Composite material based on KDP (KH2PO4) crystal matrix with incorporated aluminum oxyhydroxide Al2O3·nH2O nanoparticles is obtained and peculiarities of the formation of KDP:Al2O3·nH2O composite structure are studied by selective etching, optical and scanning electron microscopy. Influence of the nanoparticles on the formation of defect subsystem is analyzed. The obtained material is shown to have a zonal structure with a period independent of the concentration of nanoparticles. By means of FTIR‐spectroscopy, interaction of nanoparticles with KH2PO4 solution is studied. A model of the capture of nanoparticles by the {100} KDP crystal face is proposed.