嫘縈系碳纖維吸附材鍍銀加工及其物化性質之研究｜國立臺灣科技大學博碩士論文系統

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研究生：	彭兆群 CHAO-CHUN PENG
論文名稱：	嫘縈系碳纖維吸附材鍍銀加工及其物化性質之研究 Study of Viscose Rayon Based Carbon Fiber Adsorbents Modified by Supporting Silver and Its Physical and Chemical Properties
指導教授：	蘇清淵 Ching-Iuan Su
口試委員:	王英靖 none 李貴琪 none 黃博雄 none 邱士軒 Shih-Hsuan Chiu 邱顯堂 Hsien-Tang Chiu
學位類別：	博士 Doctor
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2011
畢業學年度：	99
語文別：	中文
論文頁數：	178
中文關鍵詞：	嫘縈系碳纖維吸附材、抗菌、比表面積、含氧官能基
外文關鍵詞：	viscose rayon-based activated carbon fiber, antibacterial ability, BET specific surface area, oxygen function groups.
相關次數：	點閱：353 下載：3
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本研究的目的在製備出具有抗菌能力的碳纖維吸附材。實驗中以嫘縈（Viscose Rayon）針織物為前驅體（Precursor），以硫酸銨和磷酸氫二銨(混合比 95/5，濃度為30%之水溶液)複合式耐燃劑之前處理後，經直立狀連續半開放式高溫爐，進行氧化、碳化及活化工程，並使用三種複合式氣體作為活化源：(1)水蒸氣＋氮氣(N2)、 (2)水蒸氣+空氣(N2/O2)與(3)水蒸氣+氮氫(N2/H2)混合氣，製備出各種不同孔洞特性的碳纖維吸附材，再分別應用物理及化學方式，進行鍍銀加工。物理方式即應用電漿及濺鍍銀原子於碳纖維吸附材上，而化學方式則是採用金屬鹽改質的方式，將銀離子在碳纖維吸附材上還原成金屬銀，以製備具有抗菌效果的碳纖維吸附材。而後分別探討鍍銀前後，金屬銀在碳纖維吸附材表面分佈、孔洞大小分佈、表面化學性質、微細結構及有機氣體吸附的影響。最後，評估碳纖維吸附材的抗菌能力以及銀離子的溶出情形。
實驗結果顯示，以水蒸氣與空氣混合之活化劑所製備出的碳纖維吸附材有較多的中孔，其BET比表面積(1713 m2/g)最高，對四氯化碳氣體具有最大的吸附量(100.5%)，而其結晶厚度較大，結構較緻密，具有較高的真密度值，且其含氧官能基的比例也最高。經過電漿及濺鍍銀加工，因受到蝕刻而破壞孔洞及銀顆粒沉積的影響，造成碳纖維吸附材比表面積下降。另經過銀離子還原鍍銀加工後，在官能基團中，羰基團的峰值會增加，醇類以及醚基的峰值也會增加。而等溫吸附曲線則低於未鍍銀加工，其比表面積與平均孔徑也相對較小，對於有機氣體吸附而言，吸附量隨銀含量增加而明顯下降。兩種方式鍍銀加工，皆可製備出具有良好的抗菌及抑菌效果的碳纖維吸附材。至於銀離子溶岀試驗，發現不同試樣在去離子水中靜置96小時後，溶出量均趨於緩和。而在靜置168小時後，試樣中最大溶出量僅為0.2855∼0.4294ppm。

