Tb
3+- and Eu
3+-doped lanthanum oxysulfide nanocrystals (NCs) with homogeneous grain size have beenprepared by a gel-network coprecipitation method using gelatin as the template and ammonium sulfate as thesulfurizing agent and a following reduction process at relatively low temperatures (750
C) in a H
2 atmosphere.The products were characterized using thermogravimetry-differential thermal analysis (TG-DTA), X-raydiffractometry (XRD), and transmission electron microscopy (TEM). The gelatin template can act as a"nanoreactor", which is beneficial to the dispersion and size control of the coprecipitation product. The highdecomposition temperature (about 482
C) of the gelatin network is advantageous to prevent aggregation ofthe newly formed (LaO)
2SO
4 NCs during calcination of the coprecipitation product. Single hexagonal phaseLa
2O
2S NCs were obtained by reduction of the (LaO)
2SO
4 powder, and the NCs are equiaxial in shape withparticle sizes ranging from 40 to 50 nm. The photoluminescence spectra and time-resolved spectra of theLa
2O
2S:Tb(Eu) in phosphate buffer were investigated. The results show that the La
2O
2S:Tb NCs have a strongluminescence at 544 nm, whose intensity decreases along with decreasing particle size. Concentration quenchingoccurs when the Tb concentration reaches 8 mol %. The fluorescence color of the La
2O
2S:Eu NCs dependson the concentration of Eu
3+ ions. The red emission (at 625 nm) from
5D
0 transition has a much longer decaytime than the green emission from
5D
1 transition of the La
2O
2S:Eu NCs. The Tb
3+- and the Eu
3+-dopedLa
2O
2S NCs have respective fluorescence
lifetimes of 1.10 and 0.41 ms in phosphate buffer, allowing theirpotential app
lications in biological labe
ling.