The one-pot process, which combines the polymerization of polyaniline (i.e., PANI) with subsequent reduction of iron nanowire (i.e., Fe NW) under a magnetic field, was developed to produce Fe@PANI core–shell nanowires. The synthesized nanowires with various PANI additions (0–30 wt.%) were characterized and used as microwave absorbers. Epoxy composites with 10 wt.% absorbers were prepared and examined using the coaxial method to reveal their microwave absorbing performance. Experimental results showed that the Fe NWs with PANI additions (0–30 wt.%) had average diameters ranging from 124.72 to 309.73 nm. As PANI addition increases, the α-Fe phase content and the grain size decrease, while the specific surface area increases. The nanowire-added composites exhibited superior microwave absorption performance with wide effective absorption bandwidths. Among them, Fe@PANI-90/10 exhibits the best overall microwave absorption performance. With a thickness of 2.3 mm, effective absorption bandwidth was the widest and reached 3.73 GHz, ranging from 9.73 to 13.46 GHz. Whereas with a thickness of 5.4 mm, Fe@PANI-90/10 reached the best reflection loss of −31.87 dB at 4.53 GHz.
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