聚苯胺與金屬奈米結構複合材料之研究

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洪筱鵬(Shiau-Peng Hung) 查詢紙本館藏

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化學工程與材料工程學系

論文名稱

聚苯胺與金屬奈米結構複合材料之研究

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摘要(中)

摘要
本研究主題主要有兩大部分:第一部分利用過硫酸銨或四氯金酸做為氧化劑,在氧化鋁濾膜或聚碳酸酯膜的模板中,化學合成聚苯胺奈米管。並藉由SEM及TEM影像觀察聚苯胺奈米管的表面形態及中空管柱結構。以FT-IR鑑定在模板中化學合成的產物是否為聚苯胺結構。另一方面,亦利用四氯金酸/硝酸銀/硫酸銅/硝酸鈀做為氧化劑,直接與苯胺鹽單體進行化學合成。藉由SEM影像分析聚苯胺纖維的表面形態；以及金屬顆粒沉積的現象。再者,以TEM影像分析聚苯胺及金屬複合材料,由EDX分析金屬顆粒成份；再由選區電子繞射(SAED)來判別聚苯胺及金屬複合材料中金屬顆粒的晶型,並且可知道其晶格構造。由FT-IR鑑定這些不同氧化劑與苯胺鹽單體間所形成的產物是否為聚苯胺結構。最後以四點探針去量測聚苯胺及金屬複合材料塊材的導電度。
第二部分則利用聚苯胺具有還原的特性，以聚苯胺奈米管將金、銀、銅或鈀離子還原,因此可得到聚苯胺金/銀/銅/鈀雙層奈米管。本研究以氧化鋁膜或聚碳酸酯膜做為模板,利用電化學法先合成聚苯胺的管狀結構，再將聚苯胺管浸置於HAuCl4/AgNO3/CuSO4/Pd(NO3)2溶液中，即可得到聚苯胺金/銀/銅/鈀雙層管，並利用NMP將聚苯胺完全溶解後,即可得到金、銀、銅或鈀奈米管。另一方面,本研究也利用無電電鍍的方法,成功製備出聚苯胺銅/鎳奈米雙層管。先將電化學合成的聚苯胺管浸置於無電電鍍銅或無電電鍍鎳的混合溶液中，利用還原劑將銅或鎳離子還原並沉積在聚苯胺管,如此可製備出聚苯胺銅或鎳的奈米雙層管。藉由SEM影像觀察聚苯胺金屬雙層管及奈米金屬管的表面型態；並利用EDX成份分析確定是否為金、銀、鈀、銅或鎳管。以TEM影像分析所合成的聚苯胺金屬雙層管的內部結構；另外,由選區電子繞射(SAED)、暗視野影像(DF)分析各種不同金屬管的晶型及晶格結構；並以EDX成份分析確定是否為金、銀、鈀、銅或鎳管。由FT-IR鑑定在不同模板及孔徑中,其電化學合成的產物是否為聚苯胺結構。最後以循環伏安圖譜(CV)分析在不同模板及孔徑中,聚苯胺管的不同氧化態。

摘要(英)

Abstract
In this study, we have two main topics: Firstly, we synthesized polyaniline (PANI) nanotubes using ammonium peroxydisulfate (APS) or chloroaurate acid (HAuCl4) as the oxidant by chemical method within the pores of anodic aluminum membrane (AAO) or polycarbonate track-etched membrane (PTM). We observe the surface morphology and hollow tube structure of PANI nanotubes by SEM and TEM photographs. From the study of FT-IR spectra, we confirm that the product is PANI produced in the pores of the template. On the other hand, we also use aqueous solutions of HAuCl4/ AgNO3/CuSO4/Pd(NO3)2 as the oxidant for the synthesis of PANI/metal composites. We observe the composites of PANI fibers and metal particles by SEM and TEM photographs. In addition, the metal particles formation can be proved from EDX analysis. Selected area electron diffraction (SAED) results indicate the crystal type and structure of the metal particles in PANI/metal composites material. We confirm that the product is PANI produced from the reaction between aniline and HAuCl4/ AgNO3/CuSO4/Pd(NO3)2 by means of FT-IR spectra. we also measure the conductivity of PANI/metal composites bulk material by Four-Point Conductive measurements.
Secondly, we can prepare gold/silver/copper/palladium nanotubes by reducing ability of PANI nanotubes. In this study, we use AAO or PTM as templates to synthesize PANI nanotubes by electrochemical method. AAO or PTM with PANI nanotubes were then immersed in HAuCl4 /AgNO3/CuSO4/Pd(NO3)2 solution. PANI Au/Ag/Cu/Pd bilayer nanotubes can be obtained. After dissolving polyaniline with NMP, then we obtain Au/Ag/Cu/Pd nanotubes. Besides, we also prepare PANI Cu/Ni bilayer nanotubes by electroless plating method. AAO or PTM with PANI nanotubes were immersed in electroless plating of copper or nickle solution.Therefore,we can obtain PANI Cu/Ni bilayer nanotubes by reductant to reduce copper or nickle ions and deposit them in PANI nanotubes. Cu/Ni nanotubes can be obtained by dissolving PANI with NMP. We observe the surface morphology of PANI metal bilayer nanotubes or metal nanotubes by SEM photographs. In addition, the formation of Au/Ag/Cu/Pd/Ni nanotubes can be proved from EDX analysis. We also observe hollow tube structure of PANI metal bilayer nanotubes from TEM photographs. Furthermore, SAED and Dark Field (DF) results indicate the crystal type and structure of the metal tube. The reduction/oxidation (redox) behaviors of PANI nanotubes within AAO or PTM in HCl solution were studied by Cycilic Voltammmetry.

