運用金奈米粒子/單壁奈米碳管複合材料修飾電極進行砷(ІІІ)之伏安法分析

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張雅雯(Ya-wen Chang) 查詢紙本館藏

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環境工程研究所

論文名稱

運用金奈米粒子/單壁奈米碳管複合材料修飾電極進行砷(ІІІ)之伏安法分析
(Voltammetric determination of arsenic (ІІІ) using gold nanoparticles / single walled carbon nanotubes composite-modified electrode)

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摘要(中)

本研究利用化學還原法及電鍍沉積法，以SWCNT為載體，透過前驅物四氯化金酸(HAuCl4)，製備GNP/SWCNT複合材料，進行材料特性分析與As(III)之伏安法分析。特性分析的部分，觀察材料的表面特性、表面積與孔洞大小、晶相變化、元素組成、官能基與製備條件在伏安法分析表現之影響，選出最佳金奈米粒子與奈米碳管合成比例。根據UHR-SEM與TEM觀察得知，金奈米粒子會隨著濃度高低附著或包覆於奈米碳管上，特別是電鍍形成的金奈米顆粒約2－5 nm，較容易均勻控制大小與分散於碳管表面。伏安法分析的同時也發現2－5 nm顆粒大小的金奈米顆粒測定As(III)造成的氧化峰電流最為尖銳，碳管能放大氧化峰電流值約3.8倍。後續以最佳比例進行As(III)之伏安法分析，選定最佳掃描條件，如掃速、pH。以及觀察修飾電極在掃描電位範圍上的限制，探討氧化峰電流與濃度之間的關係。結果顯示電鍍複合材料修飾電極以LSV測定50－5000 μg/L As(III)，得到良好濃度與電流的線性關係。最後推測干擾物Cu(II)對As(III)伏安法分析的影響與記憶效應。發現以LSV偵測As(III)及Cu(II)氧化峰電流的優點在於無明顯的記憶效應。具有開發線上即時監測放流水中As(III)之潛力與應用價值。

摘要(英)

Gold nanoparticle/SWCNT (GNP/SWCNT) composites were synthesized via chemical reduction and electro-plating using HAuCl4 as precursor. The surface characteristics of GNP/SWCNT, such as surface area as well as pore size, crystallinity, elemental composition, and functional groups were examined. From SEM and TEM analysis, it was shown that GNP synthesized via electroplating were about 2－5 nm and evenly distributed on the surface of SWCNT. Besides, it was found that when GNP were about 2－5 nm, the oxidation peak of As(III) was the sharpest and the peak current was about 3.8 times larger than the GCE electrode coated with GNP only. The linear scanning voltammetry of As(III) at different concentrations showed that the peak current has good relationship to the concentration of As(III) in the range of 50－5000 μg/L. At last, the interference of copper and the memory effects were also investigated. It was found that when analyzing As(III) via LSV, the was not obvious interference of copper and the memory effects.

關鍵字(中)

★ 伏安法
★ 金奈米粒子
★ 單壁奈米碳管
★ As(III)

關鍵字(英)

