The increased compression strength of an epoxy resin with the addition of heat-treated natural nano-structured diatom frustules

Abstract

Natural diatom frustules composing nanometer size silica particles were heat-treated at temperatures between 600 and 1200℃ for 2 h and used as filler/reinforcing agent (15 wt%) in an epoxy resin. The opal structure of as-received natural diatom frustules was transformed into cristobalite after the heat-treatment above 900℃. The epoxy resin test samples reinforced with heat-treated and as-received frustules and neat epoxy test samples were compression tested at the quasi-static strain rate of 7 × 10⁻³ s⁻¹. The results showed that the inclusion of the frustules heat-treated at 1000℃ increased the compressive yield strength of the resin by 50%, while the addition of the diatom frustules heat-treated above and below 1000℃ and the as-received frustules increased the strength by ∼25% and 16%, respectively. The heat treatment above 1000℃ decreased the surface area of the frustules from 8.23 m² g⁻¹ to 3.46 m² g⁻¹. The cristobalite grains of the frustules heat-treated at 1000℃ was smaller than 100 nm, while the grain size increased to ∼500 nm at 1200℃. The increased compressive stresses of the resin at the specific heat treatment temperature (1000℃) were ascribed to nano size crystalline cristobalite grains. The relatively lower compressive stresses of the epoxy resin filled with frustules heat-treated above 1000℃ were attributed to the micro-cracking of the frustules that might be resulted from higher density of the cristobalite than that of the opal and accompanying reduction of the surface area and the surface pore sizes that might impair the resin-frustule interlocking and intrusion.