The Ca 1−2x Ce 2x Mo 1−x Ge x O 4 (0 ≤ × ≤ 0.2) micro/nanosized powders were prepared by aqueous nitrate-tartrate sol-gel synthesis. The obtained samples were characterized by XRD analysis, SEM microscopy, and IR spectroscopy. It was shown, that increase of cerium concentration in the series of compounds does not lead to obvious changes in their crystal structure, but changes of unit cell lattice parameters was fixed. According to SEM analysis, particles of investigation molibdates have diameter 100–500 nm. Luminescence properties of the synthesized powders were studied. The photoluminescence spectra contain wide bands of matrix emission and narrow lines caused by f-f transitions in the RE 3+ ions.