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 search for graphene or few-layer graphene production methods that are simple, allow mass production, and yield good quality material continues to provoke intense investigation. The present work contributes to this investigation through the study of the aqueous exfoliation of four types of graphene sources, which are namely graphite and graphite nanoflakes with different morphologies and geographical origins. The exfoliation was achieved in an aqueous solution of a soluble pyrene derivative that was synthesized to achieve maximum interaction with the graphene surface at low concentration (5 × 10−5 M). The yield of bilayer and few-layer graphene obtained was quantified by Raman spectroscopic analysis, and the adsorption of the pyrene derivative on the graphene surface was studied by thermogravimetric analysis and X-ray diffraction. The whole procedure was rationalized with the help of molecular modeling.
Carboxylic acid-terminated pyrrolidine functionalities were covalently bonded to the surface of graphene nanoplatelets via a solvent-free approach and characterized by Boehm titration.
Graphene and its derivatives are promising as reinforcement for polymer nanocomposites. Additionally to their inherent outstanding mechanical properties, these nanoparticles may be functionalized to enhance their compatibility with the polymeric matrix and provide specific chemical and physical properties. In this work, new freestanding films (FS) based on chitosan (CHI), alginate (ALG) and functionalized graphene were developed using the layer-by-layer assembly. Suspensions of functionalized graphene nanoflakes (f-GF) and nanoribbons (f-GNR) were prepared from expanded graphite (EG) and multiwalled carbon nanotubes (MWNTs), respectively. The graphene nanoflakes and MWNTs were covalently functionalized using a 1,3-dipolar cycloaddition reaction that allowed the nanoparticles exfoliation. f-GNR and f-GF suspensions were characterized to demonstrate that graphene nanoflakes and MWNTs were successfully functionalized and exfoliated. Then, the layer-by-layer deposition of CHI, ALG and both types of functionalized graphene was investigated and FS films were produced. The morphology, thermal and mechanical characteristics of the produced FS films were assessed. Their degradation and swelling profiles as well as their biological behavior were evaluated. The incorporation of f-GF resulted in smoother films while the incorporation of f-GNR resulted in rougher films. When compared with the CHI/ALG bi-component films. Both graphene containing films remained hydrophobic. The graphene incorporation in the multilayered FS was estimated to be 1.7 wt% for f-GF and 2.5 wt% for f-GNR. The presence of functionalized graphene did not affect the thermal stability of the films, it increased the storage modulus and the dynamic mechanical response at 1 Hz and 37 C, and decreased the electrical resistivity. The biological assays revealed cytocompatibility towards L929 cells when both f-GF and f-GNR were incorporated in the CHI/ALG matrix. In conclusion, these new f-GF and f-GNR reinforced FS films present great potential for use in biomedical applications such as films for wound healing or cardiac and bone engineering.
Silane-functionalized graphene nanoplatelets (GNPs) were prepared using a newly developed approach based upon a simple two-step strategy. The effect of their dispersion and interfacial bonding on the mechanical properties and thermal conductivity of reinforced silicone rubber (SR) was investigated. It was found by Raman mapping that the silane-functionalized GNPs could be dispersed uniformly into the SR matrix, leading to an increase of up to 25% in Young’s modulus at only 2 parts per hundred rubber (phr) loading and a considerable enhancement of up to 150% in the thermal conductivity at 5-phr loading. Both the Young’s modulus and thermal conductivity experimental results were found to be in agreement with the values predicted using theoretical models.
Graphical abstract
Graphene nanoplatelets (GNPs) were functionalized through 1,3-dipolar cycloaddition of azomethine ylide using a solvent-free approach and under different reaction conditions. The yield and the functionality of the carboxyl-terminated pyrrolidine ring attached on the surface of GNPs could be affected by varying the reaction temperature as well as the reactant to GNP weight ratio. The functionalized GNPs were characterized extensively using a range of spectroscopic and microscopy techniques.
In this study, composite scaffolds based on poly(caprolactone) (PCL) and non‐covalently functionalized few‐layer graphene (FLG) were manufactured by an extrusion‐based system for the first time. For that, functionalized FLG powder was obtained through the evaporation of a functionalized FLG aqueous suspension prepared from a graphite precursor. Cryomilling was shown to be an efficient mixing method, producing a homogeneous dispersion of FLG particles onto the PCL polymeric matrix. Thereafter, fused deposition modeling (FDM) was used to print 3D scaffolds and their morphology, thermal, biodegradability, mechanical, and cytotoxicity properties were analysed. The presence of functionalized FLG demonstrated to induce slight changes in the microstructure of the scaffold, did not affect the thermal stability and enhanced significantly the compressive modulus. The composite scaffolds presented a porosity of around 40% and a mean pore size in the range of 300 μm. The cell viability and proliferation of SaOs‐2 cells were assessed and the results showed good cell viability and long‐term proliferation onto produced composite scaffolds. Therefore, these new FLG/PCL scaffolds comprised adequate morphological, thermal, mechanical, and biological properties to be used in bone tissue regeneration.
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