★ voltammetry
★ gold nanoparticles
★ single-walled carbon nanotube
★ arsenic

論文目次

目錄
摘要 I
ABSTRACT II
謝誌 III
目錄 V
圖目錄 IX
表目錄 XII
第一章　前言 1
1.1. 研究緣起 1
1.2. 研究目的 2
1.3. 研究流程 3
第二章　文獻回顧 4
2.1. 砷的型態與偵測方法 4
2.2. 伏安法分析 9
2.2.1 電化學反應與系統 9
2.2.2 伏安法分析原理 11
2.2.3 伏安法分析無機砷原理與應用 19
2.2.4 伏安法分析無機砷的電極種類與修飾基材 20
2.3. 奈米碳管 38
2.3.1 奈米碳管基本材料結構 39
2.3.2 奈米碳管之電學特性 41
2.3.3 奈米碳管的純化與改質 45
2.3.4 奈米碳管表面改質後對於電化學訊號的影響 48
2.3.5 奈米碳管固定於電極表面分析應用 53
2.4. CNT/金屬複合材料 56
2.4.1 GNP/CNT之金屬催化特性 56
2.4.2 GNP/CNT製備方式 58
2.4.3 GNP/CNT複合材料進行砷之電化學分析應用 62
第三章　實驗方法 64
3.1 材料與設備 65
3.1.1 實驗設備 65
3.1.2 實驗材料 68
3.2 實驗方法 70
3.2.1 GNP/SWCNT複合材料製備 70
3.2.2 材料特性分析 72
3.2.3 GNP/SWCNT複合材料修飾電極之製備 74
3.2.4 伏安法對砷之分析 74
第四章　結果與討論 77
4.1. 材料特性鑑定分析 77
4.1.1 奈米碳管純化前後之特性分析 77
4.1.2 化學合成(CGNP/SWCNT)複合材料之特性分析 83
4.1.3 電鍍合成(EGNP/SWCNT)複合材料之特性分析 91
4.1.4 製備條件在伏安法分析表現之影響 94
4.2. 掃描條件確定 99
4.2.1伏安法分析As(ІІІ)之掃速選定 99
4.2.2伏安法分析As(ІІІ)之pH選定 102
4.3. 伏安法分析不同濃度As(III) 105
4.3.1 電位範圍的限制 105
4.3.2 氧化峰電流與濃度之間的關係 108
4.4. Cu之干擾 111
4.4.1 GNP/SWCNT電極對Cu(II)之伏安法分析 111
4.4.2 GNP/SWCNT電極對As(ІІІ)與Cu(II)之伏安法分析 113
4.5. 記憶效應 115
第五章結論與建議 119
5.1. 結論 119
5.2. 建議 121
參考文獻 122
附錄 136

