In this work the cationic photoinduced crosslinking of the diglycidylether of 4-hydroxyphenyl-4'-hydroxybenzoate was investigated in the liquid crystalline state as well as in the isotropic state. The photochemical curing technique was applied because only small amounts of the initiating species were necessary to form networks of epoxy compounds. As the photoin itiator system , a m ixtu re of a,a'-dimethoxydeoxybenzoin and dicumyliodon iumhexafluorophosphate proved to be the most effective. FTIR-spectra of the networks were compared with those of the starting material. Only small amounts of nonreacted epoxy groups were found in the networks synthesized either in the isotropic state or in the liquid crystalline state. Furthermore, different results were obtained with DSC-measurements. Networks prepared in the liquid crystalline state showed two glass transition temperatures. In contrast, networks synthesized in the isotropic state have only one glass transition temperature.Moreover, polarization microscopy was used to find ordered structures. The networks formed in the liquid crystalline state showed frozen ordered structures. Heating of such networks above the melting point of the starting material did not lead to a change of the frozen ordered structures. Additionally, differences between the frozen ordered structure of the networks and the crystalline structure of the starting compound were observed by this method. Finally, the material properties of networks with ordered structures are different from common networks with disordered structures.
ZUSAMMENFASSUNG:Zur Charakterisierung der iibermolekularen Struktur von schmelzegemischten Poly-
butylenterephthalat(PBT)/Polycarbonat(PC)-Blends
SUMMARY:Light-microscopic, X-ray and calorimetric investigations were carried out to characterize the morphology of melt-mixed poly(buty1ene terephthalate)(PBT)/polycarbonate(PC)-blends. A completely spherulitic structure up to a concentration of about 20 wt.-% PC was found by polarizing microscopy. A second separate, amorphous phase appears at higher PC concentrations. By differential scanning calorimetry, a shift of the glass transition temperature of PBT as well as PC, a slight melting point depression of the crystalline PBT-phase and different crystallization temperatures depending on the concentration of the pure components were measured. Wide-angle X-ray studies and additional density measurements gave reason to believe that the crystallinity of PBT in the blend is decreasing and that there is a possibility of crystallization of PC, particularly by a thermal post-treatment.* Korrespondenzautor.
KurzfassungMessende lichtmikroskopische Methoden, wie z.B. die Bestimmung der optischen Doppelbrechung haben überall dort eine überragende Bedeutung, wo in den zu untersuchenden Materialien bedingt durch den molekularen Aufbau mit lichtmikroskopischen Methoden kein Gefüge sichtbar gemacht werden kann. Das trifft auf alle amorphen Kunststoffe, wie z. B. Polystyrol zu.Ein besonderer Vorteil der Bestimmung optischer Daten an Kunststoffen besteht in der engen Korrelation dieser Daten zu den Kunststoffeigenschaften. Dadurch lassen sich relativ einfach online Einrichtungen zur zerstörungsfreien Charakterisierung der Produkte im Fertigungsprozess integrieren.Aber auch an teilkristallinen Polymeren können messende Verfahren zusätzlich zu der dort oft möglichen Gefügebewertung eingesetzt werden und liefern zusätzlich wertvolle Informationen. Diese Methoden werden im Teil B des Artikels ausführlich dargestellt.Neben der Bestimmung optischer Daten können zu den messenden Verfahren der Lichtmikroskopie noch eine Reihe weiterer Messmethoden gerechnet werden. Dazu gehören z. B. die Bestimmung der Mikrohärte, die Tief- und Hochtemperaturmikroskopie, Kristallisations-, Auflösungs-, Quell- und Diffusionserscheinungen im Mikroskop in Mikroküvetten sowie DTA – Untersuchungen an geringsten Mengen teilkristalliner Kunststoffe und an Kunststoffgemischen sowie-blends in speziellen Mikroheiztischen. Diese Verfahren werden ebenfalls im Teil B beschrieben.
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