This study concerns the preparation of activated carbon fiber (ACF) adsorbents with antibacterial ability. Viscose rayon-based knitted fabrics is used as the precursor and pre-treated by a composite flame retardant of ammonium sulfate ((NH4)2SO4) and ammonium phosphate dibasic ((NH4)2HPO4) mixed at a ratio 95:5. It then undergoes oxidation, carbonization and activation processes in a semi-open high-temperature erect furnace with three types of activating agents, namely (1) steam + N2, steam + air (N2/O2), and (3) steam +N2/H2, to produce ACF adsorbents with different pore characteristics. The ACF adsorbents were modified by supporting silver for physical and chemical method and ACF-Ag adsorbents were produced with antibacterial. It is applied etching and deposition of silver for physical methodis. It is followed by spraying and decomposition of silver regarding to chemical method. The effect of variation on the silver particle distribution of surface, distribution of pore size, surface chemical properties, microstructure and the absorption of volatile organic compounds (VOCs) of ACF and ACF-Ag adsorbents are investigated. In addition, the antibacterial ability and Ag+ elution of the ACF-Ag adsorbent are also measured.
Experimental results show that carbon fiber activated by steam and air has more mesopores and largest BET specific surface area (1713 m2/g) and the maximum absorption amounts (100.5%) of CCl4. In addition, the crystals thus formed are thicker and of a denser structure with relatively higher true density values. The ratio of the oxygen containing functional groups is also higher. However, the BET specific surface area of ACF-Ag adsorbents decreased because pores were destroyed by etching and deposition of silver particles. Among the functional groups of ACF-Ag by spraying and decomposition of silver, the peak value of the carbonyl function group will increase, and so will the peak value of alcohol and ether. ACF-Ag adsorbent have lower isotherm, less BET specific surface area and smaller mean pore diameter. The adsorption of volatile organic compounds by ACF-Ag adsorbent reduces significantly as a result of increased silver content. Different ACF-Ag adsorbent all show effective antibacterial and sterilizing properties. The elution of Ag+ from ACF-Ag adsorbent placed in deionized water for 96 hours decreases gradually. After 168 hours, the maximum Ag+ eluted is only 0.2855∼0.4294ppm ppm.

