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Combustion methods are a promising strategy for the lanthanide oxide nanomaterials preparation. They are environmentally friendly, they have feasible experimental setup and can be easily upscaled. As a part of our broader research dealing with amino acid-nitrate processes, several samples of the Gd2O3, synthesized with four amino acids (alanine, glycine, proline, and serine) were prepared to observe an influence of amino acids on the final product's nature and morphology. All of the four samples were prepared via thermal decomposition of a transient complex formed in situ from Gd(NO3)3·6H2O and selected amino acid. The resulting products were characterized by the X-ray powder diffraction analysis, which demonstrated an influence of amino acids on the crystal structure of the final Gd2O3 nanocrystallites. The elemental composition and morphology of the samples of Gd2O3 were examined by the scanning electron microscopy with energy dispersive X-ray spectroscopy. We also measured particle size and particle size distribution as all final products (Gd2O3) had tendency to form agglomerates. Fourier-transform infrared spectroscopy and X-ray powder diffraction analysis revealed that glycine and proline, used as an organic fuel, yields the cubic structure of Gd2O3 nanocrystallites.