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 Spec-troscopy, 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.
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