Nano-sized Eu 3+-doped GdBO 3 vaterite type nanophosphors have been synthesized successfully via acetylacetone assisted aqueous sol-gel route. Systematic investigation of the influence of Eu 3+ ion content and pH value of the suspension of precursors on structural, morphological and luminescence spectroscopic properties has been performed. X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, field emission-scanning electron microscopy (FE-SEM), Thermogravimetric and differential thermal gravimetry (TG/DTA), room temperature steady and time resolved photoluminescence (PL) spectroscopy techniques were employed to characterize the obtained powder samples. It has been found that the Eu 3+ ion content and pH value precursors suspension have important effect on the structural, morphology and emission properties. The XRD analysis reveals that GdBO 3 : 10% mol Eu 3+ synthesized at pH = 2 and pH = 10 exhibit the quasipurest P6 3 /mmc vaterite structure. The vibrational absorption of (BO 3) 3group is assigned to the GdBO 3 with calcite type or other vaterite structure namely triclinic and monoclinic. The morphologies of GdBO 3 particles size increases with increasing of pH value. All sample present only the orange-red colors emission from 5 D 0 levels to the 7 F J levels (J = 0-3) of Eu 3+ ion. Furthermore, it was found that 10% concentration of Eu 3+ presents the quenching of emission in GdBO 3. Also, it was that the emission intensity was affected by the pH value and sample with pH = 10 exhibits the highest emission intensity. The asymmetry ratio parameter R between red and orange emission intensities in function of Eu 3+ content and pH value is determinate and discussed.