YVO₄:Er³⁺ and YVO₄:Er³⁺, Yb³⁺ nanomaterials were prepared via combustion synthesis using urea as fuel and metal nitrates as precursor. The morphology and the structure of the prepared samples were characterized by x-ray diffraction, scanning electron microscopy and transmission electron microscopy. The average size of the prepared materials ranged from 20 to 30 nm in diameter. The effects of Er³⁺ and Yb³⁺ doping concentrations on structure and optical properties have been investigated. Optical properties of YVO₄:Er³⁺ and YVO₄:Er³⁺, Yb³⁺ nanoparticles were measured by photoluminescent excitation and emission spectroscopies. For the YVO₄:Er³⁺ and YVO₄:Er³⁺, Yb³⁺ samples, two strong green emissions centered at 524 and 552 nm are found, corresponding to the ²H_11/2—⁴I_15/2 and ⁴S_11/2—⁴I_15/2 transitions of Er³⁺ ions, respectively. Upconversion emission in the green region of the YVO₄:Er³⁺ nanoparticles under 980 nm excitation was also investigated. Strong emission from these materials is promising for luminescent biolabeling applications.