The fabrication and the characterization of Al 2 O 3 /Ni composites with a gradient distribution of the Ni particles are reported. The composites have been obtained by centrifugal-slip casting and subsequent sintering and had the shape of a hollow cylinder. TG/DTA analysis was done for the nickel powder with the addition of the dispersant used in centrifugal-slip casting as well as for the composite green body. The measurements were performed in two atmospheres: argon and the mixture of argon and hydrogen (1:1). Additionally, coupling the thermobalance with the mass spectrometer allowed to determine type of gases released from the samples during thermal treatment. The morphology and chemical composition of the produced composites were analyzed using a scanning electron microscope equipped with an EDS detector. Interface between alumina and nickel was described. Moreover, the X-ray diffraction was made. The stereological analysis confirmed that the nickel particles are distributed in the composite in a gradient way.