磁场诱导环氧树脂/纳米石墨微片有序复合材料及其各向异性研究
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摘要
纳米石墨微片是一种新型的碳纳米填料。它的平均厚度约为50纳米,径向尺寸0.5-20微米,具有巨大的径厚比,保持了天然石墨良好的导电性及导电各向异性。由于纳米石墨微片具有特有的片层结构及突出的导电各向异性,当其在聚合物中有序排列后,结构上的有序化使复合材料表现出来的相关性能在不同方向上也会有所差异。目前设计制备具有有序化结构的高分子复合材料已成为聚合物基功能复合材料的发展方向之一。本文首次利用磁场对填充在环氧树脂中的纳米石墨微片进行定方向诱导排列,实现了纳米石墨微片与环氧树脂的有序化复合。与机械力诱导相比,纳米石墨微片在基体中的有序程度更高,方向可调性更好,材料具有更加广阔的设计空间。
论文主要研究内容为通过外加磁场对填充在环氧树脂中的经过磁改性后的纳米石墨微片进行诱导,使其在基体中定方向取向排列,得到环氧树脂/纳米石墨微片结构有序复合材料,并在此基础上对复合材料表现出来的性能各向异性进行了分析表征。
首先采用湿化学共沉淀法,以Fe2+和Fe3+的混合溶液为覆层前驱液,滴加氢氧化钠,使生成的四氧化三铁纳米粒子沉积在纳米石墨微片表面,采用XRD,SEM对产品进行表征。结果表明在大气气氛中,将反应温度控制在30℃,铁盐摩尔比n(Fe2+)/n(Fe3+)=5:1的条件下,在纳米石墨微片表面均匀沉积了一层物相组成单一的α-Fe3O4纳米粒子,改性后的纳米石墨微片表现出良好的软磁特性。
在对纳米石墨微片进行磁改性后,将其均匀分散在环氧树脂预聚物中,在体系固化前对其施加磁场。改性后的纳米石墨微片在磁场作用下,在树脂基体中沿石墨002面平行磁场的方向取向排列形成有序结构。通过单方向取向,得到一维有序复合材料;通过双方向取向得到二维有序复合材料。采用XRD与AFM对材料的有序结构进行了表征。纳米石墨微片单方向取向后,一维有序复合薄膜在可见光区的透光性明显增强,复合材料在垂直于纳米石墨微片取向方向上的拉伸强度明显提高。在二维有序复合材料中,磁性纳米石墨微片相互之间平行排列,材料表现出电磁屏蔽各向异性。
Graphite nanosheets (GNs), a new carbon nanofiller, 50 nm in thickness and 0.5-20 micrometer in diameter averagely, possess a high aspect ratio of diameter to thickness and much better in-plane conductivity compared to that in c-direction. It is understandable that the alignment of GNs in polymer will result in the composite with anisotropic properties, due to the anisotropy of GNs. In this study, for the first time, GNs have been aligned in an epoxy resin through the inducement of magnetic field. Compared with the shear-force inducement, by this method, the composites have a much higher degree of alignment which can be adjusted much easily.
Herein, we have investigated the alignment of magnetically modified GNs in epoxy resin by subjecting the mixture to an external constant magnetic field before the system cured to form epoxy resin/GNs highly ordered composites, and special attentions were paid on their anisotropic properties.
GNs obtained from sonicating the expanded graphite were modified chemically by depositing magnetite nanoparticles onto their surface through wet-chemical coprecipitation of ferric and ferrous ions with sodium hydroxide in the absence of nitrogen protection and surfactant, and were characterized using XRD and SEM. It was found that excellent magnetite-coated GNs can be obtained at 30 oC with 5:1 molar ratio of Fe2+ to Fe3+ in the air. The coated GNs are electrically conducting and ferromagnetic at room temperature.
