Abstract Percolation threshold is an important phenomenon to be addressed when producing nanocomposites, especially because the literature suggests a depression of properties near this region. In this study, epoxy matrix nanocomposites were produced with different volume fractions of multi-walled carbon nanotubes and were characterized according to their electrical, thermal, and mechanical properties. In addition, digital image correlation (DIC) was used to measure the strain of nanocomposites and to show how it behaves in different percolation states. Electrical conductivity indicated a percolation threshold near 0.22% v/v of nanoparticles. Differential scanning calorimetry analysis showed a depression followed by an increase in glass transition temperature near the percolation threshold. Tensile strength tests presented a depression followed by an increasing near percolation threshold. DIC images showed that nanocomposites present a different behavior when near the percolation threshold, with a more distributed strain over the surface of the sample under stress and fracture toughness decreased near the percolation threshold.

The dispersion of nanoparticles in nanocomposites of an epoxy matrix reinforced with alumina (10nm) and zinc oxide (100nm) is analyzed using FIB/FESEM images, varying the volumetric fraction of fillers from 0.2 % to 6.0 %. The nanofillers dispersion images were transformed to binary files and the multifractal spectrum was calculated. From these data the relation between agglomerate and individual particle dimensionalities related to the interphase percolation was investigated. Interphase percolation of nanocomposites should be achieved when the dimensionality of agglomerations is greater than the dimensionality of individual particles. The actual percolation state of the interphase is determined, matching the experimental nanocomposites behavior for electrical behavior at AC and dielectric breakdown at DC.

ABSTRACT In this paper, nanocomposites with multiwalled carbon nanotubes (MWCNT) or graphene nanosheets were prepared using a high density polyethylene (HDPE) matrix. Two different processes were employed: a solution method and a melt mixing method. The crystallinity index of the HDPE showed similar levels in nanocomposites after the addition of carbon nanotubes. It can be seen that the preparation process modified the degree of crystallinity of the HDPE matrix with graphene nanosheets. Nanocomposites prepared by the solution method showed a decrease in the crystallinity index. The addition of carbon nanotubes led to an increase of Young's Modulus with an increase in the MWCNT quantity, regardless of the preparation process used, with a 22.8 % increase for composites with 0.5 wt% of CNTs. The nanocomposites with graphene nanosheets exhibited a different behavior with each mixing method. Nanocomposites prepared by the solution method showed a higher Young's Modulus than those prepared by melt mixing. Results of transmission electronic microscopy and field emission scanning electronic microscopy indicated homogeneous dispersion for carbon nanotubes in melt mixing. Graphene nanocomposites showed some agglomerates, with smaller platelets in the nanocomposites prepared by solution mixing compared to that prepared by the melt mixing.

In this work, nanocomposites with simultaneous dispersion of carbon nanotubes and clays in a high density polyethylene (HDPE) matrix were prepared. Two different processes of preparation were employed: solution or melt intercalation. Two different montmorillonite clays were used separately: a natural (MMT-Na) or an organoclay (MMT-30B) and it was used multiwalled carbon nanotubes (MWCNT). Thermal properties were evaluated by DSC and TGA, mechanical properties were evaluated by nanoindentetion and morphology was investigated by transmission electronic microscopy (TEM). Alterations of 20% in crystallinity were detected, increases in Young´s modulus up to 12% were observed and up to 20% of increase was observed in Oliver-Pharr hardness. It is possible to explain part of those results based on the state of dispersion observed in our TEM results.

Neste trabalho são estudados os efeitos da adição de nanotubos de carbono de parede múltipla (NCPM) em uma matriz de Poli(L-ácido láctico) (PLLA). Foras avaliadas duas rotas distintas de dispersão dos NCPM, uma utilizando agitação mecânica em solvente e a outra utilizando sonificação de alta energia em solvente. As propriedades mecânicas destes nanocompósitos foram avaliadas utilizando nanoindentação e microdureza vickers. Através da calorimetria exploratória diferencial foram determinadas as propriedades térmicas dos nanocompósitos (Tg, Tc, Tm e cristalinidade) obtidas. Por último, as propriedades tribológicas foram determinadas através de ensaios de deslizamento do tipo pino sobre disco, onde foram utilizadas diferentes cargas normais. As propriedades mecânicas e térmicas não foram significativamente afetadas pela adição do nanotubos, o que não se repetiu nas propriedades tribológicas, onde tanto o método de dispersão quanto a concentração de NCPM afetaram as propriedades. A micrografia das trilhas de desgaste sugere ainda que o mecanismo atuante foi modificado com a incorporação dos nanotubos, o mesmo pode ter acontecido nas amostras sonificadas.