關鍵字(中)

★ 暗視野影像
★ 循環伏安圖譜
★ 雙層奈米管
★ 選區電子繞射

關鍵字(英)

★ Dark Field
★ Selected area electron diffraction
★ bilayer nanotubes
★ Cycilic Voltammmetry

論文目次

目錄
摘要……………………………………………………………………..Ⅰ
Abstract………………………………………………………………….Ⅲ
目錄……………………………………………………………………..Ⅴ
表目錄…………………………………………………………………..Ⅹ
圖目錄………………………………………………………..………ⅩⅠ
第一章緒論……………………………………………………………..1
第二章文獻回顧………………………………………………………..3
2.1聚苯胺………………..………………………………………...3
2.1.1簡介……………………………………..…………………3
2.1.2聚苯胺的結構………………………………………..……5
2.1.3聚苯胺的合成方式……………………………………..…9
2.1.4聚合機構及氧化還原機制………………………………12
2.1.5聚苯胺紅外光光譜分析…………………………………15
2.1.6聚苯胺的應用………..………………………………..…18
2.2聚苯胺奈米管...................……………….………21
2.2.1簡介…………………………….…….………..…………21
2.2.2 聚苯胺奈米管的合成方法………….……………….....23
2.2.3聚苯胺奈米管的合成機制……………..…………..……27
2.2.4聚苯胺奈米結構的應用………...…………………..…...28
2.3聚苯胺與金屬奈米複合材料……………………………...…30
2.3.1簡介………………………………………………………30
2.4研究動機與目的………………………………..…………….35第三章聚苯胺管與聚苯胺金屬複合材料之研究………………...….36
一、實驗…………………………………………...……..………….36
1.1藥品……………………………….…………………………36
1.2 儀器………………………………………..….…….……….37
1.3 實驗方法……………………………………….……………38
1.3.1苯胺單體的還原……………………..…………..………38
1.3.2化學合成聚苯胺奈米管……………….………..……….38
1.3.3化學合成聚苯胺及金屬複合材料…………………...….39
1.4 實驗分析…………………………………..….……………..41
1.4.1場發射掃瞄式電子顯微鏡(Field-Emission Scanning
Electron Microscope，FE-SEM)……………………..….41
1.4.2低真空掃瞄式電子顯微鏡（Low Vacuum Scanning
Electron Microscope，LV-SEM）………….………...…...41
1.4.3穿透式電子顯微鏡(Transmission Electron Microscope，
TEM)……………………………………………………41
1.4.4 霍氏轉換紅外光譜儀分析(Fourier Transform-Infrared
Spectrophotometer，FT-IR)……………...…………….42
1.4.5 四點探針導電度測試(Four-Point Conductive Meter)…42
二、結果與討論…………………………………….….…………….43
(一) 化學合成聚苯胺奈米管………………………………..…….43
2.1聚苯胺奈米管SEM影像分析……………………...…..……43
2.1.1 以過硫酸銨為氧化劑,在商業化的氧化鋁濾膜內化學合
成聚苯胺奈米管………………………….…………….43
2.1.2 以過硫酸銨為氧化劑,在商業化的聚碳酸酯膜化學合成
聚苯胺奈米管…………………………………..………46
2.1.3 以四氯金酸為氧化劑,在商業化的氧化鋁濾膜內化學合
成聚苯胺奈米管………………………………………..49
2.1.4 以四氯金酸為氧化劑, 在商業化的聚碳酸酯膜內化學合
成聚苯胺奈米管…………….…………………………..56
(二) 化學合成聚苯胺及金屬複合材料…………………..……….63
2.2聚苯胺與金屬複合材料SEM影像分析………………...….63
2.2.1以不同金屬水溶液為氧化劑,化學合成聚苯胺與金屬的
複合材料…………………………………………..……63
2.3聚苯胺奈米管TEM影像分析………………………..….…..71
