Y 2 O 3 :Eu 3+ nanocrystals were prepared via co-precipitation–solvothermal refluxing–calcination method using three kinds of organic solvents, propylene glycol, 1,3-butanediol and polyethylene glycol and yttrium chloride hexahydrate and europium chloride as starting materials. The Y 2 O 3 :Eu 3+ nanocrystals with diameter of 20–50 nm prepared by refluxing in polyethylene glycol followed by calcinations at 800–1000 °C exhibited the strongest luminescence at 611 nm under the excitation wavelength of 254 nm than the reference sample prepared via conventional co-precipitation method. The photoluminescence spectra of the samples were recorded at room temperature. The effect of concentration of Eu 3+ (Eu 3+ /Y 3+ atomic ratio: 0.01–0.1) on the photoluminescence intensity was also investigated. The samples with the Eu 3+ /Y 3+ atomic ratio of 0.07 exhibited the strongest emission at 611 nm and quenching effect was observed above 0.10.