Gallium phosphide is a semiconductor material of great interest for new modern LED technologies. HereGallium phosphide is a semiconductor material of great interest for new modern LED technologies. Herewe report the results of research on obtaining of nanostructured porous gallium phosphide layers byelectrochemical etching of the monocrystalline (100) p-type GaP substrate surface. The structure andsurface morphology of obtained samples were studied by scanning electron microscopy, atomic forcemicroscopy and Raman spectroscopy. The chemical composition of nanostructured GaP surfaces wasstudied by energy dispersive X-ray spectroscopy, which showed that the pore formation duringelectrochemical etching are mostly due to dissolution of phosphorus atoms rather than gallium .It wasfound that shape and size of structures are strongly depending on electrochemical etching conditions. Atconstant applied voltage and varied current we observe that the pore size is increasing from 10 μm to 50μm, and at fixed current, but varying the voltage the pore diameters can be achieved in the range between100 to 200 nanometers.