In this study yttrium aluminium garnet (YAG) specimens in which yttrium was partially substituted by lanthanum Y3-xLaxAl5O12 (YLaAG) were prepared by an aqueous sol-gel method. The resulting sol was concentrated by slow solvent evaporation at 65 oC. The obtained gels were dried in an oven at 120 oC for 24 h. The obtained precursor gel powders were calcined at 800 oC and 1000 oC in air. YLaAG samples were analyzed by X-ray diffraction (XRD), solid state nuclear magnetic resonance (NMR), scanning electron microscopy (SEM) and electron paramagnetic resonance (EPR) methods. Luminescence measurements of YLaAG samples were also recorded. The XRD analysis results showed that only low substitution of yttrium by lanthanum is possible in Y3-xLaxAl5O12 without destroying garnet crystal structure. It was also demonstrated in this study, that solid state NMR and EPR methods are indispensable tools for the explanation of processes and properties observed in the newly synthesized Y3-xLaxAl5O12 compounds.