Epoxy resin nanocomposites were prepared by curing bisphenol-F with an aliphatic amine in the presence of SiO 2 and ZrO 2 nanoparticles as inorganic fillers. Both types of particles were prepared with diameters of around 10 nm and 70 nm to study size effects in the nanocomposites. The nanoparticles showed a different constitution: while silica was amorphous and spherical in nature, zirconia was crystalline and non-spherical. Both nanoparticles were surface-functionalized with novel diethyleneglycol-based capping agents to increase the compatibility with the epoxy matrix. The organic functionalities were attached to the nanoparticle surface via phosphonic acid (zirconia) and trialkoxysilane (silica) anchor groups. The homogeneity of the distribution of surface-modified inorganic nano-sized fillers in the matrix up to 5.8 vol% in case of silica and 2.34 vol% in case of zirconia was determined by small-angle X-ray scattering and transmission electron microscopy. Mechanical properties such as hardness and storage modulus were increased with increasing filler content while thermal stability of the obtained materials was nearly unaffected after incorporation of nanoparticles.
The surface functionalization of inorganic nanoparticles is an important tool for the production of homogeneous nanocomposites. The chemical adaptation of the nano-filler surface can lead to effective weak to strong interactions between the fillers and the organic matrix. Here we present a detailed systematic study of different surface-functionalized particles in combination with a SAXS method for the systematic investigation of the interface interaction in the development of epoxy nanocomposites. We investigated the effect of surface modification of spherical SiO2 nanoparticles with 9 nm and 72 nm diameter and crystalline ZrO2 nanoparticles with 22 nm diameter on the homogeneous distribution of the fillers in diethylenetriamine (DETA) cured bisphenol-F-diglycidylether epoxy resin nanocomposites. Unmodified nanoparticles were compared with surface-modified oxides having diethylene glycol monomethyl ethers (DEG), 1,2-diols, or epoxy groups attached to the surface. The influence of surface modification on dispersion quality was investigated by transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS) for inorganic filler contents of 3, 5 and 10 wt%. It was shown that the dispersion quality can be optimized by varying the coupling agent end group to obtain homogeneous and transparent nanomaterials. UV/VIS measurements confirmed the transparency/translucency of the obtained materials. The relationship between particle–matrix interaction and particle–particle interaction plays a decisive role in homogeneity and is controlled by the surface groups as well as by the type, size, and morphology of the nanoparticles themselves.
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