Abstract-Tadpole-shaped (Ni, Al)/AlN nanoparticles were synthesized via evaporating Ni-Al alloy in a mixed atmosphere of N 2 and H 2 . As a counterpart, the spherical-shaped (Ni, Al)/Al 2 O 3 nanoparticles were also prepared from the same target alloy while in a mixture of Ar and H 2 . The electromagnetic parameters of as-made nanoparticles/paraffin composites were then investigated in the frequency range of 2-18 GHz. Excellent microwave absorption can be obtained for the tadpole-shaped (Ni, Al)/AlN-paraffin composite at high frequencies and in a thin layer, which is thought to be the result of the enhanced polarization in the anisotropic tadpole-shaped nanoparticles. With the increasing of the composite thickness, the frequency of effective reflection loss shifts towards lower frequencies due to an improved impedance match and absorption.