ABSTRACT Lately, nanomaterials have been largely studied as reinforcements for epoxy resin. Although their usage is highly promising, the literature has reported some drawbacks regarding the improvement of mechanical properties in nanocomposites. These difficulties are usually due to dispersion of nanomaterials and its adhesion to the polymeric matrix. One approach to this problem is the functionalization of nanomaterials such as carbon nanotubes (CNTs) and graphene. In this work, we have studied the synthesis and functionalization process of CNTs and graphene oxide (GO) to be used as reinforcements for epoxy resin nanocomposites. CNTs were synthesized at 850 °C in a quartz furnace, from hexane and ferrocene vapor, and functionalized by acids and ethylenediamine treatments. GO was obtained by graphite exfoliation through a modified Hummer's method. The nanomaterials were characterized by Raman spectrum, FT-IR, XRD, and SEM images. Nanocomposites were prepared using these nanomaterials and evaluated by DMA. While both nanomaterials showed an improvement in mechanical properties, suggesting a chemical bond between nanomaterial and the epoxy matrix, it was clear that GO reinforced samples presented a higher storage modulus.

ABSTRACT: The focus of this study is to evaluate the effect of carboxyl and amino functionalization of multiwalled carbon nanotubes on the mechanical property of the epoxy resin filled with modified carbon nanotubes. The carbon nanotubes were treated with sulfuric and nitric acids and also with hexamethylenediamine. The presence of acid and amine chemical groups on the carbon nanotube surface was confirmed by X-ray photoelectron spectroscopy. The composites were produced with epoxy resin and modified carbon nanotubes. Vickers hardness tests were carried out on the composites and neat resin. The results showed an increase of hardness in the composite prepared with functionalized carbon nanotubes. This phenomenon is due to the fact that the chemical interaction between modified carbon nanotube and epoxy resin is much stronger than between pristine carbon nanotube and epoxy resin. This stronger interaction is related to the presence of functionalized carbon nanotubes.

ABSTRACT: Mullite is an excellent structural material due to its high temperature stability, high electrical insulation capabilities and creep resistance. This material has a number of technological applications, such as rocket nozzles used in the aerospace industry. In this work, mullite was obtained by sol-gel process, using silicic sol, aluminum nitrate and ethylene glycol, besides the following volume ratios of silica sol dispersion to ethylene glycol: 1/0; 1/1; 1/2; and 1/3. After drying, the samples were thermal treated at temperatures of 1,000; 1,100; 1,200 and 1,250°C. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and specific surface area (Bruner-Emmett-Teller - BET). SEM showed that mullite particles are fine and nearly equiaxed. The sample without ethylene glycol showed 3/2 mullite after heat treatment at 1,250°C. The sample with intermediate ethylene glycol concentration presented two crystallization processes: the first at 1,000°C forming mullite and spinel phases, and the second at 1,250°C forming only 3/2 mullite. However, the sample with the highest ethylene glycol concentration crystallized directly to mullite at 1,000°C with the highest yield. There is a strong dependence on the specific surface area with temperature. The Rietveld refinement showed that the a cell lattice of mullite and the Al/Si molar ratio in the mullite formula depend on the ethylene glycol presence and on the calcination temperature. The lattice parameters b and c are not dependent on the alumina content, but the parameter a increases with the increase in the alumina content. Samples prepared with higher ethylene glycol concentrations reached higher mullite yields at lower temperatures.

The crystallization kinetics of ceramics composed by Bi2O3-ZnO-Nb2O5 (BZN) was studied using non-isothermal method. The BZN samples were prepared by the polymeric precursors method. Phase evolution was evaluated by X ray diffraction and the thermal events were evaluated by differential scanning calorimetry (DSC). The crystallization of BZN occurs from 500 to 700 °C, which corresponds to a secondary event in DSC curves. The principal exothermic event in these curves is related to the decomposition of organic material and was isolated from the crystallization peak by deconvolution into two Gaussian curves. Those related to crystallization processes were evaluated in terms of crystallized fraction. Kinetic parameters were determined from Ligero (E = 242 ± 7) kJ.mol-1 and Kissinger (E = 241 ± 24) kJ.mol-1 methodologies and they are very close. The activation energy Ea = (241 ± 24) kJ.mol-1 and (242 ± 7) kJ.mol-1 (by the Kissinger and Ligero methodology, respectively), frequency factor k0 =10(13).s-1 and exponent of Avrami n = (1.3 ± 0.1) were determined. The n value indicates that the crystallization is diffusion controlled, with decreasing nucleation rate. Scanning electronic microscopy showed the presence of nanoparticulated powder.