Die elektronenmikroskopische Darstellung der Morphologie partiell kristalliner Polymere am Beispiel des Polyamid‐6

Abstract

Zur Charakterisierung der ubermolekularen Struktur von kompaktem Polyamid-6 wurden elektronenmikroskopische Untersuchungen an Ultradunnschnitten unter Anwendung verschiedener Hartungs-und Kontrastierungsmethoden durchgefuhrt. Neben der konventionellen Transmissionselektronenmikroskopie wurde die Hochstspannungselektronenmikroskopie eingesetzt, die es ermoglicht, dickere Schnitte zu untersuchen. Vergleichende Untersuchungen wurden an Dunnfilmen vorgenommen. Die durch den EinfluR hohen Druckes bei der Kristallisation von PA-6 verursachten morphologischen Veranderungen wurden sowohl anhand von Bruchflachenabdrucken als auch rasterelektronenmikroskpisch nachgewiesen. 3~e~m p o n n o -~~~. p o c l~0 n~~e~~0 e uaobpa~wenue ~o p~o a o z u u a.wop&o-~pucmwaucJcu.teciEua: noauaepoa na npunepe noauuuaa-G AJIH XapaKTepHCTHKH HaJ&MOJXeKyJIRpHOfi CTPYKTYPM KOMIIaKTHOI'O n o~r~a~~n a -6 IIpOBeAeHbI aJIeKTPOHHO-MkIKPO- Electron microscopic investigations of the morphology of partially c ystalline polymers with polyamided as an exampleThe supramolecular structure of compact polyamide-6 was investigated by electron microscopy with ultrathin sections using different methods of solidification and contrasting. Besides usual transmission electron microscopy the high voltage electron microscopy was applied which allows to investigate thick sections. Comparative investigations were performed with thin films. The changes in morphology caused by high pressure in the crystallization of polyamide-6 are demonstrated by fracture surface replication as well as by scanning electron microscopy.

The electron microscope characterization of the fine structure of nylon 6: I. The supermolecular structure in melt-cast, isotropic bulk material

“…This method has yielded detailed information on the fine structure of PE in recent years. Concerning other crystalline polymers, staining techniques have rarely been used up to now (see [7]). K 75 Phosphotungstic acid (PTA) which is well known for the negative staining of proteins, seems to be a suitable reagent for all polyamids according to the early investigations by Hess et al [8] on dispersed fibrils from nylon 6 fibres, by Spit [9,10] on solutiongrown nylon 6 films, and by Crystal and Hansen [11] on sections from nylon 66 bulk material.…”

“…For investigations on the bulk it proved, however, to be very difficult in general to combine the requirements of high efficiency staining with appropriate sectioning properties of the material so as to produce suitable ultrathin sections. In [7,12] we reported the first systematic application of PTA to visualize the structure of bulk nylon 6. In the meantime, Weber et al [13][14][15] have proposed a new staining method using a mixture of formaldehyde and osmium tetroxide in an aqueous solution.…”