This study presents the systematic potential effects of reaction parameters on the synthesis of Co-doped ZnNi ferrite/polyaniline composites prepared via novel interfacial polymerization. Through intensive experiments and analysis, optimum reaction conditions including the polymerization temperature and reaction time are proposed so that the performance of the material is significantly improved. The structure, functional groups and morphologies of composites are investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Fourier transform-infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). In addition, the electromagnetic properties and microwave absorption properties of Co-doped ZnNi ferrite/polyaniline composites are examined by a vibrating sample magnetometer (VSM), Quantum Design (MPMS-VSM and MPMS-XL), the superconducting quantum interference device (SQUID) magnetometer and vector network analysis. Based on these analyses, it is found that by tuning the reaction conditions, i.e., polymerization temperature and reaction time, microwave absorption capabilities in terms of the maximum reflection loss (R L) value and absorber thickness can be readily optimized. The results show that the composite with an optimized polymerization condition of 20 °C for 12 h displays remarkable microwave absorption properties with maximum reflectivity of -54.3 dB, and the effective bandwidth (R L < -10 dB) is about 6.02 GHz at a thickness of 6.8 mm. Furthermore, the discussion shows that the promising microwave absorption may be due to the uniform urchin-like structure of the composites.
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