A basic study of fibrillation and void development during drawing of melt spun polypropylene filaments is presented. The filaments are characterized by small angle x-ray scattering (SAXS), density, differential scanning calorimetry (DSC), scanning electron microscopy (SEM), wide angle x-ray diffraction (WAXS), and birefringence. The latter two methods were used to characterize the molecular orientation produced by processing while SEM studies of peeled filaments revealed, qualitatively, the development of the fibrillated internal superstructure. The volume fraction of microvoids was computed from the intensity of SAXS and from a combination of DSC and density measurements. The microvoid fractions determined by these two techniques were in good agreement. The volume per cent of microvoids varied from 0.04 to 2.8%. It was found that the fibrillation observed qualitatively by SEM and the measured volume fraction and number density of microvoids increased with (i) increase in draw ratio, (ii) decrease in draw temperature, (iii) increased orientation of melt spun filaments, and (iv) increased molecular weight of the polypropylene. Using Guinier analysis of the SAXS data it was found that the voids had dimensions of 25–40 nm, parallel to the fiber axis and of order 15 to 30 nm perpendicular to the fiber axis. As the drawing temperature increased the SAXS void size increased and void number density decreased. The longitudinal mechanical properties of the fibers were found to be mainly a function of the orientation and were not very much affected by changes in fibrillation or void structure per se.
Poly(p-phenylene terephthalamide) (PPD-T) films have been prepared by continuous extrusion of liquid crystalline 17 percent PPD-T/sulphuric acid solutions through an annular die followed by coagulation. Films extruded without drawdown exhibit some polymer chain orientation in the machine direction. This is increased by uniaxially drawing down films. Films produced with a lubricated conical mandrel sitting between the die and the coagulation bath exhibit an equal biaxial orientation. The uniaxially oriented films exhibit highly anisotropic mechanical properties, while the mandrel-produced film exhibits balanced properties. Heat treatment at 350°C results in significant enhancement of the tensile strength of the mandrel film. Void structures in the films have been investigated by mass density, scanning electron microscopy (SEM), and small-angle X-ray scattering (SAXS). Density measurements indicate a void content decreasing with decreasing film thickness and heat treatment. SEM locates micron-size voids in the thickest films, apparently caused by rapid coagulation. SAXS indicates much smaller void sizes which are roughly prolate ellipsoids (long axis in machine direction) for uniaxial films and oblate ellipsoids (short axis in thickness direction) for the mandrel produced films. Various techniques are used to estimate mean void size.(16) used a lubricated mandrel and developed significant levels of biaxial orientation, i.e., orientation in the transverse as well as the machine direction.In this paper, w e continue our studies of the development of a process for biaxially oriented films of PPD-T and the characterization of such films. W e again consider the mandrel process technology, but include the post-extrusion annealing step. W e compare such films with those of different process histories. The crystalline orientation of the films is carefully characterized. In addition, we will carefully characterize the void sizes/distribution developed in the films.
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