Fluorosilicone rubber (F-LSR) is a promising material that can be applied in various cutting-edge industries. However, the slightly lower thermal resistance of F-LSR compared with that of conventional PDMS is difficult to overcome by applying nonreactive conventional fillers that readily agglomerate owing to their incompatible structure. Polyhedral oligomeric silsesquioxane with vinyl groups (POSS-V) is a suitable material that may satisfy this requirement. Herein, F-LSR-POSS was prepared using POSS-V as a chemical crosslinking agent chemically bonded with F-LSR through hydrosilylation. All F-LSR-POSSs were successfully prepared and most of the POSS-Vs were uniformly dispersed in the F-LSR-POSSs, as confirmed by Fourier transform infrared spectroscopy (FT-IR), proton nuclear magnetic resonance spectroscopy (1H-NMR), scanning electron microscopy (SEM), and X-ray diffraction (XRD) measurements. The mechanical strength and crosslinking density of the F-LSR-POSSs were determined using a universal testing machine (UTM) and dynamic mechanical analysis (DMA), respectively. Finally, differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) measurements confirmed that the low-temperature thermal properties were maintained, and the heat resistance was significantly improved compared with conventional F-LSR. Eventually, the poor heat resistance of the F-LSR was overcome with three-dimensional high-density crosslinking by introducing POSS-V as a chemical crosslinking agent, thereby expanding the potential fluorosilicone applications.
Due to the growing demand for versatile hybrid materials that can withstand harsh conditions (below −40 °C), fluorosilicone copolymers are becoming promising materials that can overcome the limited operating temperature of conventional rubber. In order to synthesize a fluorosilicone copolymer, a potent initiator capable of simultaneously initiating various siloxane monomers in anionic ring-opening polymerization (AROP) is required. In this study, tetramethyl ammonium silanolate (TMAS), a quaternary ammonium (QA) anion, was employed as an initiator for AROP, thereby fluoro-methyl-vinyl-silicone (FVMQ) and fluoro-hydrido-methyl-silicone (FHMQ) were successfully synthesized under optimized conditions. FT-IR, NMR, and GPC analyses confirmed that the chain length and functional group content of FVMQ and FHMQ are controlled by changing the ratio of the components. Moreover, fluorine-involved liquid silicone rubber (F-LSR) was prepared with FVMQ as the main chain and FHMQ as a crosslinker. The tensile strength, elongation, and hardness of each F-LSR sample were measured. Finally, it was confirmed through TGA, DSC, TR-test, and embrittlement testing that elastic retention at low temperatures improved even though the heat resistance slightly decreased as the trifluoropropyl group increased in F-LSR. We anticipate that the optimization of fluorosilicone synthesis initiated by QA and the comprehensive characterization of F-LSRs with different fluorine content and chain lengths will be pivotal to academia and industry.
11 May 2023 in Journal of Thermal Analysis and Calorimetry
The objective of this study is to compare rice husk-derived silica (biosilica) synthesized via an environmentally friendly method with conventional silica (Zeosil 175) for reinforcing the mechanical properties of silicone rubber. The silanol group content of Zeosil 175 (9.45 OH/nm2) is higher than that of biosilica (7.07 OH/nm2), whereas the specific surface area of biosilica (159.52 m2/g) exceeds that of Zeosil 175 (144.90 m2/g). Silicone rubber specimens containing two types of silica nanoparticles were prepared at loading levels of 5, 10, 15, 20, 25, and 30 parts per hundred rubber to evaluate their mechanical properties and characteristics. Results indicate that silicone rubber filled with biosilica shows comparable tensile strength to Zeosil 175 at low filler contents, which can be attributed to its higher specific surface area. However, at higher loading levels, the mechanical properties are somewhat diminished due to the Payne effect and filler agglomeration resulting from the larger particle size of biosilica. These experimental findings offer insights into the potential utilization of rice husk-derived biosilica as an alternative to conventional silica in enhancing the properties of silicone rubber alongside the findings of the mechanical analysis.