Mixed-metal oxides with the composition Y 3 Sc x Ga 5Àx O 12 (x ¼ 2.0, 2.1, 2.2, 2.25, 2.3, 2.4, 2.5, and 3.0) have been prepared by an aqueous sol-gel method. The effects of scandium substitution on the garnet phase formation were studied by IR spectroscopy and X-ray powder diffraction (XRD). The XRD data indicate that single-phase Y 3 Sc x Ga 5Àx O 12 ceramic samples were obtained for x ¼ 2.0, 2.1, 2.2, 2.25, 2.3, and 2.4. The results also show that the formation of Y 3 Sc x Ga 5Àx O 12 garnets depends on the molar ratio of scandium and gallium in the investigated composition, and consequently on the mean cationic radius at the Al 3þ sites. The variation of lattice parameters for the Y 3 Sc x Ga 5Àx O 12 phases with different x is reported.