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In carbide ceramics, ZrC has a high melting point, high hardness, and excellent thermal conductivity and electrical conductivity. It can be used as a suitable additive phase for SiC nanomaterials to enhance its high-temperature resistance to oxidation and its microwave absorption property. In our work, heterogeneous SiC/ZrC/SiZrOC hybrid nanofibers with different ZrC contents are prepared using polycarbosilane and zirconium acetylacetonate as raw materials through electrospinning and hightemperature pyrolysis processes. With an increase in the ZrC content from 0 to 10 wt %, the electrical conductivity of the hybrid nanofibers increases from 0.3448 to 2.5676 S/cm, and the average diameter decreases from 800 to 200 nm. The SiC/ZrC/SiZrOC hybrid nanofibers result in improved microwave-absorbing capability with a minimum reflection loss of about −40.38 dB at 14.1 GHz, a thickness of 4 mm, and antioxidant properties at 600 °C. These results prove that the heterogeneous SiC/ZrC/SiZrOC hybrid nanofibers have reasonable electrical conductivity. This results in dielectric loss, which is mainly because of the added ZrC. The dipole polarization, interfacial polarization, quarter-wave cancellation, and conductivity loss are the main reasons for the enhanced microwave absorption.

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