RESUMEN
Carbon nanotubes (CNTs), functionalized by a cycloaddition reaction, were studied by ultrahigh vacuum scanning tunneling microscopy (STM). The STM images provided evidence for partial or total unzipping of the outer CNT layer. The formation of graphene ribbons was triggered by the STM tip, under specific operating conditions. A model for the unzipping is proposed, based on the perturbation of the pi-conjugation along the CNT surface induced by the cycloaddition reaction.
Asunto(s)
Cristalización/métodos , Microscopía de Túnel de Rastreo/métodos , Nanotecnología/métodos , Nanotubos de Carbono/química , Nanotubos de Carbono/ultraestructura , Sustancias Macromoleculares/química , Ensayo de Materiales , Conformación Molecular , Tamaño de la Partícula , Propiedades de SuperficieRESUMEN
Carbon nanofibres were functionalized by a Diels-Alder cycloaddition reaction of 1,3-butadiene, generated in situ from sulfolene. The experimental conditions were selected on the basis of a differential scanning calorimetry (DSC) study on the reagents and the functionalization was confirmed by thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Analysis performed on the surface of the functionalized material by X-ray photoelectron spectroscopy (XPS) and FT-IR using the Attenuated Total Reflectance (ATR) technique indicates that the carbonyl and sulfoxide groups are present on the surface of the functionalized material. The acidic surface of the functionalized nanofiber suggests the presence of carboxylic acid and possibly sulfonic acid groups.
RESUMEN
The present work reports the solvent-free, one-pot functionalization of multiwall carbon nanotubes (CNTs) based on the 1,3-dipolar cycloaddition of azomethine ylides using N-benzyloxycarbonyl glycine and formaldehyde. The surface morphology of the functionalized CNTs was investigated by scanning tunneling microscopy. The effect of temperature on the reaction was studied by thermogravimetry and X-ray photoelectron spectroscopy (XPS). XPS was a key technique for the detailed chemical analysis of the CNT surface. The formation of two major reaction products was observed, namely a cyclic benzyl carbamate and a pyrrolidine. The concentration of the two products varied with reaction temperature and time. At 180 °C, the main product was the cyclic benzyl carbamate, while at 250 °C the major product was the pyrrolidine. This simple, solvent-free chemical procedure yields CNTs with fine-tuned surface functionality.