This work studied the effects of the addition of Multiwalled Carbon Nanotubes (MWCNT) to a PLLA matrix. Two distinct methods of preparation were employed: a combination of a solvent/ mechanical stirring and a combination of a solvent/high energy sonication. The mechanical properties of the nanocomposites were determined by nanoindentation and by the Vickers hardness test. Thermal properties of the nanocomposites (Tg, Tc, Tm and crystallinity degree) were determined by DSC. The tribological properties of the nanocomposites were determined by using a pin-on-disc apparatus. Mechanical and thermal properties did not present significant alterations, although tribological properties presented significant changes caused by the method of preparation and different loads. SEM images indicated that the wear mechanism was changed by the addition of MWCNT.

In this study, the thermal, dynamic-mechanical and tribological behavior of nanocomposites of a photocurable epoxy-acrylate resin and multiwalled carbon nanotubes (MWCNT) are investigated. A route consisting of a combination of sonication, mechanical and magnetic stirring is used to disperse 0.25-0.75 wt. (%) MWCNT into the resin. Two photocuring cycles using 12 hours and 24 hours of UV-A radiation are studied. The storage modulus, the loss modulus and the tan delta are obtained by dynamic mechanical analysis. Thermal stability is investigated by thermogravimetry, morphology by transmission electronic microscopy (TEM) and tribological performance using a pin-on-disk apparatus. The results indicate an increase in stiffness and higher ability to dissipate energy, as well as a shift in the glass transition temperature for the nanocomposites. The addition of nanofillers also decreased friction coefficient and wear rate of the nanocomposites but did not change the observed wear mechanisms.

Arc discharge is the most practical method for the synthesis of single wall carbon nanotubes (SWCNT). However, the production of SWCNT by this technique has low selectivity and yield, requiring further purification steps. This work is a study of purification of SWCNT by heat treatment in an inert atmosphere followed by supercritical fluid extraction. The raw arc discharge material was first heat-treated at 1250 °C under argon. The nanotubes were further submitted to an extraction process using supercritical CO2 as solvent. A surfactant (tributylphosphate, TBP) and a chelating agent (hexafluoroacetylacetone, HFA) were used together to eliminate metallic impurities from the remaining arc discharge catalysts. Analysis of Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) showed an efficient removal of iron and cobalt (>80%). The purified nanotubes were further analyzed by TGA and Raman spectroscopy.

In this study, carboxylated (SWCNT-c) and pristine (SWCNT) single-walled carbon nanotubes were randomly dispersed in a hardener prior to mixing it with an epoxy resin. The influence of several parameters on the dispersion process were investigated. The produced samples were characterized by infrared spectroscopy, differential scanning calorimetry, dilatometry, dynamic mechanical analysis, scanning electron microscopy and mechanical testing (tensile, flexural and microhardness). The results obtained with the nanocomposites with SWCNT-c suggested that the lowest time and amplitude of sonication improved the mechanical properties. The use of a solvent (acetone) was important to improve dispersion, ultimately increasing microhardness and Young's Modulus up to 32%. Nanocomposites with 0.25 wt. (%) SWCNT-c presented superior mechanical properties compared to those with 0.50 wt. (%) SWCNT. Two simple mathematical models (rule of mixtures and Halpin-Tsai) were used to predict Young's Modulus of the composites yielding results very close to the experimental ones.

In this work, nanocomposites were prepared by adding a small amount of single walled carbon nanotubes (SWCNTs) to an epoxy resin aiming to study the resulting mechanical, viscoelastic and thermal properties of the nanocomposites. To optimize the processing of the nanocomposites and to favor a homogeneous dispersion of the SWCNTs on the matrix, acetone was used to reduce resin viscosity, increasing diffusion of the SWCNTs in the solution. The epoxy/SWCNTs/acetone systems were also sonicated in order to minimize entanglement of the SWCNTs. The systems were characterized by Fourier transform infrared spectroscopy, Raman spectroscopy, thermogravimetry, differential scanning calorimetry and dynamic mechanical analysis. The results indicated that the addition of small amounts of SWCNTs to epoxy leads to slight structural changes in the epoxy matrix which, together with the presence of SWCNTs, may reflect on its mechanical and viscoelastic properties