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Studium der Röntgen-Kleinwinkelstreuung von Nylon-6 unter Verwendung der absoluten Intensitätsmessung

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Zusammenfassung

Das Ziel der vorliegenden Untersuchung ist vor allem die Ermittlung des kristallinen und amorphen Anteils der untersuchten Proben aus dem mittleren Schwankungsquadrat der Elektronendichte, die aus der Absolutintensität der Röntgenkleinwinkelstreuung hergeleitet werden kann. Es sollen ferner die mittleren Dimensionen der kristallinen Anteile aus der Intensität des Auslaufes der Streukurven berechnet werden.

Abstract

The mean square electron density fluctuations\(\overline {\Delta \rho ^2 }\) of three Nylon-6 samples (untreated, stretched, stretched and tempered) were obtained from the scattering curves. The degree of crystallinity of each sample was calculated from\(\overline {\Delta \rho ^2 }\) and from the densities of the crystalline and amorphous phases,d c =1.23 andd a =1.10, which were available from the literature. Crystallinities thus obtained were found to be as much as 50% less than those calculated from measured sample densitiesd. The discrepancy was ascribed to a small uncertainty ind a , the amorphous density: the calculated crystallinities are very sensitive to small changes in this parameter. If one sets the crystalline volume fractions obtained from\(\overline {\Delta \rho ^2 }\) equal to those obtained fromd, an equation ford a in terms of\(\overline {\Delta \rho ^2 }\) andd results, and is solved to yieldd a -values only about 1% higher than the literature value and of course consistent with both X-ray and density determinations. The volume fractions of the crystalline phases range from 20 to 30%. The possibility that the samples contained small amounts of air-filled holes may be excluded, since thed a -values (based on\(\overline {\Delta \rho ^2 }\) andd) calculated on the assumption of a volume fraction of as little as 0.3% for such holes are already much too high.

The specific inner surface and an average dimension of the regions of the two phases were also determined. The crystalline regions are roughly 30 Å in size, the amorphous ones three to four times as large, and largest for the tempered sample.

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Brumberger, H., Kratky, O. & Mittelbach, P. Studium der Röntgen-Kleinwinkelstreuung von Nylon-6 unter Verwendung der absoluten Intensitätsmessung. Monatshefte für Chemie 95, 1599–1608 (1964). https://doi.org/10.1007/BF00901718

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