Porous anodic alumina oxide (AAO) obtained via two-step anodization is a material commonly used as a template for fabricating 1D nanostructures. In this work, copper and cobalt-iron 1D nanocones were obtained by an electrodeposition method using AAO templates. The templates were produced using two-step anodization in H2C2O4. The Co–Fe nanostructures are characterized by homogeneous pore distribution. The electrocatalytic activity of the produced nanomaterials was determined in 1 M NaOH using the linear sweep voltammetry (LSV) and chronopotentiometry (CP) methods. These materials can be used as catalysts in the water-splitting reaction. The sample’s active surface area was calculated and compared with bulk materials.