This paper reports the feasibility of synthesis and characterization of nano-porous silicon (NPS) powder and (Nickel/nano-porous silicon, Ni/NPS) nano-composite prepared using dual techniques (alkaline chemical etching process and ultra-sonication technique). The structural and the optical properties of the fabricated structures are inspected using X-ray Diffraction, Fourier Transform Infrared Spectrophotometer, Raman Spectroscopy, and Fluorescence Spectrophotometer Photoluminescence. All the results have agreed that NPS is one of the most suitable materials used as active material in the LED fabrication; by changing the main factors in the preparation process, so the different physical and chemical properties are obtained. NPS produces two emission regions that correspond to orange-red and dark red; on the other hand, (Ni/NPS) produce the yellow emission. So, the photoluminescence emission is controllable by adjusting the preparation conditions. The optical data recorded here are useful for the production of the nanoscale optical devices.