Sol-gel autocombustion is confirmed to be an efficient method in the synthesis of Co-Ni alloy powder. Addition of adequate amount of ethanol can make the reduction reaction thorough and increase the purity of the samples. X-ray diffraction measurement indicates that the obtained samples consist of a single phase with bcc structure. Transmission electron microscopy study shows the grain size is about 10 nm. The magnetic measurements show that the samples are a soft magnetic material with the coercive field smaller than 100 Oe and the saturation magnetization about 95% of the theoretical value. (C) 2011 Elsevier B.V. All rights reserved.