This study explores the synthesis, structural characterization, and photoluminescence properties of Eu³⁺ -doped Mg₄ P₂ O₇ andCa₄ P₂ O₇ nanophosphors. Utilizing glycine-assisted solution combustion and high-temperature solid-state methods, phase-pure andhighly crystalline phosphors were developed. Structural features were investigated through X-ray diffraction (XRD), Fourier-transforminfrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The Mg₄ P₂ O₇ :Eu³⁺phosphor exhibited intense red emission centered at 615 nm under 395 nm excitation, corresponding to the ⁵ D₀ → ⁷ F₂ electric dipoletransition. In contrast, Ca₄ P₂ O₇ :Eu showed strong blue emission around 422 nm, attributed to the partial reduction of Eu³⁺ to Eu²⁺ .Thermogravimetric analysis (TGA) confirmed excellent thermal stability, supporting the potential of these phosphors in white light-emittingdiodes (w-LEDs) and optoelectronic devices.Keywords: Europium, Mg₄ P₂ O₇ , Ca₄ P₂ O₇ , Photoluminescence, Nanophosphors, Red-emitting phosphors