Considerable efforts have been exerted on the facile synthesis of magnetic composite materials because of their unique properties and potential applications. Especially for ferromagnetic-antiferromagnetic systems, the magnetic exchange bias effect is essential for the development of magneto-electronic switching devices and magnetic storage media. In this research, a facile ethylene glycol in situ reduction strategy has been successfully employed in the preparation of Ni-Cr 2 O 3 composite hollow spheres. X-Ray powder diffraction was used to determine the phase composition. Scanning electron microscopy and transmission electron microscopy was employed to characterize the morphologies of the as-prepared samples. Experiments proved that the volume ratio of ethylene glycol to water played a determinative role in the final morphology of the products. The magnetization vs. temperature results revealed a spin-glass-like behavior with blocking temperature of about 150 K for the as-prepared Ni-Cr 2 O 3 composites. Induced by the coupling between ferromagnetic Ni and antiferromagnetic Cr 2 O 3 , a small exchange bias effect could be observed in the magnetic hysteresis loops. At lower temperature, a larger exchange bias field and coercivity are obtained. A high surface area of 145.1 m 2 g −1 was obtained for the prepared porous hollow spheres.