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Ta/NiO/NiFe/Ta multilayers were prepared by rf reactive and dc magnetron sputter-ing. The exchange coupling field (Hex) between NiO and NiFe reached 120Oe. Thecomposition and chemical states at the interface region of NiO/NiFe were studied us-ing the x-ray photoelectron spectroscopy (XPS) and peak decomposition technique. Theresults show that there are two thermodynamically favorable reactions at NiO/NiFeinterface: NiO+Fe = Ni+FeO and 3NiO+2Fe 3Ni+Fe2 O3. The thickness of thechemical reaction as estimated by angle-resolved XPS was about 1-1.5nm. These in-terrace reaction products are magnetic defects, and we believe that the Hex and thecoereivity (He) of NiO/NiFe ave affected by these defects. Moreover, the results alsoshow that there is an intermixing layer at the Ta/NiO (and NiO/Ta) interface dueto a thermodynamically favorable reaction: 2Ta+5NiO＝5Ni+Ta2O5. This interfacereaction has an effect on the exchange coupling as well. The thickness of the inter-mixing layer as estimated by XPS depth-profiles was about 8-10nm.