Eu3+ doped yttrium hydroxide nanosheets were successfully synthesized from layer compound of Y2(OH)5NO3 doped by Eu3+. Firstly layer compound of Y2(OH)5NO3 doped by Eu3+ was obtained by hydrothermal reaction. After ion exchange reaction with SDS, the layer space became lager. Furthermore stable nanosheet sol was prepared after exfoliation. The structure of layer compound and nanosheets were determined by XRD, TEM. The luminescence properties of yttrium hydroxide nanosheets doped with Eu3+ were examined; the relationship between structure and spectra was discussed.