Hydrolysis products of aqueous yttrium nitrates obtained by sol-gel method at room temperature, under atmospheric pressure without any templates and structure directing agents were investigated by thermal analysis combined with mass spectrometry of thermolysis products, XRD and scanning electron microscope with elemental EDS analyzer. Formation of yttrium hydroxonitrocarbonates with various ratio depending on synthesis conditions was found. The samples obtained at 8.5 pH with hydrolysis time at least 40 min using ammonia water solution have the least quantity of impurities and demonstrates the most visible layered morphology. The most explicit layered morphology and the least amount of impurities were revealed in the samples obtained at 8.5 pH with hydrolysis time at least 40 min using ammonia water solution as a hydrolytic agent.