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Preparation of electro conductive nano-composite from surface modified carbon nanotube and their application to sensing material

表面改性碳纳米管导电纳米复合材料的制备及其在传感材料中的应用

基本信息

批准号：
15360357
负责人：
TSUBOKAWA Norio
金额：
$ 8.9万
依托单位：
Niigata University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (B)
财政年份：
2003
资助国家：
日本
起止时间：
2003 至 2005
项目状态：
已结题

项目摘要

1.The grafting of polymers onto carbon nanotube (CNT) and vapor grown carbon fiver (VGCF) by ligand-exchange reaction of polymers containing ferrocene moieties with aromatic ring of these surfaces was successfully achieved in the presence of Al powder and AlCl_3 as catalyst. The percentage of grafting (wt% of grafted polymer to CNT) reached to 60.9%. It was also found that the percentage of poly(vinyl ferrocene-co-methyl methacrylate) grafting increased with increasing vinyl ferrocene content of the copolymer. The copolymer was also grafted onto VGCF and carbon micro coil surface by use of the ligand-exchange reaction.2.The introduction of carboxyl groups onto CNT and VGCF surface was successfully achieved by the ligand-exchange reaction of polycondensed aromatic rings of these surfaces with 1,1'-dicarboxyferrocene. The grafting of hydroxyl and amino group terminated polymers, such as poly(ethylene glycol) (PEG) and poly(ethylene adipate), onto CNT surface was achieved by direct conden … More sation of carboxyl groups of CNT and VGCF with terminal hydroxyl groups of these polymers in the presence of N,N'-dicyclohexylcarbodiimide.3.The introduction of peroxyester groups onto CNT by the trapping of radicals having peoxyester moieties which were formed by the thermal decomposition of Perhexa C in toluene at 70℃ for 10 h was examined. As a result, peroxyester groups were successfully introduced onto CNT surface. The amount of peroxy groups introduced onto CNT was determined to be 9.5 mmol/g by titration. It was found that the radical graft polymerization of vinyl monomers was successfully initiated by the peroxyester groups introduced onto the CNT surface at 100℃ to give the corresponding polymer-grafted CNT. The percentage of grafting of ptoly(methyl methacrylate) reached to 6.6%.4.Poly(vinyl ferrocene-co-methyl methacrylate)-grafted CNT gave a stable dispersion in good solvent for grafted polymer, such as THF. The precipitation of the polymer-grafted CNT was scarcely observed even after 4 weeks. In addition, polymer-grafted VGCF and CNT readily and uniformly dispersed in grafted polymers to give nano-composites.It was found that electric resistance of the composites prepared from PEG-grafted VGCF and CNT drastically increased at melting point of PEG, 50℃. Therefore, the composites from PEG-grafted VGCF and CNT show positive temperature coefficient (PTC) characteristic.The electric resistance of the composites prepared from polymer-grafted VGCF and CNT suddenly increased in organic solvent vapor, such as methanol, THF, and toluene, and returns immediately to initial resistance when the composite was transferred in dry air. The responsiveness of electric resistance was reproducible even after 20 cycles of exposure to methanol vapor and dry air. Less

1.在Al粉和AlCl_3催化剂的作用下，通过二茂铁聚合物与碳纳米管（CNT）和气相生长碳五（VGCF）表面芳香环的配体交换反应，成功地实现了聚合物的接枝。接枝率（接枝到碳纳米管的wt%）达到60.9%。随着乙烯基二茂铁含量的增加，聚乙烯基二茂铁-共甲基丙烯酸甲酯接枝率也随之增加。利用配体交换反应将共聚物接枝到VGCF和碳微线圈表面。通过碳纳米管和VGCF表面的聚缩合芳香环与1,1'-二羰基二茂铁的配体交换反应，成功地将羧基引入到碳纳米管和VGCF表面。在N，N'-双环己基碳二酰亚胺的存在下，碳纳米管和VGCF的羧基与末端羟基的络合可以实现羟基和氨基端端聚合物（如聚乙二醇（PEG）和聚己二酸乙烯）的接枝。研究了过氧酯C在甲苯中70℃热分解10 h形成的过氧酯基团被捕获到碳纳米管上的过程。结果，过氧酯基团被成功地引入到碳纳米管表面。通过滴定法测定碳纳米管上引入过氧基团的量为9.5 mmol/g。结果表明，在100℃的温度下，在碳纳米管表面引入过氧酯基团，成功地引发了乙烯基单体的自由基接枝聚合，得到了相应的聚合物接枝碳纳米管。聚甲基丙烯酸甲酯接枝率达6.6%。聚乙烯基二茂铁-共甲基丙烯酸甲酯接枝碳纳米管在接枝聚合物（如THF）的良好溶剂中具有稳定的分散性。即使在4周后，聚合物接枝碳纳米管的沉淀也几乎没有观察到。此外，聚合物接枝的VGCF和碳纳米管易于均匀地分散在接枝聚合物中，从而形成纳米复合材料。结果表明，在PEG熔点为50℃时，接枝VGCF和碳纳米管制备的复合材料的电阻显著提高。因此，聚乙二醇接枝的VGCF和碳纳米管复合材料表现出正的温度系数（PTC）特性。由聚合物接枝的VGCF和碳纳米管制备的复合材料的电阻在有机溶剂蒸气（如甲醇、四氢呋喃和甲苯）中突然增加，当复合材料在干燥空气中转移时立即恢复到初始电阻。即使在甲醇蒸气和干燥空气中暴露20个循环后，电阻的响应性仍可重现。少