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Zinc ferrite (ZnFe2O4) nanoparticles is one of the semiconductor materials that can be used as a catalyst in photodegradation of Malachite Green. In this research, the synthesis of ZnFe2O4 nanoparticles was conducted by using coprecipitation method with microwave assistance, and then its effectivity in photodegradation of Malachite Green was studied. Synthesis of ZnFe2O4 nanoparticles with NaOH concentration variations of 1 M, 1.5 M, and 2 M had been successfully synthesized based on the results of XRD characterization. The peaks produced are following JCPDS Card No. 22–1012. The analysis of BET method showed that the surface area of ZnFe2O4 nanoparticles with NaOH concentrations of 1 M, 1.5 M, and 2 M are 1030.268 m2/g, 225.193 m2/g, and 1974.447 m2/g respectively. In addition, the photodegradation result of Malachite Green showed that ZnFe2O4 nanoparticles with NaOH concentration of 2 M was able to degrade 88.5% of malachite green in 90 minutes.