In this paper, we report the mild sonochemical synthesis of hexagonal (?) NaYF4:Yb,Er mesocrystals at low temperature 40 °C. The nucleation and transformation crystal structures is investigated in course time, it shown that pure ? phase obtained after 2 h pulsed sonication. crystallization orthorhombic YF3:Yb,Er cubic (?) precedes appearance a thermodynamically stable phase. Based on evolution ...