等离子体活化接枝功能化CNTs及其环氧树脂纳米复合材料的研究
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摘要
本文以简单、经济、环保的碳纳米管(CNTs)功能化途径,制备出可在热固性树脂基体中均匀分散,与树脂界面相容好、界面粘结强度高的高度功能化的CNTs为目的,着重研究了热引发等离子体诱导接枝聚马来酸酐功能化CNTs,马来酸酐(MA)固相升华等离子体聚合功能化CNTs的工艺条件,聚马来酸酐功能化CNTs表面聚合物链端官能团的化学修饰和功能化CNTs/环氧树脂纳米复合材料的制备等。
本文采用氩等离子体处理CNTs,暴露于空气一段时间使其表面产生大量的羟基过氧化物和过氧化物,通过热引发,羟基过氧化物或过氧化物与带有活性基团的马来酸酐(MA)反应,实现CNTs的高度功能基化;接着采用胺类环氧树脂固化剂对功能化CNTs进行修饰,得到链端带有氨基的高度功能基化CNTs,将其与环氧树脂复合,制备出功能化CNTs/环氧树脂纳米复合材料。本文探讨了等离子体放电参数(如放电时间、放电功率、工作压力等)等离子体处理工艺参数对CNTs表面羟基过氧化物和过氧化物含量的影响,热引发温度、时间对接枝率的影响及CNTs的添加量对复合材料的热学和力学性能的影响;使用能谱分析仪(EDS)、描电子显微镜(SEM)、透射电子显微镜(TEM),红外光谱仪(IR)和热重分析仪(TGA)对相关产物的结构、组成、形貌进行了表征。动态力学分析仪(DMA)和材料万能试验机的测试结果表明,此功能化CNTs能显著提高环氧树脂基体的力学强度和耐热性能。
本文还发展了MA固相升华等离子体聚合功能化CNTs的研究,考察了放电功率、压力、时间和温度对酸酐基团保留和薄膜厚度的影响,并选择最佳MA等离子体聚合条件实现其对CNTs的功能化,并制备出MA等离子体聚合功能化的CNTs/EP复合材料。借助SEM、XPS、IR及TGA等手段均证实了CNTs被高度功能化,其环氧复合材料SEM显示此功能化CNTs在环氧树脂中具有较好的分散性。
Highly functionalized carbon nanotubes (CNTs) with good dispersion, good interface compatibility and high interface bonding strength were prepared in a simple, economical and environment-friendly way.
Argon plasma treated CNTs were exposed in the air to form peroxides and hydroperoxides on the surface. Through thermal initiation, these peroxides and hydroperoxides reacted with maleic anhydride (MA) to functionalize CNTs. The functionalized CNTs were further modified with amino groups. The as-obtained functionalized CNTs then reacted with epoxy matrix to prepare the CNTs/Epoxy composites. The effect of the plasma discharge parameters (discharge time, plasma power, working pressure, plasma time etc.) on the content of the peroxides and hydroperoxides on the surface of CNTs was investigated, as well as the effect of thermal initiation temperature and time on the grafting ratio. In addition, thermal and mechanical properties of the CNT/Epoxy composites were evaluated in correlation to the content of CNTs. Structure, composition and morphology of the related products were characterized by Energy spectrometers (EDS), Scanning electron microscopy (SEM) , Transmission electron microscopy (TEM), X-ray photoelectron spectrometers (XPS), Thermogravimetric anylyzer (TGA)and Infrared spectrometer (IR). Dynamic mechanics analyses (DMA) and mechanical testing results show that the functionalized CNTs can significantly improve the mechanical strength and heat resistance of the epoxy matrix.
The technique of sublimation plasma polymerization of MA was also developed. The effect of the plasma discharge parameters on the anhydride group reservation and the thickness of the film were studied. The optimal plasma discharge parameters were selected to functionalize CNTs. SEM,XPS, IR, TGA and other methods all verified CNTs were highly functionalized, thus improve the CNTs’dispersion in the epoxy matrix.
本文采用氩等离子体处理CNTs,暴露于空气一段时间使其表面产生大量的羟基过氧化物和过氧化物,通过热引发,羟基过氧化物或过氧化物与带有活性基团的马来酸酐(MA)反应,实现CNTs的高度功能基化;接着采用胺类环氧树脂固化剂对功能化CNTs进行修饰,得到链端带有氨基的高度功能基化CNTs,将其与环氧树脂复合,制备出功能化CNTs/环氧树脂纳米复合材料。本文探讨了等离子体放电参数(如放电时间、放电功率、工作压力等)等离子体处理工艺参数对CNTs表面羟基过氧化物和过氧化物含量的影响,热引发温度、时间对接枝率的影响及CNTs的添加量对复合材料的热学和力学性能的影响;使用能谱分析仪(EDS)、描电子显微镜(SEM)、透射电子显微镜(TEM),红外光谱仪(IR)和热重分析仪(TGA)对相关产物的结构、组成、形貌进行了表征。动态力学分析仪(DMA)和材料万能试验机的测试结果表明,此功能化CNTs能显著提高环氧树脂基体的力学强度和耐热性能。
本文还发展了MA固相升华等离子体聚合功能化CNTs的研究,考察了放电功率、压力、时间和温度对酸酐基团保留和薄膜厚度的影响,并选择最佳MA等离子体聚合条件实现其对CNTs的功能化,并制备出MA等离子体聚合功能化的CNTs/EP复合材料。借助SEM、XPS、IR及TGA等手段均证实了CNTs被高度功能化,其环氧复合材料SEM显示此功能化CNTs在环氧树脂中具有较好的分散性。
Highly functionalized carbon nanotubes (CNTs) with good dispersion, good interface compatibility and high interface bonding strength were prepared in a simple, economical and environment-friendly way.
Argon plasma treated CNTs were exposed in the air to form peroxides and hydroperoxides on the surface. Through thermal initiation, these peroxides and hydroperoxides reacted with maleic anhydride (MA) to functionalize CNTs. The functionalized CNTs were further modified with amino groups. The as-obtained functionalized CNTs then reacted with epoxy matrix to prepare the CNTs/Epoxy composites. The effect of the plasma discharge parameters (discharge time, plasma power, working pressure, plasma time etc.) on the content of the peroxides and hydroperoxides on the surface of CNTs was investigated, as well as the effect of thermal initiation temperature and time on the grafting ratio. In addition, thermal and mechanical properties of the CNT/Epoxy composites were evaluated in correlation to the content of CNTs. Structure, composition and morphology of the related products were characterized by Energy spectrometers (EDS), Scanning electron microscopy (SEM) , Transmission electron microscopy (TEM), X-ray photoelectron spectrometers (XPS), Thermogravimetric anylyzer (TGA)and Infrared spectrometer (IR). Dynamic mechanics analyses (DMA) and mechanical testing results show that the functionalized CNTs can significantly improve the mechanical strength and heat resistance of the epoxy matrix.
The technique of sublimation plasma polymerization of MA was also developed. The effect of the plasma discharge parameters on the anhydride group reservation and the thickness of the film were studied. The optimal plasma discharge parameters were selected to functionalize CNTs. SEM,XPS, IR, TGA and other methods all verified CNTs were highly functionalized, thus improve the CNTs’dispersion in the epoxy matrix.
引文
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