This paper presents on the results of the sol-gel preparation of the microcrystalline gadolinium aluminate (GdAlO3, GAP) ceramics at slightly different synthetic conditions. Metal ions generated by dissolving the starting materials of metals in the diluted acetic acid were complexed by different complexing agents (natural and synthetic tartaric acids, 1,2-ethanediol, citric acid, ethanolamine)to obtain the precursors for the GAP. In the sol-gel processing different starting gadolinium materials such as gadolinium nitrate or gadolinium oxide were also employed. Phase transformations, composition and microstructural features in the gels and polycrystalline samples were studied by powder X-ray diffraction analysis (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM).