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Poly(ester urethane) with varying polyester chain length: Polymorphism and shape-memory behavior
(2013)
The swelling, viscoelastic, and mechanical behavior of phase-segregated poly(ester urethane) (PEU) block copolymers, composed of 4,4'-methylenediphenyl diisocyanate, 1,4-butanediol as a chain extender, and crystallizable poly(1,4-butylene adipate) (PBA) with molecular weights between 1330 and 4120 g mol-1, are investigated. Wide-angle X-ray scattering (WAXS) is employed to study the overall PEU crystallinity, which increases from 8.6 to 13.6% at higher PBA contents. The existence of two crystalline, polymorphic PBA phases, a thermodynamically stable α phase and a metastable β phase, is confirmed by further WAXS measurements. Calorimetric and thermomechanical investigations give evidence for controllable PBA polymorphic behavior. The crystallization conditions, like the cooling rate, affect the emerging polymorphic mixture, whereas the storage conditions either promote or inhibit the polymorphic (β to α) transition. The introduced concepts represent a new approach for gaining control over programmable thermoresponsiveness, which may be transferable to other shape-memory polymers with polymorphic switching segments.
We demonstrate that phase-segregated poly(ester urethane) (PEU) with crystallizable switching segments of poly(1,4-butylene adipate) (PBA) excels as high-performance temperature-memory polymer. Temperature-memory effects (TMEs) with regard to strain and stress recovering could be programmed by polymer elongation at temperatures below or within the PBA melting transition, followed by cooling under constant stress below the PBA crystallization transition and unloading. Beyond that conventional approach, a novel TME programming route was designed, mostly consisting in specimen elongation and unloading at the same temperature. As a result, an enhanced control over the onsets of strain and stress recovering could be achieved. With these findings, the TME could be exploited to switch quick response (QR) codes in recently developed information carriers from unreadable to readable. We conjecture that such behavior can be programmed into virtually all semicrystalline elastomers and anticipate applicability as label technology to monitor temperature abuse of food and pharmaceuticals.
Hydrolytic degradation and functional stability of a segmented shape memory poly(ester urethane)
(2009)
In order to understand the effects of water and hydrolytic ageing on semi-crystalline poly(ester urethane) and its shape memory functionality, water immersion experiments at elevated temperature have been performed on a model substance and various parameters were monitored: change of the melting/crystallisation temperatures, substantial increase in crystallinity, temperature dependence of the water diffusion coefficient and solubility, hydrogen-bonding index and phase mixing by peak deconvolution of the FT-IR carbonyl region and day-to-day tensile and thermo-mechanical cyclic tensile tests. A rising fraction of freezable water agglomerates in the polymer was found for specimens cooled from the immersion temperature. The degradation process could be divided into three phases: an induction phase, a phase of continuous degradation and a phase of accelerated degradation. Shape recovery remains fairly constant during phase one and decreases slowly during phase two. The increase in crystallinity in phase two is accompanied by an increase in shape fixing ability.