Highly aligned, single-layered hollow fibrous membranes are prepared using two-fluid coaxial electrospinning (ES). Polyethylene oxide (PEO) is used as the core, and polyurethane (PU) and blends of PU with silica (SiO2) are used as the shell to extract the PEO. The effects of the polymer-complex concentration, the ES parameters, and the SiO2 blending ratio on the morphologies and mechanical properties of fibers are explored. Using an appropriate PU concentration and applied spinning voltage combination yields a high fiber-alignment degree. The hollow fibrous average area increases as the inner-to-outer flow-rate ratio (FRRi/o) increases because the inner flow increases. When using a PU concentration of 13 wt%, a spinning voltage of 7 kV, and an FRRi/o of 0.8, along with blending 15% SiO2 with PU, the fiber alignment of the PU/SiO2 membranes is 95%. The Young's modulus indicates that adding SiO2 enhances the mechanical properties, causing a monolayer hollow-fiber assembly with interconnected fibers to form.
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