The investigation on core@shell structured nanocomposites is a hotspot in material science. The dispersion and stability of core particles can be enhanced by coating with a stable shell layer to prevent the physical or chemical changes. Compared to single nanoparticles, improved performance can be achieved via the combined interactions of the cores and shells of the nanocomposites. Thus, core@shell nanocomposites are widely used in the fields of catalysis, photochemistry, electro chemistry, microelectronics, microwave absorption, drug therapy, and so on. In this study, nano-scale nickel-hydrazine complex(NHC)is fabricated by the reverse micelle approach in the oil phase with the nickel chloride and the hydrazine hydrate. Core@shell structured nickel-hydrazine composites (NHC@RF, NHC@SiO₂, NHC@RF@SiO₂) are synthesized by NHC coated with the resorcinol formaldehyde (RF) resin and silicon dioxide(SiO₂). The fabricated samples are characterized by transmission electron microscope (TEM), X-ray diffraction (XRD), transmission, attenuated total reflection and diffuse reflection Fourier transform of infrared spectroscopy (TR-FTIR, ATR-FTIR and DRS-FTIR). It is proved that the nano-rod structured NHC mainly includes Ni(N₂H₄)₂Cl₂ with a little Ni(NH₃)₆Cl₂. For TR-FTIR, the structure and surface properties might be changed by the potassium bromide though the possible ion exchange during the process of KBr tablet pressing. No sample pretreatment is needed for ATR-FTIR without any damage to the core@shell structured composites. ATR-FTIR focuses on the shell characterization of core@shell structure and can be used for the qualitative analysis of coating. Similar to ATR-FTIR, the nondestructive DRS-FTIR still requires the potassium bromide for dilution, and its detection depth and intensity are higher than that of ATR-FTIR and lower than that of TR-FTIR. The RF coating has little influence on the characteristics of NHC peak, while SiO₂ coating leads to red-shift of the stretching vibration and blue-shift of the bending vibration of N—H bonds, demonstrating the interaction between SiO₂ and N—H bonds.