Sesame-like TbF3:Eu3+ microcrystals were prepared via sonochemical route without the assistance of any templates. The results suggested that the sesame-like particles with diameter of 250 nm at the center and length of about 500 nm can be obtained via assembly of thin nanosheets. The efficient energy transfer from Tb3+ to Eu3+ was observed under the 369 nm UV light excitation. With the increase of Eu3+ ions concentration, the emission colors and energy transfer efficiency of TbF3:Eu3+ microcrystals can be adjusted. The mechanism of energy transfer between Tb3+ and Eu3+ was also confirmed as electrical dipole-dipole interaction. (C) 2014 Elsevier Ltd. All rights reserved.