In this paper, Fe3O4-ZnO heterostructure multifunctional nanoparticles (NPs) were successfully prepared in aqueous solution by ultrasound assisted thermolysis. First, iron oxide (Fe3O4) magnetic NPs were prepared by co-precipitation method. The Fe3O4 NPs were modified by 3-aminopropyltriethoxysilane (APTES) to have free amine (-NH2) groups on their surface, then, Zn2+ ions were added and stirred to adsorb onto the surface of Fe3O4-NH2 NPs in alkaline solution at a pH of 11. | VNU Journal of Science: Mathematics – Physics, Vol. 33, No. 1 (2017) 14-21 Synthesis, Magnetic Properties and Enhanced Photoluminescence of Fe3O4-ZnO Heterostructure Multifunctional Nanoparticles Chu Tien Dung1,2, Luu Manh Quynh1, Tran Thi Hong3, Nguyen Hoang Nam1,* 1 Faculty of Physics, VNU University of Science, 334 Nguyen Trai, Thanh Xuan, Hanoi, Vietnam Department of Physics, University of Transport and Communications, 3 Cau Giay, Hanoi, Vietnam 3 VNU University of Science, 334 Nguyen Trai, Thanh Xuan, Hanoi, Vietnam 2 Received 10 January 2017 Revised 25 February 2017; Accepted 20 March 2017 Abstract: In this paper, Fe3O4-ZnO heterostructure multifunctional nanoparticles (NPs) were successfully prepared in aqueous solution by ultrasound assisted thermolysis. First, iron oxide (Fe3O4) magnetic NPs were prepared by co-precipitation method. The Fe3O4 NPs were modified by 3-aminopropyltriethoxysilane (APTES) to have free amine (-NH2) groups on their surface, then, Zn2+ ions were added and stirred to adsorb onto the surface of Fe3O4-NH2 NPs in alkaline solution at a pH of 11. This solution was decomposed through thermolysis in ultrasound bath. The results of measurements show that photoluminescence of Fe3O4-ZnO heterostructure multifunctional NPs was enhanced in visible light at 565 nm wavelength to allow detection, labeling, diagnosis, and therapy in biomedicine. Moreover, they exhibit superparamagnetic properties of Fe3O4 with high saturation magnetization (MS), which can be used for seperation application in biomedicine under an external magnetic field. Keywords: Fe3O4-ZnO, multifunctional nanoparticles, heterostructure, enhanced photoluminescence. 1. Introduction In recent years, multifunctional nanoparticles (MNPs) based on fluorescent, magnetic, and plamonic nano-materials are becoming very important materials, which have been a hot research field in material sciences. Among these MNPs, the NPs combining luminescent and magnetic are the most popular .