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Yb3+/Er3+ co-doped NaYF4 (NaYF4: Yb3+, Er3+) hexagonal nanoplates were synthesized by a tetrasodium iminodisuccinateassisted hydrothermal synthesis method for the first time. The crystal structure and morphology was investigated by the Xraydiffraction and scanning electron microscope analysis. The upconversion luminescent property of the synthesized NaYF4:Yb3+, Er3+ hexagonal nanoplates was discussed as a function of Yb3+ and Er3+ concentration. Under 980 nm excitation, NaYF4:Yb3+, Er3+ hexagonal nanoplates exhibited strong red emissions near 660 nm and green upconversion emissions at 530 and 550nm corresponding to the intra 4f transitions of Er3+ (4F9/2, 2H11/2, 4S3/2) → Er3+ (4I15/2). The Yb3+ 5 mol% and Er3+ 0.5 mol%co-doped NaYF4 sample exhibited strongly shiny upconversion emission, which was considered to be the optimum dopingconcentration. A possible upconversion mechanism for NaYF4: Yb3+, Er3+ depending was discussed in detail.