1 Department of Mechanical and Manufacturing Engineering, The Faculty of Engineering and Science, Aalborg University, VBN2 Materials Engineering and Science, The Faculty of Engineering and Science, Aalborg University, VBN3 The Faculty of Engineering and Science, Aalborg University, VBN4 Department of Chemistry, Institute TMC, University of Hamburg, Bundesstrasse 45, D-20146 Hamburg5 Leibniz-Institut für Polymerforschung (IPF), D-01069 Dresden6 Polymer Consult Ltd, Dorfgrund 6, D-22397 Hamburg7 National Research and Development Institute of Chemistry and Petrochemistry ICECHIM, Splaiul Independentei 202, Bucharest8 HASYLAB at DESY, Notkestraße 85, D-22603 Hamburg
The core–shell structure in oriented cylindrical rods of polypropylene (PP) and nanoclay composites (NCs) from PP and montmorillonite (MMT) is studied by microbeam small-angle x-ray scattering (SAXS). The structure of neat PP is almost homogeneous across the rod showing regular semicrystalline stacks. In the NCs the discrete SAXS of arranged crystalline PP domains is limited to a skin zone of 300μm thickness. Even there only frozen-in primary lamellae are detected. The core of the NCs is dominated by diffuse scattering from crystalline domains placed at random. The SAXS of the MMT flakes exhibits a complex skin–core gradient. Both the direction of the symmetry axis and the apparent perfection of flake-orientation are varying. Thus there is no local fiber symmetry, and the structure gradient cannot be reconstructed from a scan across the full rod. To overcome the problem the rods are machined. Scans across the residual webs are performed. For the first time webs have been carved out in two principal directions. Comparison of the corresponding two sets of SAXS patterns demonstrates the complexity of the MMT orientation. Close to the surface (<1 mm) the flakes cling to the wall. The variation of the orientation distribution widths indicates the presence of both MMT flakes and grains. The grains have not been oriented in the flowing melt. An empirical equation is presented which describes the variation from skin to core of one component of the inclination angle of flake-shaped phyllosilicate filler particles.
Science and Technology of Advanced Materials, 2014, Vol 15, Issue 1, p. 1-11