Abstract
Using dynamic transmission electron microscopy, we have studied in-situ the effects of thermal curing/annealing on microstructural elements within films of unstained siloxaneimide (SiIm) and stained styrene–butadiene–styrene (SBS) block copolymers. Samples of the SiIm multiblock copolymer, only partially cured, were heated to 100°C and 212°C, with the appearance of siloxane domains increasing with curing time. Microstructural coalescence was observed at 324°C, suggesting the presence of a phase transition. SBS transition kinetics are prefaced by theoretical predictions of the equilibrium separation temperature Ts as a function of molecular weight and composition, leading to Ts∝M̅0.8n. Since the presence of a stain alters all kinetic phenomena, a model based on free-volume theory was devised to estimate how the stain concentration affects local viscosity. Annealing of initially non-equilibrated SBS sample films was observed to cause increased ordering of styrene domains as temperature increased, with phase inversion at elevated temperatures. Lamellar development was found to occur by coarsening in areas where some lamellae initially formed; structure bands, measuring 110nm across and separated by 280 nm, were observed to form in initially homogeneous regions.
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Spontak, R., Williams, M. Microstructural Response of SiIm and SBS Block Copolymers to Heat Treatment. Polym J 20, 649–671 (1988). https://doi.org/10.1295/polymj.20.649
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DOI: https://doi.org/10.1295/polymj.20.649
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