Two-dimensional KTa0.77Nb0.23O3 (KTN) nanoplates with edge sizes of about 100 nm and thickness of about 10 nm have been fabricated by hydrothermal method at 200 degrees C using Ta2O5, Nb2O5, and KOH served as the precursors. Detailed structural studies indicate that the synthesized products are made up of large quantity single crystalline nanoplates with quadrilateral shape, which have a cubic perovskite structure without any other impurity phase and (011) growth direction. The stacking faults may be the key in the formation and growth, of the (011) plate. Room temperature photoluminescence spectra excited at different wavelengths exhibit a strong emission hand centered at 470 nm (2.63 eV) as well as two weak emission peaking at 423 nm (3.06 eV) and 505 nm (2.46 eV), respectively. The electron-hole recombination of localized excitons should responsible for the light emissions at 423 and 470 nm. Room temperature Raman spectrum of KTN nanoplates reveal that the frequencies of vibration mode are lower slightly than that of KTN bulk materials, and the scattering profile is to be more diffused and enlarged, which may be induced by the crystal structure defects, such as stacking faults. (c) 2007 Elsevier Inc. All rights reserved.