The modified GNs were dispersed in epoxy prepolymer, and then subjected to a magnetic field before the suspension solidified. Modified GNs were aligned with their 002 planes parallel to the field direction in epoxy matrix forming an ordered structure. We have successfully obtained 1-dimensionally ordered composite through single-directional inducement and 2-dimensionally ordered composite by double-directional inducement which were confirmed by XRD and AFM measurements. The 1-dimensional orientation of GNs brought about an improvement in transmittance of composite films in the visible light region of 400-750 nm in wavelength and an remarkable enhancement in the tensile strength in direction perpendicular to the magnetic filed. The two-dimensionally ordered composites with modified GNs being induced to align with layers parallel to each other display interesting anisotropic electromagnetic interference fielding shielding properties.
论文主要研究内容为通过外加磁场对填充在环氧树脂中的经过磁改性后的纳米石墨微片进行诱导,使其在基体中定方向取向排列,得到环氧树脂/纳米石墨微片结构有序复合材料,并在此基础上对复合材料表现出来的性能各向异性进行了分析表征。
首先采用湿化学共沉淀法,以Fe2+和Fe3+的混合溶液为覆层前驱液,滴加氢氧化钠,使生成的四氧化三铁纳米粒子沉积在纳米石墨微片表面,采用XRD,SEM对产品进行表征。结果表明在大气气氛中,将反应温度控制在30℃,铁盐摩尔比n(Fe2+)/n(Fe3+)=5:1的条件下,在纳米石墨微片表面均匀沉积了一层物相组成单一的α-Fe3O4纳米粒子,改性后的纳米石墨微片表现出良好的软磁特性。
在对纳米石墨微片进行磁改性后,将其均匀分散在环氧树脂预聚物中,在体系固化前对其施加磁场。改性后的纳米石墨微片在磁场作用下,在树脂基体中沿石墨002面平行磁场的方向取向排列形成有序结构。通过单方向取向,得到一维有序复合材料;通过双方向取向得到二维有序复合材料。采用XRD与AFM对材料的有序结构进行了表征。纳米石墨微片单方向取向后,一维有序复合薄膜在可见光区的透光性明显增强,复合材料在垂直于纳米石墨微片取向方向上的拉伸强度明显提高。在二维有序复合材料中,磁性纳米石墨微片相互之间平行排列,材料表现出电磁屏蔽各向异性。
Graphite nanosheets (GNs), a new carbon nanofiller, 50 nm in thickness and 0.5-20 micrometer in diameter averagely, possess a high aspect ratio of diameter to thickness and much better in-plane conductivity compared to that in c-direction. It is understandable that the alignment of GNs in polymer will result in the composite with anisotropic properties, due to the anisotropy of GNs. In this study, for the first time, GNs have been aligned in an epoxy resin through the inducement of magnetic field. Compared with the shear-force inducement, by this method, the composites have a much higher degree of alignment which can be adjusted much easily.
Herein, we have investigated the alignment of magnetically modified GNs in epoxy resin by subjecting the mixture to an external constant magnetic field before the system cured to form epoxy resin/GNs highly ordered composites, and special attentions were paid on their anisotropic properties.
GNs obtained from sonicating the expanded graphite were modified chemically by depositing magnetite nanoparticles onto their surface through wet-chemical coprecipitation of ferric and ferrous ions with sodium hydroxide in the absence of nitrogen protection and surfactant, and were characterized using XRD and SEM. It was found that excellent magnetite-coated GNs can be obtained at 30 oC with 5:1 molar ratio of Fe2+ to Fe3+ in the air. The coated GNs are electrically conducting and ferromagnetic at room temperature.
The modified GNs were dispersed in epoxy prepolymer, and then subjected to a magnetic field before the suspension solidified. Modified GNs were aligned with their 002 planes parallel to the field direction in epoxy matrix forming an ordered structure. We have successfully obtained 1-dimensionally ordered composite through single-directional inducement and 2-dimensionally ordered composite by double-directional inducement which were confirmed by XRD and AFM measurements. The 1-dimensional orientation of GNs brought about an improvement in transmittance of composite films in the visible light region of 400-750 nm in wavelength and an remarkable enhancement in the tensile strength in direction perpendicular to the magnetic filed. The two-dimensionally ordered composites with modified GNs being induced to align with layers parallel to each other display interesting anisotropic electromagnetic interference fielding shielding properties.
引文
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