Thermal curing and water re‐exposure of silane–PVA/PVAc complex film on glass fiber surface

Because glass fiber reinforced composites are in industrial demand, chemistry and topography of the glass fiber sizing are of interest. Silane–PVA/PVAc (polyvinyl alcohol/polyvinyl acetate) complex film on the glass fiber surface is studied during thermal curing and water re‐exposure by using atomic force microscopy. The complex film consists of silane with the honeycomb structure film and PVA/PVAc with the hexagonal close pack structure of ellipsoidal shaped microspheres (270 × 620 nm). The thermal curing at 100 °C is leading to the evaporation of water contained in the microspheres. Because of water evaporation, the average roughness value of 1‐min thermal curing decreases from initial 7.3 to only 2.7 nm. Such a collapse of microsphere is followed by an intermixing between silane film and PVA/PVAc microspheres leading to a change of silane honeycomb structure along with silane tips. The average value of the silane honeycomb structure wall width decreases from 144 nm to 54 nm, for curing times of 15 and 30 min, respectively. A re‐exposure to an aqueous environment after 100 °C curing leads to almost completely restored microspheres regarding shape and size. The average complex film thickness increases from 180 nm for thermal curing for 30 min to 225 nm for water re‐exposed film. Interestingly, the pits in the microsphere structure are observed presumably because of the tips from intermixing. The thermal curing at 200 °C enhances the intermixing, and after 15 min, an intramixing is suggested to occur between PVAc core and PVA shell of the microsphere. The water re‐exposure after 15 min of 200 °C curing leads to a re‐containing of water but without restored microsphere structure; Because of the intramixing, leaving the silane–PVA/PVAc film is not complex anymore. Copyright © 2014 John Wiley & Sons, Ltd.