向比例的協同作用(synergistic effect)，讓Sn2+的偵測能力提升。根據此結果，由部分因素實驗設計，我們找出影響最佳成晶面向比例的因素為溶液的pH值和溫度。因此，我們可以控制最佳成晶面向比例由0.09至1.09，並建立最佳成晶面向比例和偵測Sn2+感測能力的關係。
在重金屬離子感測器得第二部分，乃致力於開發氟烯磺酸聚合物(Nafion)修飾石墨烯/奈米碳管及金屬Bi的網版印刷複合電極(簡寫為：Nafion-G/CNT-BiSPE)，並將此電極用於微量的鉛離子偵測。結果發現，Nafion-G/CNT-BiSPE複合電極對於Pb2+的偵測，其電流應答(current response)遠大於其他單一成分之Bi電極。由部分因素實驗設計結果發現，對於Nafion-G/CNT-BiSPE複合電極，影響Pb2 +的偵測的主要因素影響為分析溶液的和Nafion濃度。由此結果，進一步進行陡升實驗，發現在pH值4.75及Nafion濃度0.3%時，偵測1ppm Pb2+的電流可由0.65uA上升至1.03uA。最後，我們使用此複合電極與其他電極在最佳偵測條件下相比較，發現複合電極對於 1ppm Pb2+的偵測，有最佳的偵測電流。
在最後一章節，我們介紹一種新穎的非酵素葡萄糖感測器，此感測器經由使用電沉積方式製備(Ni-Co)(OH)2複合材料於網版印刷碳電極上。研究結果顯示，相較於Ni(OH)2 和Co(OH)2 ，(Ni-Co)(OH)2有明顯的葡萄糖催化行為及較低的氧化電位，此特性歸因於Ni離子和Co離子的原子級混合。在定電位安培法檢測下，可得校準曲線(calibration curve)線性範圍為0 - 3.7mM，靈敏度為122.45 uA mM−1 cm−2，相關係數為0.989。此外， 25uM的抗壞血酸(Ascorbic acid)，尿酸(Uric acid)和多巴胺 (Dopamine) 的干擾測試結果顯示：其干擾百分比為10.76％，14.29％和1.41％，(相較於0.2mM葡萄糖的電流應答)。因此，由以上實驗結果得知本實驗室所開發之非酵素型葡萄糖感測器複合材料，擁有較明顯的葡萄糖催化行為，較低的氧化電位及較大校準曲線範圍。

The study aims at the development of the heavy metal ion sensors and the non-enzymatic glucose sensor consisting of binary materials due to the growing concerns about the environmental pollution and the health care issue, respectively.
In the first part of the study for heavy metal ion sensors, we developed the bismuth film electrodes (BFEs) for the detection of Sn2+. The preferred orientation ratio (f) of the deposited bismuth was found to be a key factor determining the Sn2+-sensing ability of BFEs. Especially when f is above 0.11, the synergistic effect from the grain size and the f value on the sensing ability for Sn2+ can be observed. Since the fractional factorial design (FFD) of experiments indicate that the deposition pH value and the temperature affect the f of the deposited bismuth, the f was controlled from 0.09 to 1.09 by adjusting these two factors to establish the relationship between the preferred orientation of the deposited bismuth and the sensing ability for Sn2+.
The second heavy metal ion sensor utilized Nafion-modified (graphene/carbon nanotube) composite to deposit with Bi on the screen printed electrodes (SPEs) for detecting trace amount of Pb2+. The preliminary test shows that the Pb2+-sensing ability for Nafion-(G/CNT)-BiSPE was 50-times higher than that of BiSPE. The FFD study revealed that the key factors determining the sensing ability are the deposition pH value and the concentration of Nafion. The steepest ascent pathway (SAP) study further established that the highest sensing ability for Pb2+ can be achieved when utilizing 0.3% Nafion and the stripping buffer solution with the pH equals to 4.75. Finally, the sensitivity and the sensing current obtained under the optimal conditions for SPE, Bi/SPE, Bi/Nafion/SPE, Bi/G-CNT/SPE, and Bi/Nafion/G-CNT/SPE were compared by the results from sqaure wave anodic stripping voltammetry (SWASV).
In the last part, we introduced a novel non-enzymatic glucose sensor via the cathodic deposition of nickel-cobalt hydroxide (denoted as (Ni-Co)(OH)2) on the screen-printed carbon electrodes (SPCEs). Due to the atomic-scale mixing of Ni and Co ions, (Ni-Co)(OH)2 demonstrates the more significant signal and the less positive detecting potential for glucose oxidation compared with Co(OH)2 and Ni(OH)2, respectively. The detection sensitivity for glucose is 122.45 uA mM−1 cm−2 (R2 = 0.989) in the linear detection range up to 3700 uM. In addition, low interference responses from 25 uM ascobic acid (AA), uric acid (UA), and dopamine (DA) were obtained, which were 10.76 %, 14.29 %, and 1.41 % of the detection signal from 0.2 mM glucose, respectively. Consequetly, the non-enzymatic glucose sensor exhibits the low detecting potential, the wide linear detection range, and the high signal-to-noise ratio.

