For the first time, a systematic study to investigate the electrospinnability of cyclic olefin polymer (COP) was performed. Different solvents and mixtures were tested together with different electrospinning parameters and post-treatment types to prepare bead-free fibers without defects. These were successfully obtained using a chloroform/chlorobenzene (40/60 wt.%) solvent mixture with a 15 wt.% COP polymer, a 1 mL/h polymer solution flow rate, a 15 cm distance between the needle and collector, and a 12 kV electric voltage. COP fibers were in the micron range and the hot-press post-treatment (5 MPa, 5 min and 120 °C) induced an integrated fibrous structure along with more junctions between fibers, reducing the mean and maximum inter-fiber space. When the temperature of the press post-treatment was increased (from 25 °C to 120 °C), better strength and less elongation at break of COP fibers were achieved. However, when applying a temperature above the COP glass temperature (Tg = 138 °C) the fibers coalesced, showing a mechanical behavior similar to a plastic film and a low elongation at break with a high strength. The addition of a high dielectric constant non-solvent, N,N-dimethylacetamide (DMAc), resulted in a considerable reduction in the COP fiber diameter. Based on the cloud point approach, it was found that the use of DMAc and the solvent chloroform or chlorobenzene improved the electrospinnability of COP polymer solution.

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