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研究生:李美津
研究生(外文):Mei-Chin Li
論文名稱:環境應用奈米複合材料Fe-Ni/CNT之製備及特性分析
論文名稱(外文):Fabrication and characterization of Fe-Ni nanoparticles supported onto CNT for environmental applications
指導教授:謝淑惠謝淑惠引用關係
指導教授(外文):Shu-Huei Hsieh
學位類別:碩士
校院名稱:國立虎尾科技大學
系所名稱:材料科學與綠色能源工程研究所
學門:工程學門
學類:綜合工程學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:中文
論文頁數:109
中文關鍵詞:奈米碳管無電鍍
外文關鍵詞:carbon nanotubeselectroless
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本研究主要結合奈米材料Fe-Ni雙金屬的氧化分解能力及奈米碳管的吸附能力,發展新的奈米複合材料Fe-Ni/CNT,以處理日趨複雜的水污染。
本研究首先將多壁奈米碳管以化學氧化法做純化改質處理能使其純度較純化改質前提高5 wt%、比表面積提高1.89倍、表面電位下降約10~20 mV以及表面官能基(-COOH及-OH)提高1.45倍,再控制無電鍍技術之製備參數包括:析鍍時間、析鍍溫度,鍍液中金屬離子比(Fe2+/Ni2+)、鍍液pH值及是否添加分散劑(SDS)等,研究朝提高Fe-Ni粒子的含鐵量與Fe-Ni粒子散佈固定在MWCNT上等目標進行,研究結果發現當製備參數為50 ℃、pH10、不添加分散劑、鍍液金屬離子比(Fe2+/Ni2+)7時,可得到最高鐵含量Fe = 40.55 at%(單位鐵含量111.17 mg/g)之奈米複合材料Fe-Ni/CNT,接著對其作一系列性質分析,最後評估奈米複合材料Fe-Ni/CNT對共處理混合汙染物之應用效益,結果顯示其在120分鐘時能夠同時吸附重金屬硝酸鉛離子10 ppm、重金屬硒酸根離子1 ppm及降解偶氮橘色染料AO7 50 ppm達放流水標準,且共處理後奈米Fe-Ni粒子以SEM/EDS分析仍剩餘50 %以上。
The purpose of this study combined with nanoparticles Fe-Ni bi-metallic oxidation capacity and the adsorption capacity of carbon nanotubes, the development of new nanocomposites Fe-Ni/CNT, to deal with the increasing complexity of water pollution.
First of all, this study will be multi-walled carbon nanotubes by chemical oxidation process purified so it can be modified to deal with than the purification of purity before the modified 5 wt%, more than 1.89 times the surface area to increase the surface potential decrease of about 10 ~ 20 mV and the surface functional base (-COOH and-OH) to increase 1.45 times, and then the control technology of electroless preparation parameters include: analysis of plating time, plating analysis of temperature, metal ions in solution than the (Fe2+ / Ni2+), bath pH and the added value of dispersion Agent (SDS) and other research towards Fe-Ni particles to increase the iron content and Fe-Ni particles spread in the MWCNT upper fixed targets,the results found that when the parameters for the preparation of 50 ℃, pH10, do not add dispersant, metal ions than the solution (Fe2 + / Ni2 +) 7, the highest iron content can be Fe = 40.55 at% (flat iron content 111.17 mg / g) of nanocomposites Fe-Ni/CNT, then for a series of the nature of its analysis, the final evaluation Fe-Ni/CNT nanocomposites were processed on the effectiveness of the application of mixed pollutants, the results showed that in 120 minutes at the same time when Adsorption of heavy metal ions lead nitrate 10 ppm, selenium heavy metal ion degradation of 1 ppm and orange azo dye AO7 50 ppm standard of effluents, and after a total Fe-Ni nano-particles to SEM / EDS analysis of more than 50% still remaining.
摘要 I
致謝 III
目錄 IV
圖目錄 VIII
表目錄 XI
第一章 緒論 1
1.1研究緣起與動機 1
1.2 研究目的 2
1.3研究架構 4
第二章 文獻回顧 5
2-1 無電鍍技術 5
2-1-1 無電鍍配方 5
2-1-2 無電鍍過程 6
2-1-3 無電鍍反應機構 7
2-2 奈米粒子製造方法及特性 9
2-2-1 奈米粒子常見之合成方法 9
2-2-2 奈米複合粉體的結構特性 9
2-2-3 無電鍍技術製備奈米粒子之研究 10
2-2-4 奈米碳管上沉積奈米粒子之研究 14
2-3 奈米碳管之特性與應用 16
2-3-1 奈米碳管之合成 16
2-3-2 奈米碳管之性質與結構 17
2-3-3 奈米碳管前處理之研究 20
2-3-4 奈米碳管之應用 23
2-4 奈米碳管去除重金屬及有機物之研究 25
2-4-1 奈米碳管吸附重金屬之研究 25
2-4-2 奈米碳管去除有機汙染物之研究 29
2-5 水體汙染物 32
2-5-1含鉛汙染危害性及去除方法 32
2-5-2含硒汙染危害性及去除方法 33
2-5-3偶氮染料之危害性及去除方法 34
第三章 實驗方法 36
3-1 實驗材料和藥品 36
3-2 實驗儀器設備 38
3-3實驗流程概述 40
3-4製備奈米複合材料Fe-Ni/CNT 41
3-5 TEM試片製作 44
3-6多壁奈米碳管性質分析儀器 45
3-6-1 掃描式電子顯微鏡分析(SEM/FE-SEM) 45
3-6-2 穿透式電子顯微鏡(TEM) 46
3-6-3 比表面積分析儀(BET) 47
3-6-4 熱重量分析儀(TGA) 47
3-6-5 傅立葉轉換紅外線光譜(FTIR) 48
3-6-6 反滴定法(Boehm`s titration method) 49
3-6-7 表面界達電位測定(Zeta Pontential) 49
3-6-8 拉曼磷光共軛雷射顯微光度計(Raman) 50
3-7複合奈米材料Fe-Ni/CNT性質分析儀器 51
3-7-1 化學成分鑑定(ICP-OES) 51
3-7-2 晶相測定 (XRD) 52
3-7-3分光光度計分析儀 53
3-8環境應用效益分析 53
3-9樣品分析之QA/QC 54
3-9-1 分光光度計分析 54
3-9-2 ICP重金屬離子分析 55
3-9-3 pH量測分析 55
第四章 結果與討論 56
4-1 奈米碳管改質前後特性分析 56
4-1-1 表面微觀結構分析 56
4-1-2 純度分析 58
4-1-3 拉曼繞射基分析 60
4-1-4 表面官能基分析 61
4-1-5 酸鹼反滴錠法分析 63
4-1-6 比表面積分析 63
4-1-7 界達電位分析 64
4-2 製備奈米複合材料Fe-Ni/CNT 65
4-2-1 製備參數對Fe-Ni/CNT之影響 65
4-2-2奈米Fe-Ni/CNT物性分析 76
4-3 環境應用測試 84
4-3-1 共處理混合汙染物(偶氮染料AO7及重金屬Pb2+、HSeO3-)測試 84
4-3-2 Fe-Ni/CNTs共處理水中汙染物後穩定性評估 89
4-4 綜合討論 93
第五章 結論與建議 94
參考文獻 96
附錄 109
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