Uniform Gd2O2S flower-like nano-assemblies were prepared through one-pot mild solvothermal synthesis. The parallel nanoplates are the building blocks, ∼3 nm in thickness and 20–30 in diameter. Ethanediamine, the main solvent, plays an important role in dissolving a large amount of sulphur and producing active S2− ions, which results in the direct formation of Gd2O2S. Oleylamine, the capping agent, controls the growth of the plate-like structure. Under UV excitation, the Gd2O2S:Eu3+ nano-phosphor shows good red luminescence with a main emission peak at 627 nm. Under 980 nm laser excitation, Gd2O2S:xYb3+,1%Er3+ nano-phosphors exhibit a tuneable emission, shifting from greenish-yellow to orange-yellow, with increasing Yb3+ content.
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