© 2015.A methylnadic anhydride-cured diglycidylether of bisphenol A, is prepared and characterised and a mono-epoxy POSS reagent added (0.5-4wt-%) to produce a series of nanocomposites. Two reaction mechanisms are observed involving esterification at lower temperatures (60-180°C) and etherification at temperatures above 180°C. Using the Ozawa and Kissinger methods, the activation energy for the first reaction was found to be 87-90kJ/mol and 122-124kJ/mol for the second reaction. Incorporation of POSS into the epoxy-anhydride network increases the Tg and cross-link density, indicating a more rigid network, but the values do not follow a trend based solely on POSS content. The char yield increases with POSS content with very little change in the degradation temperature. Incorporation of POSS (1wt-%) can reduce the moisture uptake in the cured resin by ~25% at 75% relative humidity. This is accompanied by a lower impact on glass transition temperature: the Tg is reduced by 10K at saturation, compared with 31K for the unmodified epoxy.
We report a method for the growth of carbon nanotubes on carbon fibre using a low temperature growth technique which is infused using a standard industrial process, to create a fuzzy fibre composite with enhanced electrical characteristics. Conductivity tests reveal improvements of 510% in the out-of-plane and 330% in the in-plane direction for the nanocomposite compared to the reference composite. Further analysis of current-voltage (I-V) curves confirm a transformation in the electron transport mechanism from charge - hopping in the conventional material, to an Ohmic diffusive mechanism for the carbon nanotube modified composite. Single fibre tensile tests reveal a tensile performance decrease of only 9.7% after subjecting it to our low temperature carbon nanotube growth process, which is significantly smaller than previous reports. Our low-temperature growth process uses substrate water-cooling to maintain the bulk of the fibre material at lower temperatures, whilst the catalyst on the surface of the carbon fibre is at optimally higher temperatures required for carbon nanotube growth. The process is large-area production compatible with bulk-manufacturing of carbon fibre polymer composites. © 2014 Elsevier Ltd. All rights reserved.
We report prediction of selected physical properties (e.g. glass transition temperature, moduli and thermal degradation temperature) using molecular dynamics simulations for a difunctional epoxy monomer (the diglycidyl ether of bisphenol A) when cured with p-3,30 -dimethylcyclohexylamine to form a dielectric polymer suitable for microelectronic applications. Plots of density versus temperature show decreases in density within the same temperature range as experimental values for the thermal degradation and other thermal events determined using e.g. dynamic mechanical thermal analysis. Empirical characterisation data for a commercial example of the same polymer are presented to validate the network constructed. Extremely close agreement with empirical data is obtained: the simulated value for the glass transition temperature for the 60 C cured epoxy resin (simulated conversion a = 0.70; experimentally determined a = 0.67 using Raman spectroscopy) is ca. 70–85 C, in line with the experimental temperature range of 60–105 C (peak maximum 85 C). The simulation is also able to mimic the change in processing temperature: the simulated value for the glass transition temperature for the 130 C cured epoxy resin (simulated a = 0.81; experimentally determined a = 0.73 using Raman and a = 0.85 using DSC) is ca. 105–130 C, in line with the experimental temperature range of 110–155 C (peak maximum 128 C). This offers the possibility of optimising the processing parameters in silico to achieve the best final properties, reducing labour- and material-intensive empirical testing.