Multi-layer NixZn1−xS/Ni foam composites were synthesized by a one-step hydrothermal reaction generating in situ growth on the Ni foam. The doping of Zn into the NixZn1−xS/Ni composite constructs the multi-layer nanostructure. The as-fabricated Ni1−xZnxS/Ni foam-2 h supercapacitor electrode shows outstanding rate properties.