Studies of Structure and Morphology Development During the Heat-Draw Process of Nylon 66 Fiber by Synchrotron X-ray Diffraction and Scattering Techniques

Online studies of structure and morphology development during continuous drawing of a nylon 66 fiber at different temperatures were carried out using synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS) techniques. From the two-dimensional (2D) WAXD measurement, unit-cell parameters were determined. The results confirm that the triclinic cell structure persists above the Brill transition temperature (about 443 K). With increasing temperature, the unit-cell dimension a (dominated by hydrogen bonding) remains almost unchanged, while b increases and c decreases (both show a step-change at 403 K, prior to the Brill transition). The constant value of a agrees with the argument that the hydrogen bonding is relatively immobile at high temperatures prior to melting. The step-changes in b and c suggest that a premelting process of small (or defective) crystals precedes the Brill transition. As a result, the anisotropic thermal expansion of the surviving larger crystals results in a step-change behavior. This hypothesis is consistent with the crystal density data as well as the morphology evaluation by SAXS. Several dimensions were extracted from the 2D SAXS data: lamellar crystal and amorphous thicknesses (along the fiber) determined by the correlation function method, and crystal fibril width (perpendicular to the fiber) determined by the Porod analysis. These results also indicate that drawing annihilates small crystals, but the strain effect is much less than the temperature effect.