Ta/NiOx/Ni81Fe19/Ta and Co/AiOx/Co multilayers were prepared by rf reactive and dc magnetron sputtering. The exchange coupling field (Hex) and the coercivity (Hc)of NiOx/Ni81Fe19 as a function of the ratio of Ar to O2 during the deposition process were studied. The composition and chemical states at the interface region of NiOx/NiFe were also investigated using the X-ray photoelectron spectroscopy (XPS) and peak decomposition technique. The results show that when the ratio of Ar to O2 is equal to 7 and the argon sputtering pressure is 0.57 Pa, the x value is approximately 1and the valence of nickel is +2. At this point, NiOx is antiferromagnetic NiO and the corresponding Hex is the largest.As the ratio of Ar/O2 deviates from 7, the Hex will decrease due to the presence of magnetic impurities such as Ni+3 or metallic Ni at the interface region of NiOx /NiFe, while the Hc will increase due to the metallic Ni. Al layers in Co/AIOx/Co multilayers were also studied by angle-resolved XPS. Our finding is that the bottom Co could be completely covered by depositing an Al layer about 1.8 nm. The thickness of AIOx was 1.2 nm.