In order to study a new methodology that will provide a better size distribution and morphology of NaYbF4:Tm,Ho,Gd@NaYF4 nanoparticles two different syntheses methodology were used. This optimized system composition and hierarquical nanostructure is intended to improve the upconversion emission of the Tm(III) and Ho(III) ions in the UV-VIS-NIR regions. In the future, this system may be tested for bioimaging and phototherapy studies .