Poly(hydroxybutyrate-co-3-hexanoate) (PHBH) is a biodegradable thermoplastic polyester with the potential to be used in textile and medical applications. We have aimed at developing an upscalable melt-spinning method to produce fine biodegradable PHBH filaments without the use of an ice water bath or offline drawing techniques. We have evaluated the effect of different polymer grades (mol% 3-hydroxy hexanoate, molecular weight etc.) and production parameters on the tensile properties of melt-spun filaments. PHBH monofilaments (diameter < 130 µm) have been successfully melt-spun and online drawn from three different polymer grades. We report thermal and rheological properties of the polymer grades as well as morphological, thermal, mechanical, and structural properties of the melt-spun filaments thereof. Tensile strengths up to 291 MPa have been achieved. Differences in tensile performance have been correlated to structural differences with wide-angle X-ray diffraction and small-angle X-ray scattering. The measurements obtained have revealed that a synergetic interaction of a highly oriented non-crystalline mesophase with highly oriented α-crystals leads to increased tensile strength. Additionally, the effect of aging on the structure and tensile performance has been investigated.
This data in brief article summarizes structural data obtained from monocomponent melt-spun and offline drawn poly(ethylene terephthalate) (PET) monofilaments, as well as from melt-spun bicomponent core-sheath PET-polyamide 6 (PA6) filaments. The diameters of the single filaments range from 27 µm to 79 µm. Presented analysis techniques and results thereof are (i) Raman mapping of filament cross-sections: 2D maps of peak positions, widths, peak area ratios; (ii) attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR): ATR-FTIR spectra and extraction of surface crystallinity; (iii) wide-angle x-ray diffraction (WAXD): WAXD patterns and extraction of average crystallinity; (iv) small-angle x-ray scattering (SAXS): SAXS patterns and determined crystallite sizes and long-spacings; (v) differential scanning calorimetry (DSC): thermograms and extracted average crystallinity as well as thermal properties; (vi) atomic force microscopy (AFM): AFM image of the surface of an embedded fiber cross-section. For more information, see the publication by E. Perret et al. 'High-resolution 2D Raman mapping of mono- and bicomponent filament cross-sections' [1].
Mechanical properties of as-spun, aged and stress-annealed melt-spun poly(3-hydroxybutyrate) (P3HB) fibers are presented in section 1.1. Section 1.2 presents tables with stress/temperature conditions and exposure times during in-situ laboratory WAXD and SAXS experiments, and section 1.3 presents azimuthal profiles of the corresponding WAXD patterns with extracted orientation factors of the α-crystals. Section 1.4 presents the extracted long-spacings, coherence lengths and crystal sizes from SAXS patterns. The corresponding fits of meridional and transversal SAXS profiles are shown in sections 1.5 and 1.6, respectively. In-situ synchrotron measurements during tensile drawing of differently pre-annealed P3HB fibers are presented in section 1.7. A detailed description of the tensile, SAXS/WAXD measurements and analysis is given in the experimental section 2. The laboratory SAXS/WAXD measurements during stress annealing were performed with a Bruker Nanostar U diffractometer (Bruker AXS, Karlsruhe, Germany) and a heating stage H+300 (Bruker AXS, Germany). Different weights were attached to the fibers during heating to apply stress. The synchrotron measurements during tensile drawing were performed at the cSAXS beamline at the Swiss Light Source of the Paul Scherrer Institute in Switzerland. The fibers were drawn with a TS 600 tensile stage (Anton Paar GmbH, Austria) using a 5 N load cell. For more information see 'Structural response of melt-spun poly(3-hydroxybutyrate) fibers to stress and temperature' [1].