Table of contents
謝 誌    i
Abstract    iii
中文摘要    v
Table of contents    vii
List of Tables    x
List of Figures    xii
Chapter 1 Introduction and Objective    1
Chapter 2 Literature Review    3
1    Introduction of sensor    3
1.1    Introduction of chemical sensor    4
1.2    Recognition elements of heavy-metal ion sensor:    8
1.3    Brief introduction of tin ion sensor:    12
1.4    Brief introduction of lead ion sensor:    14
1.5    Glucose sensor    16
2    Electroplating    24
2.1    Basic electroplating concepts    24
2.2    Metal electrodeposited mechanism    26
2.3    Metal oxide/hydroxide electrodeposited mechanism    29
3    Design of experiments    32
3.1    Fractional factorial design    32
3.2    ANOVA test    35
3.3    Path of the steepest decent/ascent study    36
Chapter 3 Experimental    37
1    Chemicals    37
2    Instruments    39
2.1    Common instruments    39
2.2    Electroplating system    40
2.3    CHI (electrochemical analytical system)    41
3    Preparations of various electrodes    42
3.1    Preparation of Bismuth electrodes    42
3.2    Preparation of Nafion-G/CNT-BiSPE    46
3.3    Preparation of Ni(OH)2, Co(OH)2 and (Ni-Co)(OH)2    50
4    Electrochemistry analytical methods    51
4.1    Cyclic voltammetry (CV)    51
4.2    Square-Wave voltammetry (SWV)    54
4.3    Differential pulse voltammetry (DPV)    57
4.4    Amperometric method    59
Chapter 4 Results and Discussion    61
1    Bismuth film electrode for square wave voltammetric determination of tin    ………………………………………………………………………….61
1.1    Introduction    61
1.2    Textural Analysis of four different bismuth samples    62
1.3    Key factors affecting the Sn2+ sensitivity of Bi deposits    66
1.4    The reason of f factor affecting the Sn2+sensitivity    68
1.5    Fractional factorial design of f    73
1.6    The steepest decent/ascent study of f    81
1.7    The relationship between f and Sn2+-sensing ability    84
1.8    Summary    87
2    Green electrode for square wave voltammetric determination of lead ion    ………………………………………………………………………………..88
2.1    Introduction    88
2.2    Textural analyses of various composite electrodes    89
2.3    Study on Nafion-G/CNT-BiSPE    93
2.4    Qualitative descriptions for the SWASV measurement    95
2.5    Fractional factorial design    97
2.6    The effect of pH & concentration of Nafion    105
2.7    Study of the steepest decent/ascent path    107
2.8    Study of SPE modified with different films    110
2.9    Comparison of SPE modified with different films    112
2.10    Summary    114
3    Non-enzymatic Glucose Sensor with (Ni-Co)(OH)2 Composite Material    ………………………………………………………………………………115
3.1    Introduction    115
3.2    Textural analyses of various composite electrodes    116
3.3    Concentration effects of Ni2+ & Co2+    120
3.4    Concentration effects of electrolyte    124
3.5    Concentration effects of electrolyte mixture    127
3.6    Study on binary (Ni-Co)(OH)2    130
3.7    Amperometric response of Ni(OH)2/Co(OH)2    136
3.8    Real sample test    141
3.9    Summary    143
Chapter 5 Conclusions and Future Prospects    144
1    Conclusions    144
2    Future Prospects    146
Reference    155
CV and Publications    164
 

                                

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