Nickel-indium alloys were considered as potential hydrogen storage materials. X-ray diffraction studies showed that with increase in the indium concentration in the Ni–In composite intermetallic phases were formed (InNi2, InNi3, In3Ni2, η-In27Ni10, InNi). Thermal desorption was used to quantify the content of hydrogen included in composites during their synthesis by the electrolysis method. Hydrogen peaks were observed at temperatures of 550 and 850 K. Mass spectroscopy was used to study the spectrum of thermal desorption of deuterium from Ni70In30-Dx composites, and the temperature ranges of desorption of ion-implanted deuterium were determined depending on the implantation dose. An increase in the content of implanted deuterium to 3×1018 D / cm2 leads to the formation of a solid solution of deuterium in the Ni70In30 composite, the decomposition temperature of which in vacuum is ∼ 530 K, and nickel hydride with hydrogen with a decomposition temperature of ∼ 350 K. The integral amount of desorbed deuterium was determined from the irradiation dose to 4 × 1018 D / cm2 for the Ni70In30 composite. The maximum concentration of deuterium is ∼ 2 at. D/at. Met., Corresponding to the ratio Met.: D2 = 1:2. The calculation of the activation energy of thermal desorption for a hydrogen peak with a maximum temperature of 500 K. The value of the activation energy for a peak with a maximum temperature of 500 K is 2.9 eV.