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We report the procedure for hydrothermal synthesis of ultrasmall Yb³⁺/Tm³⁺ co-doped Sr₂LaF₇ (SLF) upconversion phosphors. These phosphors were synthesized by varying the concentrations of Yb³⁺ (x = 10, 15, 20, and 25 mol%) and Tm³⁺ (y = 0.75, 1, 2, and 3 mol%) with the aim to analyze their emissions in the near IR spectral range. According to the detailed structural analysis, Yb³⁺ and Tm³⁺ occupy the La³⁺ sites in the SLF host. The addition of Yb³⁺/Tm³⁺ ions has a huge impact on the lattice constant, particle size, and PL emission properties of the synthesized SLF nanophosphor. The results show that the optimal dopant concentrations for upconversion luminescence of Yb³⁺/Tm³⁺ co-doped SLF are 20 mol% Yb³⁺ and 1 mol% Tm³⁺ with EDTA as the chelating agent. Under 980 nm light excitation, a strong upconversion emission of Tm³⁺ ions around 800 nm was achieved. In addition, the experimental photoluminescence lifetime of Tm³⁺ emission in the SLF host is reported. This study discovered that efficient near IR emission from ultrasmall Yb³⁺/Tm³⁺ co-doped SLF phosphors may have potential applications in the fields of fluorescent labels in bioimaging and security applications. © 2022 by the authors.