Characterization of the state of dispersion of carbon nanotubes in polymer nanocomposites

A practical overview of possibilities and limits to characterize the state of dispersion of carbon nanotubes (CNT) in polymer based nanocomposites is given. The most important and widely available methods are discussed with practical employment in mind. One focus is the quantitative characterization of the state of dispersion in solid samples using microscopy techniques such as optical microscopy or transmission electron microscopy. For dispersions of CNTs in aqueous media, solvents or monomers a sedimentation analysis is presented. This way dispersability and dispersion state of CNTs can be assessed. Indirect methods such as electrical conductivity measurements and rheological tests, dynamic differential scanning calorimetry and mechanical test are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Dispersion of carbon nanotubes in polyamide 6 for microinjection moulding

The focus of this study was to investigate the dispersion state of pure and functionalized carbon nanotubes in polyamide 6, on composites prepared by twin-screw extrusion and then processed by microinjection moulding. Nanocomposites were prepared with different carbonvnanotube compositions, with and without functionalization. The nanotubes were functionalized by the 1,3-dipolar cycloaddition reaction. The dispersion of the carbon nanotube agglomerates was quantified using optical microscopy and image analysis. The effect of functionalization on the polyamide 6/carbon nanotube interface, the nanocomposite morphology and the mechanical and electrical properties were studied. It was observed that the microinjected composites with functionalized carbon nanotubes presented improved dispersion, with smaller carbon nanotube agglomerate area ratio compared to the composites with pure nanotubes. The functionalized nanotubes showed better adhesion to polyamide 6 compared to pure nanotubes, as observed by scanning electron microscopy. The incorporation of carbon nanotubes considerably improved the mechanical properties. The effect of high polymer shear rate on carbon nanotube alignment during microinjection moulding was assessed by comparing the electrical resistivity of the composite after extrusion and after microinjection moulding, through the thickness and along the flow direction. The experiments showed that the mould design and processing conditions significantly affected electrical resistivity.Fundação para a Ciência e Tecnologia (project PEst-C/CTM/LA0025/2013

Probing dispersion and re-agglomeration phenomena upon melt-mixing of polymer-functionalized graphite nanoplates

A one-step melt-mixing method is proposed to study dispersion and re-agglomeration phenomena of the as-received and functionalized graphite nanoplates in polypropylene melts. Graphite nanoplates were chemically modified via 1,3-dipolar cycloaddition of an azomethine ylide and then grafted with polypropylene-graft-maleic anhydride. The effect of surface functionalization on the dispersion kinetics, nanoparticle re-agglomeration and interface bonding with the polymer is investigated. Nanocomposites with 2 or 10 wt% of as-received and functionalized graphite nanoplates were prepared in a small-scale prototype mixer coupled to a capillary rheometer. Samples were collected along the flow axis and characterized by optical microscopy, scanning electron microscopy and electrical conductivity measurements. The as-received graphite nanoplates tend to re-agglomerate upon stress relaxation of the polymer melt. The covalent attachment of a polymer to the nanoparticle surface enhances the stability of dispersion, delaying the re-agglomeration. Surface modification also improves interfacial interactions and the resulting composites presented improved electrical conductivity.The authors acknowledge the financial support to Project Matepro Optimizing Materials and Processes, with reference NORTE-07-0124-FEDER-000037 by the Programa Operacional Regional do Norte (ON.2) and Portuguese Foundation for the Science and Technology (FCT) for PEst-C/CTM/LA0025/2013. EC acknowledges FCT for a PhD grant SFRH/BD/87214/2012