中文摘要.....................................................................................................I
英文摘要................................................................................................. III
誌謝..........................................................................................................Ⅴ
目錄........................................................................................................ Ⅵ
圖表索引..............................................................................................ⅩⅢ
第一章 緒言.............................................................................................1
1活性碳及碳纖維吸附材的發展…......................…..........................2
2活性碳及碳纖維吸附材的異同........................................................5
3碳纖維吸附材的用途...............................................................…….9
第二章 研究動機及目的................................................……….……..10
第三章 理論與文獻回顧.......................................................................12
1 碳纖維吸附材的製備.......................................................................12
1.1  原料.........................................................................................13
1.2  前處理工程.............................................................................14
1.3  氧化工程..................................................................................16
1.4  碳化工程…........................................................……….……19
1.5  活化工程.................................................................................21
1.5.1  化學活化法......................................................................21
1.5.2  物理活化法......................................................................22
2電漿加工..................................................................25
2.1  電漿的發展.....................................................25
2.2  電漿定義及分類.............................................26
2.3  電漿加工之原理.................................................28
2.4  電漿應用領域.................................................30
3 金屬鹽改質碳纖維吸附材..............................................................33
3.1  金屬鹽在碳纖維吸附材上的分佈..........................................34
3.2  金屬鹽在碳纖維吸附材上的聚集情形..................................35
3.3  活性碳對銀離子的吸附機理.................................................37
3.3.1  離子交換反應吸附..........................................................38
3.3.2  銀離子還原反應吸附......................................................38
4 碳纖維吸附材的吸附現象..............................................................41
4.1  物理吸附.................................................................................42
4.2  化學吸附.................................................................................43
4.3  細菌在活性碳上的吸附現象.................................................45
4.4  吸附機構.................................................................................45
5 吸附理論與孔洞分析.....................................................................48
5.1  吸附平衡.................................................................................48
5.2  等溫吸附曲線.........................................................................49
5.3  Langmuir等溫吸附................................................................54
5.4  BET等溫吸附.........................................................................57
5.5  BJH分析法.............................................................................59
5.6  t-plot分析法............................................................................64
6 真實密度測試..................................................................................66
7 抗菌理論..........................................................................................68
7.1  定義.........................................................................................68
7.2  抗菌劑與抗菌機制.................................................................70
第四章 實驗方法...................................................................................72
1實驗材料.........................................................................................72
2實驗藥劑.........................................................................................72
3實驗設備.........................................................................................73
4實驗氣體.........................................................................................76
5測試儀器.........................................................................................77
6實驗流程.........................................................................................78
7實驗方法.........................................................................................79
7.1  前處理工程.............................................................................79
7.2  氧化、碳化及活化工程.........................................................79
7.3  後處理工程.............................................................................81
7.4  碳纖維吸附材之電漿改質.....................................................83
7.5  金屬鹽改質碳纖維吸附材......................................................85
7.5.1  真空噴灑..........................................................................85
7.5.2  裂解反應(decomposition)................................................86
8碳纖維吸附材性質分析.....................................................................88
8.1  X射線繞射分析......................................................................88
8.2  X射線光電子分析..................................................................88
8.3  比表面積與及孔洞性質分析.................................................89
8.4  真實密度測試.........................................................................89
8.5  掃描式電子顯微鏡.................................................................90
8.6  有機氣體吸附.........................................................................90
8.7  抗菌試驗.................................................................................91
8.8  銀離子溶出試驗.....................................................................93
8.9  碳纖維吸附材水中之殘留物質測試......................................94
第五章 結果與討論...............................................................................95
1碳纖維吸附材在水中之殘留物質測試.................................95
1.1碳纖維吸附材pH值測試......................................95
1.2碳纖維吸附材在水中之離子殘留物測試..................................96
2活化源對碳纖維吸附材之影響........................................98
2.1活化源（水蒸氣）供給量對碳纖維吸附材之影響......................99
2.1.1氮氣等溫吸附...............................................99
2.1.2 ＢＥＴ比表面積...............................................101
2.1.3孔洞分析...............................................102
2.2不同活化源對碳纖維吸附材之影響...........................104
2.2.1氮氣等溫吸附............................................... 104
2.2.2 ＢＥＴ比表面積............................................................107
2.2.3孔洞分析.............................................................109
2.2.4微細構造分析...............................................114
2.2.5表面化學組成分析.............................................115
2.2.5.1表面元素含量變化......................................................117
2.2.5.2官能基分析..........................................................118
2.2.6真實密度分析.............................................121
3電漿及濺鍍銀加工對碳纖維吸附材之影響...............................122
3.1氮氣等溫吸附............................................................................122
3.2 ＢＥＴ比表面積.....................................................................124
3.3孔洞分析................................................................................126
3.4 ＳＥＭ微結構及表面形態觀察............................................130
3.5氣相吸附..............................................................135
3.6抗菌測試..............................................................137
3.6.1抗菌測試...............................................137
3.6.2銀離子溶出測試...............................................138
4金屬鹽改質碳纖維吸附材........................................... 139
4.1鍍銀對碳纖維吸附材性質之影響....................................139
4.1.1比表面積與孔洞性質分析............................................... 139
4.1.2表面形態觀察.................................................. 141
4.1.3微細構造分析...................................................... 142
4.1.4表面化學組成分析.................................................. 144
4.1.4.1表面元素含量變化......................................................144
4.1.4.2官能基分析..........................................................146
4.2裂解反應對ACF-Ag材料之影響.............................................147
4.2.1 比表面積與孔洞性質分析.............................................147
4.2.2表面形態觀察...............................................151
4.2.3表面化學組成分析.................................................. 154
4.2.3.1表面元素含量變化......................................................154
4.2.3.2官能基分析..........................................................157
4.2.4真實密度分析...............................................159
4.3有機氣體吸附...........................................................................161
4.4 抗菌性質..................................................................................163
4.4.1抗菌試驗.................................................. 163
4.4.2銀離子溶出試驗.................................................. 165
第六章 結論.........................................................................................166
參考文獻...............................................................................................171

                                

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