Presented results describing properties of alloys deposited at potentiostatic conditions in Ni2+ - Pd2+ - Cl- - H2O system. Electrolysis parameters were defined based on results of thermodynamic analysis as well as voltammetry coupled with electrochemical quartz crystal microbalance (EQCM). Influence of electrode potential and electrolyte components concentration on alloy composition, morphology and its structure was investigated. Alloys were deposited at different Ni(II) and Pd(II) complexes concentrations. Results indicated possibilities of electrochemical synthesis of alloys of wide composition range. Deposits structure as well as crystallites size were discussed based on results of XRD measurements. Alloys composition was determined with the use of energy dispersive spectroscopy (EDS). Morphology of alloys was characterized with the use of scanning electron microscopy (SEM). (C) 2016 Elsevier B.V. All rights reserved.