The future applications of hyperbolic metamaterials demand stacks of materials with alternative ultra-thin conductive/dielectric films with good homogeneity of the thickness and reduced roughness level. In this work, the technology of pulsed-DC magnetron sputtering of aluminum was optimized using the Taguchi method in order to fabricate Al films with improved roughness level. The performed structural characterization proved the smaller Al domains and better homogeneity of the surface. The optimized process was used to fabricate a multilayer structure of Al/HfOx as the metamaterial media. The fabricated structures were optically characterized in the UV/VIS range. The presented findings demonstrated the tunability effect of the effective reflectance of the examined stacks. The presented results are promising for the future application of multilayer structures in novel photonic devices based on hyperbolic metamaterials.