Dual modified nanosilica particles as reinforcing fillers for dental adhesives: Synthesis, characterization, and properties

Abstract

A facile procedure has been devised to develop a novel dentin bonding system containing poly (acrylic acid)-grafted-silanized fumed silica particles as reinforcing filler, with high stability of nanoparticle dispersion and enhanced bond strength and mechanical properties. In the first step, the silanization of fumed silica nanoparticles was performed in the following conditions: (i) ethanol-water solution with a pH of 5 and (ii) cyclohexane with a pH of 9 using trimethoxysilylpropyl methacrylate (γ-MPS) as a reactive silane coupling agent. FTIR and TGA analyses confirmed the presence of silane in the resultant structure and enhanced dispersion stability of modified particles was proved by a separation analyzer and also zeta potential analyses. In the second step, free radical polymerization of acrylic acid monomers in the presence of silanized nanoparticles was carried out and poly (acrylic acid) -grafted- silanized fumed silica were acquired. The flexural strength and fracture toughness of the adhesive containing 0.2 wt.% of the dual modified filler reached maximum of 70.4 MPa and 1.34 MPa m^1/2, respectively, showing average improvements of 74% and 179%, respectively, in comparison with the adhesive without filler. Flexural modulus values did not significantly change with increasing the filler content except the adhesive containing 5 wt.% having the lowest flexural modulus. The highest microtensile bond strength was also observed at 0.2 wt.% filler content showing the average improvements of 197% as compared with the neat adhesive. Energy dispersive X-ray (EDX) mapping confirmed a homogenous and uniform distribution of the fillers in the adhesive matrix containing 0.2 wt.% and 0.5 wt.% of filler while incorporation of 5 wt.% led to large particle aggregates. SEM images of the fracture surface of the adhesive with different filler contents subjected to fracture toughness test showed rougher surface and longer crack path by increasing filler concentration. The adhesive containing 0.2 wt.% of filler perfectly penetrated into the dentin tubules proved by the SEM micrographs in microtensile bond strength test.

Keywords: Dental adhesives; Graft polymerization; Mechanical properties; Microtensile bond strength; Silanization; Silica nanoparticle.