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Magnetic Co1-xNixFe2O4 nanoparticles (NPs) were successfully synthesized via a solvothermal method using ethylene glycol as solvent.The samples were characterized by X-ray diffraction (XRD),field emission scanning electron microscopy (FESEM),transmission electron microscopy (TEM),vibrating sample magnetometry (VSM) and gas sensing test.The experimental results showed that the magnetic CO1-xNixFe2O4 NPs were composed of single phase spinel structure and the average crystallite size in the NPs is between 5.8 and 9.8 nm; the NPs are spherical with an average particle size of about 40-90 nm; the saturation magnetization (Ms) of the COl-xNixFe2O4 NPs decreased linearly as the contents of Ni2+ increased; and the as-prepared Co1-xNixFe2O4 NPs have a higher selectivity toward ammonia vapors and the Co0.sNi0.2Fe2O4 has the best gas sensitivity of Co1-xNixFe2O4 (0≤x≤ 1) NPs at working voltage of 8 V.