Spinel-type Li-0. (35) Zn-0. (3) Fe-2. (35) O-4 micro/nanofibers were prepared through electrospinning and calcination technique. The crystalline phase and micromorphology of the samples calcined at various temperatures( 700, 800, 900 and 1000 degrees C ) for 2 h in air were examined by differential scanning calorimetry( DSC ) -thermalgravimetric analysis ( TGA ), Fourier transform infrared spectroscopy( FTIR ), X-ray diffraction( XRD ) and field emission scanning electron microscopy( FESEM ). Microwave absorption properties of Li-0. (35) Zn-0. (3) Fe-2. (35) O-4 micro/nanofibers were deter. mined with a vector network analyzer. The results showed that pure spinel structure formed at 700 degrees C and above. As the temperature increased, Li-0. (35) Zn-0. (3) Fe-2. (35) O-4 exhibited micro/nanofibrous, 3D network, bamboo. like or granular morphology. The minimum reflectivity of Li-0. (35) Zn-0. (3) Fe-2. (35) O-4 micro/nanofibers at 700 degrees C moved to a low frequency as the matching thickness increased. The matching thickness of Li-0. (35) Zn-0. (3) Fe-2. (35) O-4 micro/nanofibers was 6 mm below 8 GHz, at which the microwave absorption properties were fine. The minimum reflectivity could reach -26 dB at 5. 0 GHz, and the frequency band with reflectivity less than -10 dB was 4. 0 8. 0 GHz.