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- ItemEffect of Molar Mass on Critical Specific Work of Flow for Shear-Induced Crystal Nucleation in Poly (l-Lactic Acid)(Basel : MDPI, 2021) Du, Mengxue; Jariyavidyanont, Katalee; Kühnert, Ines; Boldt, Regine; Androsch, RenéThe concept of specific work of flow has been applied for the analysis of critical shearing conditions for the formation of crystal nuclei in poly (l-lactic acid) (PLLA). Systematic variation in both time and rate of shearing the melt in a parallel-plate rheometer revealed that these parameters are interconvertible regarding the shear-induced formation of crystal nuclei; that is, low shear rate can be compensated for by increasing the shear time and vice versa. This result supports the view that critical shearing conditions can be expressed by a single quantity, providing additional options for tailoring polymer processing routes when enhanced nuclei formation is desired/unwanted. Analysis of PLLA of different mass-average molar masses of 70, 90, 120, and 576 kDa confirmed improved shear-induced crystal nucleation for materials of higher molar mass, with critical specific works of flow, above which shear-induced nuclei formation occurs, of 550, 60, 25, and 5 kPa, respectively.
- ItemProcess induced skin-core morphology in injection molded polyamide 66(Basel : MDPI, 2020) Spoerer, Yvonne; Androsch, René; Jehnichen, Dieter; Kuehnert, InesPolyamide 66 (PA 66) was injection-molded to obtain samples with a structure gradient between skin and core, as it was revealed by analysis of the semi-crystalline morphology using polarized-light optical microscopy (POM). Wide-angle X-ray scattering (WAXS) and small-angle X-ray scattering (SAXS) were employed to characterize thin sections with a thickness in the order of magnitude of 50 µm, allowing detection of crystals of different perfection, as a function of the distance from the surface. It was found that the transparent and non-spherulitic skin layer contains rather imperfect α-crystals while the perfection of α-crystals continuously increases with extending distance from the surface. Since variation of the molding conditions allows tailoring the skin-core morphology, the present study was performed to suggest a reliable route to map the presence of specific semi-crystalline morphologies in such samples
- ItemEnthalpy relaxation, crystal nucleation and crystal growth of biobased poly(butylene isophthalate)(Basel : MDPI, 2020) Quattrosoldi, Silvia; Androsch, René; Janke, Andreas; Soccio, Michelina; Lotti, NadiaThe crystallization behavior of fully biobased poly(butylene isophthalate) (PBI) has been investigated using calorimetric and microscopic techniques. PBI is an extremely slow crystallizing polymer that leads, after melt-crystallization, to the formation of lamellar crystals and rather large spherulites, due to the low nuclei density. Based upon quantitative analysis of the crystal-nucleation behavior at low temperatures near the glass transition, using Tammann’s two-stage nuclei development method, a nucleation pathway for an acceleration of the crystallization process and for tailoring the semicrystalline morphology is provided. Low-temperature annealing close to the glass transition temperature (Tg) leads to the formation of crystal nuclei, which grow to crystals at higher temperatures, and yield a much finer spherulitic superstructure, as obtained after direct melt-crystallization. Similarly to other slowly crystallizing polymers like poly(ethylene terephthalate) or poly(l-lactic acid), low-temperature crystal-nuclei formation at a timescale of hours/days is still too slow to allow non-spherulitic crystallization. The interplay between glass relaxation and crystal nucleation at temperatures slightly below Tg is discussed.