Nanocomposites, activated carbon/polyvinyl alcohol (AC/PVA) filled with Fe to form Fe/AC/PVA, were characterized by using X-ray fluorescence (XRF), X-ray diffraction (XRD), Fourier transform infrared (FTIR), and vector network analyzer (VNA). The crystal orientations from Fe are (104), (110), and (200) and the bonding formations of AC are O-H, C-H, and C=C show existence in nanocomposites, which may be due to the Fe that has been filled the pore of AC via a chemical bond. 20% AC (3 mm in thickness) in nanocomposites shows higher performance absorption for C-band (4.65 GHz) with maximum reflection loss of −32.5 dB.