Effective multiwalled carbon nanotube (MWCNT) fiber manufacturing methods have received a substantial amount of attention due to the low cost and excellent properties of MWCNTs. Here, we fabricated hybrid microfibers composed of hyaluronic acid (HA) and multiwalled carbon nanotubes (MWCNTs) by a wet-spinning method. HA acts as a biosurfactant and an ionic crosslinker, which improves the dispersion of MWCNTs and helps MWCNT to assemble into microfibers. The effects of HA concentration, dispersion time, injection speed, and MWCNT concentration on the formation, mechanical behavior, and conductivity of the HA/MWCNT hybrid microfibers were comprehensively investigated through SEM, UV-Vis spectroscopy, tensile testing, and conductivity testing. The obtained HA/MWCNT hybrid microfibers presented excellent tensile properties in regard to Young’s modulus (9.04 ± 1.13 GPa) and tensile strength (130.25 ± 10.78 MPa), and excellent flexibility and stability due to the superior mechanical and electrical properties of MWCNTs. This work presents an effective and easy-to-handle preparation method for high-performance MWCNT hybrid microfibers assembly, and the obtained HA/MWCNT hybrid microfibers have promising applications in the fields of energy storage, sensors, micro devices, intelligent materials, and high-performance fiber-reinforced composites.

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