Electrolytic Ni–Re alloy coatings were obtained in galvanostatic conditions from nickel–rhenium baths with different contents of ammonium rhenate(vii) (0.5, 1.25, 2.5 and 5 g·L−1). The surface morphology, chemical, and phase composition of the obtained materials were determined. The coatings’ corrosion resistance tests were carried out in a 5% NaCl solution. Based on the tests, it was found that the highest corrosion resistance characterizes the coating with the highest rhenium content (37%). This material can be recommended for practical use as a protective coating. The density of the deposited Ni–37Re alloy was determined, and its specific surface area was assessed. The melting point, hardness, and electrical conductivity were also determined.