In this study, it has been presented the influence of pH conditions on the evolution of the size, morphology and spectroscopic properties of yttrium orthovanadate during synthesis. A thorough research on the spectroscopic properties was performed. A series of highly crystalline 1 mol% Eu³⁺:YVO₄ has been synthesized via the co-precipitation method. In addition, to improve the crystallinity, the materials were heat-treated at 800 °C, and the structural and morphological properties of the particles were studied using XRD (X-ray powder diffraction) and SEM (Scanning Electron Microscopy) techniques. In order to investigate the spectroscopic properties of 1 mol% Eu³⁺:YVO₄, emission spectra and luminescence kinetics were measured. It was found that alkaline pH manifests in smaller particles compared to acidic pH conditions. In addition, superior spectroscopic properties were observed in materials obtained in alkaline pH.