Issue 25, 2014

Silica-diblock fluoropolymer hybrids synthesized by surface-initiated atom transfer radical polymerization

Abstract

Silica/diblock fluoropolymer hybrids SiO2-g-PMMA-b-P12FMA for coatings were synthesized by the silica surface-initiating atom transfer radical polymerization (SI-ATRP) of methylmethacrylate (MMA) and dodecafluoroheptyl methacrylate (12FMA). Silica surface initiator (SiO2-initiator) was obtained by 10–25 nm fumed silica particles grafted hydrosilylated undec-10-enyl, 2-bromo-2-methyl propionate with a density of 0.573 mmol g−1. The SI-ATRP approach in this paper displays the diagnostic criteria of controlled radical polymerization by the analysis of 1H NMR, 19F NMR and SEC-MALLS analysis, after comparing with the conventional initiator of ethyl 2-bromoisobutyrate (EBiB) for the E-PMMA-b-P12FMA diblock copolymer. Three mass ratios of SiO2-initiator/MMA/12FMA as 1/72.50/18.15, 1/72.50/45.38 and 1/181.26/18.15 were used to obtain the SiO2-g-PMMA-b-12FMA hybrids. The hybrids show 25–30 nm core–shell particles in CHCl3 solution composed of a P12FMA core and PMMA shell, but densely twined together as agglomerated particles. The PMMA-b-P12FMA shell grafted onto silica particles obviously increases the surface roughness of the film (50–500 nm), more than the E-PMMA-b-12FMA film (30 nm), and thereby contributes to the hydrophobic (112–118°) and oleophobic (45–78°) properties of the films. Increasing the P12FMA concentration (1/72.50/45.38) could result in stronger migration of the P12FMA segments onto the film surface, and therefore led to a lower surface free energy (10.97 mN m−1), increased advancing and receding for water contact angles (112° and 108°) and the highest cetane contact angles (74° and 70°), the lower water absorption and viscoelasticity, but a high thermostability at 420–450 °C.

Graphical abstract: Silica-diblock fluoropolymer hybrids synthesized by surface-initiated atom transfer radical polymerization

Supplementary files

Article information

Article type
Paper
Submitted
06 Dec 2013
Accepted
20 Jan 2014
First published
24 Jan 2014

RSC Adv., 2014,4, 13108-13118

Silica-diblock fluoropolymer hybrids synthesized by surface-initiated atom transfer radical polymerization

H. Huang and L. He, RSC Adv., 2014, 4, 13108 DOI: 10.1039/C3RA47393G

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