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The Effect of Thickness of Fe3O4 Film on the Nature of Photoelectrochemical (PEC) from Fabricated Fe3O4/ZnO Film Using Spin Coating Method Nandang Mufti(1,2)*, Eva Khikmiatul Maula(1), Yudyanto(1,2), Chusnana Insjaf Yogihati(1,2), Suriati Sufian(3), M. Tommy Hasan Abadi(1), Siti Maryam(1) 1Department of Physics, Faculty of Mathematics and Natural Science, State University of Malang. Jl. Semarang 5 Malang, 65145 Indonesia 2Centre of Advanced Materials for Renewable Energy, Universitas Negeri Malang, Jl. Semarang 5, Malang 65145, Indonesia 3Department of Chemical Engineering, Petronas Technology University. Bandar Seri Iskandar, 32610, Perak, Malaysia *Corresponding Author : nandang.mufti.fmipa@um.ac.id ABSTRACT: Photoelectrochemical (PEC) water splitting converts solar energy into electrical energy, and stored it in the form of hydrogen and oxygen molecules. In PEC system, semiconductor electrodes play an important role in the conversion of solar energy; ZnO is one of the semiconductor materials with excellent electrical properties which is suitable for an electrodes. However, wide band gap of ZnO about 3.37 eV only can be utilized for photon energy in the UV region of about 4%. Henceforth, a combination of ZnO with Fe3O4 is predicted to have advantages such as being able to absorb visible light, low toxicity, and easy achievement, therefore photoactivation can be improved. In this present study, Fe3O4/ZnO films were fabricated using spin coating and doctor blade methods. The XRD result shows that the crystal structure of ZnO and Fe3O4 are hexagonal and cubic spinel, respectively. while the thickness of Fe3O4, ZnO, and Fe3O4/ZnO can be seen in Cross-sectional SEM test. Fe3O4 layer can increase PEC efficiency, where the efficiency value produced in Fe3O4/ZnO film is 0.15%, greater than the single layer of ZnO film is 0.035% and a single layer of Fe3O4 film is 0.038%. Keywords: Photoelectrochemical, Crystal Structure, Efficiency