Ba 3 Y (4−4x−4y) Er 4x Yb 4y O 9 precursor was synthesized by ammonium bicarbonate co-precipitation method, and its chemical formula is: (NH 4 ) x Ba 3 RE 4 (OH) y (CO 3 ) z · n H 2 O (RE 3+ =Y 3+ , Er 3+ and Yb 3+ ). The target product was obtained by calcining at 1400 °C in muffle furnace after 5 h. By means of Thermogravimetric Analysis (TG), X-ray diffraction (XRD), Field Emission Scanning Electron Microscope (FE-SEM), Fourier transform infrared (FT-IR), photoluminescence/photoluminescence excitation (PLE/PL), fluorescence attenuation and color coordinate, the composition, structural characteristics, particle morphology and fluorescence performance of the precursor and target product were studied. The particle size of the precursor was between 50 nm–100 nm, and the particle size of the calcined product was between 1 μ m−2 μ m. The absorption capacity of the fluorescent material to light is enhanced with the increase of doped ions. The optimal dosage of Yb 3+ /Er 3+ co-doped Ba 3 Y (4−4x−4y) Er 4x Yb 4y O 9 was x = 0.05 and y = 0.20. The color coordinate of Ba 3 Y 3 Er 0.2 Yb 0.8 O 9 phosphor is (0.73, 0.27) and the color temperature is 7383.6 K, showing excellent red light emission.