We report on the synthesis and Raman scattering characterization of composite materials based on the hostnanoporous matrices filled with nanostructured KH 2 PO 4 (KDP) crystal. Silica (SiO 2 ) and anodized aluminium oxide (AAO) were used as host matrices with various pore diameters, inter-pore spacing and morphology. The structure of the nanocomposites was investigated by X-ray diffraction and scanning electron microscopy. Raman scattering reveals the creation of one-dimensional nanostructured KDP inside the SiO 2 matrix. We clearly observed the stretching ν 1 , ν 3 and bending ν 2 vibrations of PO 4 tetrahedral groups in the Raman spectrum of SiO 2 + KDP. In Raman scattering spectra of AAO + KDP nanocomposite, the broad fluorescence background of AAO matrix dominates to a great extent, hindering thus the detecting of the KDP compound spectral response.