Dehonor Mariamne, Masenelli-Varlot Karine, González-Montiel Alfonso, Gauthier Catherine, Cavaillé Jean-Yves, Terrones Mauricio
Advanced Materials Department, IPICYT, Camino a la Presa San José 2055, Col. Lomas 4a. Sección, San Luis Potosí 78216, México.
J Nanosci Nanotechnol. 2007 Oct;7(10):3450-7. doi: 10.1166/jnn.2007.817.
Polymer grafting of polystyrene (PS) on nitrogen-doped multiwall carbon nanotubes (CNx) was successfully obtained by a "grafting from" technique. The production method involves the immobilization of initiators, using wet chemistry, onto the nanotube surface, followed by an in situ surface-initiated polymerization. The polymer-grafting carbon nanotubes synthesis includes the free radical functionalization of CNx and the "controlled/living" Nitroxide Mediated Radical Polymerization (NMRP). The obtained products were studied using several microscopic techniques as scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and electron energy loss spectroscopy (EELS). The characterization also includes thermogravimetric analysis (TGA), Raman spectroscopy, infrared spectroscopy, and electron spin resonance (ESR), among others. The analyzed samples were also compared with solutions fabricated by physical blending of the polymer and CNx nanotubes. These results indicate that the nanotube radical functionalization, the chemical grafting, and the polymerization reaction were obtained over CNx when NMRP method was successfully used, giving rise to a uniform PS layer of several nanometers grafted on the outer surface of the CNx nanotubes. Several properties of the PS-grafted CNx nanotubes were also studied. It is shown that the production method leads to a narrower distribution of the external diameters. Moreover, their solubilization in organic solvents is greatly improved. Finally, the dispersion of PS-grafted CNx into a PS matrix is studied to determine the differences in filler dispersion and interfacial adhesion strength, in comparison with nanocomposites elaborated with as-produced CNx.
通过“接枝生长”技术成功实现了聚苯乙烯(PS)在氮掺杂多壁碳纳米管(CNx)上的聚合物接枝。该制备方法包括利用湿化学方法将引发剂固定在纳米管表面,随后进行原位表面引发聚合反应。聚合物接枝碳纳米管的合成包括CNx的自由基功能化以及“可控/活性”氮氧介导自由基聚合(NMRP)。使用多种显微技术对所得产物进行了研究,如扫描电子显微镜(SEM)、高分辨率透射电子显微镜(HRTEM)和电子能量损失谱(EELS)。表征还包括热重分析(TGA)、拉曼光谱、红外光谱以及电子自旋共振(ESR)等。还将分析的样品与通过聚合物和CNx纳米管物理共混制备的溶液进行了比较。这些结果表明,当成功使用NMRP方法时,在CNx上实现了纳米管自由基功能化、化学接枝和聚合反应,在CNx纳米管外表面形成了一层几纳米厚的均匀PS层。还研究了PS接枝CNx纳米管的几种性能。结果表明,该制备方法导致外径分布更窄。此外,它们在有机溶剂中的溶解性大大提高。最后,研究了PS接枝CNx在PS基体中的分散情况,以确定与用原始CNx制备的纳米复合材料相比,填料分散和界面粘合强度的差异。