2.4聚苯胺及金屬複合材料的TEM影像分析………………….79
2.5化學合成聚苯胺管及聚苯胺金屬複合材料之紅外光光譜分
析……………………………………………………………..87
2.6聚苯胺及金屬複合材料之導電度分析…………..……….…91第四章聚苯胺與金屬雙層管之研究…………………………………92
一、實驗………………………………..……………………………..92
1.1藥品……………………………….……………………….…92
1.2儀器……………………………………….…….……………94
1.3實驗方法…………………………..………………………….95
1.3.1以聚苯胺管為還原劑沉積金屬,合成聚苯胺及金屬
奈米雙層管……………………………….....…………..95
1.3.2以無電電鍍法沉積金屬,合成聚苯胺及金屬奈米雙層
管………………………………………………………...95
1.4實驗分析………………………………..……….……………97
1.4.1場發射掃瞄式電子顯微鏡(Field-Emission Scanning
Electron Microscope，FE-SEM)……………………..….97
1.4.2低真空掃瞄式電子顯微鏡（Low Vacuum Scanning
Electron Microscope，LV-SEM）……………….……….97
1.4.3穿透式電子顯微鏡(Transmission Electron Microscope，
TEM)…………………….…………….…………..……..97
1.4.4 霍氏轉換紅外光譜儀分析(Fourier Transform-Infrared
Spectrophotometer，FT-IR)…………………..………..98
1.4.5循環伏安法圖譜(Cyclic Voltammograms，CV)……….98
二、結果與討論……………………………...........……………….99
(三) 聚苯胺及金屬雙層奈米管的合成……………………..…….99
2.1聚苯胺及金屬雙層奈米管SEM影像分析………………....99
2.1.1聚苯胺及銅雙層管………………………….…………..100
2.1.1.1利用聚苯胺管本身的還原能力,將銅離子還原成銅
管……………………………………………………100
2.1.1.2將聚苯胺管及模板複合材料浸置於無電電鍍銅溶液,
以還原劑將銅離子還原成銅管………………...….105
2.1.1.3無電電鍍直接合成銅管……………………………110
2.1.2聚苯胺及鈀雙層管……………...………...…………….111
2.1.2.1利用聚苯胺管本身的還原能力,將鈀離子還原成鈀
管……………………………………………………111
2.1.2.2無電電鍍直接合成鈀管……………………..……..116
2.1.3聚苯胺及鎳雙層管……………………………………..117
2.1.3.1將聚苯胺管及模板複合材料浸置於無電電鍍鎳溶液,
以還原劑將鎳離子還原成鎳管…………………....117
2.1.3.2無電電鍍直接合成鎳管……………………………122
2.2聚苯胺及金屬雙層奈米管TEM影像分析………….……123
2.2.1金管的TEM影像分析……………………...………….124
2.2.2聚苯胺銀雙層管及銀管的TEM影像分析………...….128
2.2.3聚苯胺鈀雙層管及鈀管的TEM影像分析…..….…….132
2.2.4聚苯胺銅雙層管及銅管的TEM影像分析………...….137
2.2.5聚苯胺鎳雙層管及鎳管的TEM影像分析…………….142
2.3電化學合成聚苯胺管之紅外光光譜分析…………..……..145
2.4 聚苯胺管之電化學分析……………………..…………….146
第五章總結論…………………………………….………………….148
第六章未來發展……………………………………………………..150
參考文獻………………………………………………..……………..151
附錄一:實驗室自製氧化鋁膜……………………………………..….161
1.1自製正反面均一且孔徑為30nm的氧化鋁濾膜…….....….161
附錄二: 聚苯胺及金屬複合材料導電度的原始數據…….…………165
附錄三: 電化學方法合成聚苯胺管的電流與時間關係圖………….170
附錄四: 本論文SEM及TEM所有結果的一覽表………..…………172
附錄五: 本論文聚苯胺及金屬雙層管的選區電子繞射(SAED)圖....175

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指導教授

楊思明(Sze-Ming Yang)

審核日期

2006-7-21

推文