圖目錄
Fig. 1-1 研究流程 3
Fig. 2-1 25℃及1大氣壓下，水中砷物種之Eh-pH圖 6
Fig. 2-2 電化學反應的各種變因 9
Fig. 2-3 三電極電解槽系統 10
Fig. 2-4 循環伏安法之電位控制圖 14
Fig. 2-5 擴散控制之循環伏安圖 14
Fig. 2-6 吸附控制之循環伏安圖 16
Fig. 2-7 方波伏安法之波形圖 17
Fig. 2-8 循環伏安法之電流圖 17
Fig. 2-9 微分脈衝伏安法所施加之電位波形圖 18
Fig. 2-10 A→B氧化反應於裸電極、均相及非均相化學修飾電極示意圖 21
Fig. 2-11 近期偵測無機砷的修飾電極材料之發展 23
Fig. 2-12 透過自組裝膜(SAMs)於金電極放大電化學偵測As(III)訊號 25
Fig. 2-13 酶的反應序列偵測抑制As(V) 29
Fig. 2-14 碳管結構示意圖 40
Fig. 2-15 奈米碳管的結構二維平面石墨向量 42
Fig. 2-16 奈米碳管排列結構 42
Fig. 2-17 CNT改質之官能基化 47
Fig. 2-18 奈米碳管表面常見化學改質所引入之官能基 49
Fig. 2-19 SWCNT上羧基之還原氧化機制 50
Fig. 2-20 不同修飾電極分析cytochrome c之CV圖 51
Fig. 2-21 經由不同酸氧化劑處理後MWCNT之CV圖 53
Fig. 2-22 利用CNT/nafion/GCE電極分析不同濃度之多巴胺 54
Fig. 3-1 TEM基本構造儀器示意圖 66
Fig. 3-2 單壁奈米碳管的拉曼光譜圖 69
Fig. 3-3 電化學反應槽 75
Fig. 4-1 HUR-SEM單壁奈米碳之表面管束型態圖 79
Fig. 4-2 TEM單壁奈米碳管之管狀結構圖 80
Fig. 4-3 純化奈米碳管孔洞分佈圖 81
Fig. 4-4 純化前後SWCNT之FTIR圖譜 83
Fig. 4-5 不同SWCNT：GNP之CGNP/SWCNT之SEM影像 84
Fig. 4-6 不同SWCNT：GNP之CGNP/SWCNT之TEM影像 85
Fig. 4-7 X-ray繞射分析圖譜之CGNP/SWCNT 86
Fig. 4-8 化學合成法製程濾液之UV示意圖 89
Fig. 4-9 CGNP/SWCNT複合材料之FT-IR圖譜 91
Fig. 4-10 不同SWCNT：GNP之EGNP/SWCNT之SEM影像 92
Fig. 4-11 不同SWCNT：GNP之EGNP/SWCNT之TEM影像 93
Fig. 4-12不同濃度合成GNP複合材料修飾電極對5 mg/L As(ІІІ)LSV圖 97
Fig. 4-13 CGNP/SWCNT對As(ІІІ)不同掃速之影響 100
Fig. 4-14 EGNP/SWCNT對As(ІІІ)不同掃速之影響 101
Fig. 4-15 pH範圍0.47至12對5 mg/L As(ІІІ)之循環伏安圖 103
Fig. 4-16 5 mg/L As(III)在不同pH下之物種分布圖 104
Fig. 4-17 EGNP對不同濃度As(ІІІ)以-0.6 V至1V掃描範圍之CV圖 106
Fig. 4-18 EGNP對不同濃度As(ІІІ)以-0.4 V至0.4 V掃描範圍之CV圖 107
Fig. 4-19 CGNP/SWCNT對不同濃度As(ІІІ)之LSV圖 109
Fig. 4-20 EGNP/SWCNT對不同濃度As(ІІІ)之LSV圖 110
Fig. 4-21 不同濃度Cu(II)之LSV圖 112
Fig. 4-22 等量As(ІІІ)與Cu(II)之LSV圖 114
Fig. 4-23 固定5 mg/L As(ІІІ)與不同濃度Cu(II)之LSV圖 114
Fig. 4-24 EGNP/GCE同時對5 mg/L As(ІІІ)與Cu(ІІ)測試20次後觀察複合材料修飾電極的記憶效應 116
Fig. 4-25 CGNP/SWCNT/GCE同時對5 mg/L As(ІІІ)與Cu(ІІ)測試20次後觀察複合材料修飾電極的記憶效應 117
Fig. 4-26 EGNP/SWCNT/GCE同時對5 mg/L As(ІІІ)與Cu(ІІ)測試20次後觀察複合材料修飾電極的記憶效應 118

表目錄
Table 2-1 Esquina與Illapata村民頭髮中砷物種含量分析 5
Table 2-2 不同砷物種之游離常數(pKa) 6
Table 2-3 SWCNT和MWCNT的維度特性 40
Table 2-4 奈米碳管原子排列之結構與性質 42
Table 2-5 各種型態奈米碳管之特點及應用比較 44
Table 2-6 四種介面活性劑簡介 60
Table 4-1 單壁奈米碳管純化前後之元素半定量分析 81
Table 4-2 純化前後之Boehm titration官能基分析 82
Table 4-3 CGNP/SWCNT之元素半定量分析 87
Table 4-4 TEM與UV分析CGNP顆粒大小與文獻對照表 90
Table 4-5 EGNP/SWCNT之元素半定量分析 94
Table 4-6 CGNP/SWCNT分析5 mg/L As(ІІІ)之電容與電流值 97
Table 4-7 EGNP/SWCNT分析5 mg/L As(ІІІ)之電容與電流值 98

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Cheap Tube Inc. "http://www.cheaptubes.com/"

指導教授

秦靜如(Ching-Ju Monica Chin)

審核日期

2015-7-27

推文