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In this work was investigated the effect of the addition of barium titanate (BaTiO3) on electrical properties of two chemically recyclable thermosets, polyhemiaminal (PHA) and polyhexahydro‐s‐triazine (PHT), both fabricated from 4,4′‐oxydianiline (ODA), an ether derivative of aniline and paraformaldehyde. Thermal and mechanical properties as well as chemical recyclability of the two polymers and their nanocomposites/nanodielectrics were also investigated. In addition, a quantitative analysis was conducted of the nanoparticle dispersion in the PHA‐/PHT‐based BaTiO3‐containing nanocomposites using transmission electron microscopy imaging and the nearest‐neighbor distance index and this index was used to analyze the investigated properties in connection with the proper mechanisms. Regarding the electrical properties for both neat polymers, conductivity values of the order of 10−8 S m−1 at 100 Hz were observed and dielectric constant values close to 2.80 for both polymers at 1 kHz. The addition of 0.5 wt% of BaTiO3 ferroelectric nanoparticles increased by about 44% the dielectric constant (1 kHz) and conductivity (102 Hz) of the PHA‐based nanocomposite. PHA and PHT exhibited glass transition temperature (Tg) values in the range 125–180 °C. An increase of 7 °C in Tg was observed after the incorporation of 0.5 wt% of BaTiO3 into PHA. Concerning the mechanical properties, values in the range 4.00–4.45 GPa for reduced modulus and 0.30–0.43 GPa for nanohardness for PHA and PHT polymers were observed. Independently of filler content or polymer matrix, both mechanical properties were enhanced after the addition of BaTiO3. The chemical recycling of PHA/PHT and all nanocomposites in the initial ODA reagent after sulfuric acid treatment was successfully characterized using the NMR and Fourier transform infrared spectroscopic techniques. © 2018 Society of Chemical Industry

The effects of the silanization of multi-walled carbon nanotubes and graphene nanoplatelets with 3-APTES on thermal, mechanical and electrical properties of epoxy nanocomposites were investigated. Nanocomposites containing pristine, oxidized and silanized nanoparticles of multi-walled carbon nanotubes or graphene nanoplatelets at two different concentrations (0.15 and 0.50 vol.%) were prepared by in situ polymerization without using solvents. The functionalized nanoparticles were characterized by Fourier-transform infrared, X-ray photoelectron spectroscopy, Raman spectroscopy and transmission electron microscope techniques. The oxidation and the silanization on the surface of both nanoparticles were confirmed by Fourier-transform infrared, X-ray photoelectron spectroscopy, Raman and transmission electron microscope analysis. The thermal properties of all studied materials were analyzed by differential scanning calorimetry and the mechanical properties by nanoindentation. The addition of both nanoparticles (pristine and functionalized) into the matrix did not show significant variations on thermal properties, but decreased values for glass transition temperature (Tg) compared to the neat resin. Higher values for modulus of elasticity and hardness of epoxy/nanocomposites were obtained when silanized multi-walled carbon nanotubes or oxidized graphene nanoplatelets were added into the matrix. Adding 0.15 vol.% of silanized multi-walled carbon nanotubes the modulus of elasticity increased in approximately 60%, whereas 0.50 vol.% this increase was greater than 90% compared to the neat resin. While adding 0.15 vol.% of oxidized graphene nanoplatelets, the modulus of elasticity increased approximately 83%, whereas 0.50 vol.% this increase was greater than 88% compared to the neat resin. The formation of percolating networks has been achieved only by pristine multi-walled carbon nanotubes addition at a concentration of 0.50 vol.% and by silanized graphene nanoplatelets at a concentration of 0.15 vol.%. However, for both carbon-based nanoparticles conductivities on the order of 10−7 S/m for frequencies near 100 Hz were observed.

In this work, multiwalled carbon nanotubes (MWCNT) were oxidized in a mixture of sulfuric and nitric acid (3:1 v/v) using two distinct times (9 and 18 hours). The effects of different oxidation levels and concentrations of MWCNT on curing kinetics, thermal, and mechanical properties of bisphenol A diglycidyl ether nanocomposites were studied. The nanocomposites were produced using in situ polymerization technique at two different volume fractions (0.15% and 0.50% v/v) without using solvents. X-ray photoelectron spectroscopy results indicated that MWCNT were in fact oxidized and just 9 hours of acid treatment showed a greater amount of oxygen on the MWCNT surfaces. Results of differential scanning calorimetry and dynamic mechanical analysis showed small variations in the glass transition temperatures of the nanocomposites, indicating alterations in the quality of the interphase matrix/ carbon nanotubes. Concerning the thermogravimetric analysis results, the most thermally stable samples were those containing 0.15% v/v of pristine and 18 hours of oxidized MWCNT, which also had the highest stiffness of all nanocomposites. Finally, the cure kinetics of nanocomposites is fairly represented by Kamal and Sourour's semiempirical model with an autocatalytic behavior at 100 C and 120 C, but decelerated at 140 C.

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