Experimental methods for creating and characterization of
well-defined oriented semi-crystalline polymer samples
Citation for published version (APA):
Housmans, J. W., Peters, G. W. M., & Meijer, H. E. H. (2003). Experimental methods for creating and
characterization of well-defined oriented semi-crystalline polymer samples. In PC2003 : Polymer Crystallization
and Structure Formation in Processing, 20 years of fundamental and applied research in Linz, an international
mini-conference, September 19-20, 2003, Linz, Austria
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Published: 01/01/2003
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Polymer Crystallization and Structure Formation in Processing September 19-20 2003 – Linz, Austria
1 Recommended Format of Extended Abstracts
EXPERIMENTAL METHODS FOR CREATING AND
CHARACTERIZATION OF WELL-DEFINED ORIENTED
SEMI-CRYSTALLINE POLYMER SAMPLES.
.
Jan-Willem Housmans, Gerrit W.M. Peters,
Han E.H Meijer.
Eindhoven University of Technology, Materials Technology, Department of mechanical Engineering,
Dutch polymer Institute, P.O. Box 513, 5600 MB Eindhoven, The Netherlands
ABSTRACT
A good prediction of the final properties of a product made of semi-crystalline polymers requires an experimentally validated model that includes all the aspects required, i.e. the influence of the (numerous) parameters and of thermal and flow conditions. However, at this stage of ongoing research there is still a lack on experimental data for different polymers, both for the characterization of model parameters and model validation.
To obtain the experimental data, an experimental flow device, the multipass rheometer (MPR), Fig. 1(a), was tested and a flow cell was developed for this set-up. The MPR consists of a test section that is positioned in between two servo-hydraulically driven pistons with which a (reversed) shear flow is applied to the polymer melt. The final micro-structure of the samples was characterized with optical light microscopy (LM), transmission electron microscopy (TEM), wide angle X-ray diffraction (WAXD) and small angle X-ray scattering (SAXS).
Going from the skin to the core in samples, made in a capillary flow configuration with a repeated back and forth flow during cooling, three layers could be distinguished using LM and WAXD (Fig. 1(b)). The structures of these layers were determined from the WAXD patterns. The transparent (middle) layer is a highly oriented layer consisting of shish-kebab structures, which is confirmed with SAXS and TEM.
Comparison between samples made for different flow conditions showed that an increase in shear rate affected both the degree of orientation as well as the position and thickness of the highly oriented layer. Samples with a low initial shear rate showed almost no orientation when a small flow amplitude was applied, but the orientation increased with increasing flow amplitude.
(a) (b)
Figure 1: (a) Multipass rheometer. (A) flow cell (exchangeable), (B) pistons (within a heating/cooling cylinder).
(b) Normalized (110) plane azimuthal scans over half the width of the sample.
