The microwave hydrothermal method was applied in the synthesis of Ni0.5Zn0.5Fe2 O4 ferrite nanoparticle. X-ray diffraction (XRD), infrared spectroscopy (IR) were conducted to characterize the as-prepared samples. The experiment results revealed the as-prepared nanoparticle was 8.50-10.3 nm in size with various synthesis temperatures from 40-120°C, and synthesis temperature had effects on the magnetic and adsorption properties of Ni0.5Zn0.5Fe2 O4. The saturation magnetization values increased from 22.6 to 90.8 emu g-1 with synthesis temperature increasing. Moreover, synthesis temperature also influences the adsorption capacity of methyl orange (MO) on Ni0.5Zn0.5Fe2 O4. The as-prepared Ni0.5Zn0.5Fe2 O4 showed the highest adsorption capacity of MO in the current work when synthesis temperature was 80°C, which was contributed to the more adsorption site distributed on the nanoparticle.