Pb1-xMoO4:Er3+/Yb3+ phosphors with various doping concentrations of Er3+ and Yb3+ (x = Er3++Yb3+, Er3+ = 0.05, 0.1, 0.2, and Yb3+ = 0.2, 0.45) are successfully synthesized using a microwave sol-gel method, and the up-conversion photoluminescence properties are investigated. Well-crystallized particles, which are formed after heat treatment at 900 oC for 16 h, exhibit a fine and homogeneous morphology with particle sizes of 2-5 μm. Under excitation at 980 nm, the Pb0.7MoO4: Er0.1Yb0.2 and Pb0.5MoO4:Er0.05Yb0.45 particles exhibit a strong 525 nm emission band, a weak 550 nm emission band in the green region, and a very weak 655 nm emission band in the red region. The Raman spectra of the doped particles indicate the presence of strong peaks at higher and lower frequencies induced by the disordered structures of Pb1-xMoO4 through the incorporation of the Er3+ and Yb3+ ions into the crystal lattice, which results in the unit cell shrinkage accompanying the new phase formation of the MoO4-x group.