Abstract. Synthesis of Fe 3 O 4 /a-SiO 2 nanoparticle has been conducted based on natural materials by using the co-precipitation method. The used silica was a-SiO 2 collected from silica sand from Bancar Tuban, Indonesia. The Fe 3 O 4 collected from iron sand's Lumajang, Indonesia. The samples was set for Fe 3 O 4 : a-SiO 2 : PEG composition of 1 : 2 : 1. The process was maintained by melting the PEG 4000 and following by adding a-SiO 2 and Fe 3 O 4 . The samples were characterized by using X-Ray Diffractometry (XRD), Transmission Electron Microscopy (TEM), and Fourier Transform Infra-Red (FTIR) spectroscopy. The analysis of the XRD data showed that additional silica into Fe 3 O 4 tended to change the diffraction pattern that represents the existent of both Fe 3 O 4 and silica. The SEM images presented that the samples formed in nanometric size with core-shell structure. Furthermore, the FTIR spectra showed that Si-O-Fe bound appeared at 555-568 cm -1 . Thus, this work was able to produce the Fe 3 O 4 /aSiO 2 nanocomposites by using co-precipitation method in a core-shell structure.