Effect of reaction parameters on the structure and properties of acrylic rubber/silica hybrid nanocomposites prepared by sol-gel technique

摘要

The effects of a few reaction parameters, namely, type of solvents, tetraethoxysilane (TEOS)-to-water mole ratio, and temperature of gelation at constant concentration of TEOS (45 wt %) and pH of 1.5 were investigated for acrylic rubber/silica hybrid nanocomposites prepared by sol-gel technique. Infrared spectroscopic studies indicated the maximum, silica generation within the system when tetrahydrofuran was used as the solvent for the sol-gel reaction. The distribution of the silica particles (average dimension 100 nm) forming a network type of structure within the composite was confirmed by scanning electron microscopic studies (SEM). The other solvents studied here produced a lower amount of silica because of either high polarity of the solvents (methyl ethyl ketone and dimethyl formamide) or their limited miscibility with water (for ethyl acetate). An increase in the proportion of water caused silica agglomeration. Energy dispersive X-ray analysis (EDAX) silicon mapping also demonstrated the existence of agglomerated silica structures at high TEOS-to-water mole ratio (>2). Higher temperature for gelation of the composites caused the aggregation of silica particles. The uncured composites containing nanolevel (<90 nm) dispersion of silica particles demonstrated slightly higher storage modulus, lower value of tan and higher glass transition temperature compared to the composites with silica particles of a larger dimension (>2 mum). Improvement in tensile strength and modulus was observed in the uncrosslinked as well as in the crosslinked state (cured by a mixed crosslinking system of hexamethylenediamine carbamate and ammonium benzoate). However, the extent of improvement in strength and modulus for the nanocomposites was higher (247 and 57%, respectively) compared to the microcomposite (150 and 27%, respectively) in the cured state. (C) 2005 Wiley Periodicals, Inc.