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Annealing is one of the stages of FePt nanoparticles preparation, during which the transition to a compositionally ordered phase occurs. In order to size and shape control of the nanoparticles in the mentioned stage, it is needed that they be distributed on a suitable surface. In the present work, the spin-coating method is suggested for preparing monolayer from L12-FePt3nanoparticles colloidal solution on SiO2/Si substrates. FePt3nanoparticles were gradually deposited as droplets on the center of a 500 rpm rotating substrate. This step was performed in hexane vapor atmosphere without any stopping time. The analyses revealed that a uniform surface distribution was formed so that, after annealing at 600 °C for 1 h the 6.1 nm L12-FePt3nanoparticles were spherical in shape with standard deviation of 1.5 nm.