The effects of bath composition and deposition variables on the electrodeposition of Zn-Ni-P alloys were studied in order to develop a single bath for deposition of Ni-P/Zn-Ni compositionally modulated multilayer coatings (CMMCs). The basis for development of the bath was a large increase in the Ni deposition rate compared to that of Zn at low deposition overpotentials combined with the impossibility of codeposition of Zn with P. EDS analysis demonstrated that the deposits obtained from the Zn-Ni-P bath at low overpotentials were practically all Ni-P, while the alloy deposited at high overpotentials was mainly Zn-Ni with around 3.2 wt% P content.