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Lanthanide oxide nanocrystallites have gained a lot of attention due to their diverse use for potential applications and for this reason it is very important to find a suitable preparation method that would be economically inexpensive and easy to implement. The chapter describes the preparation of gadolinium oxide nanocrystallites (nano Gd 2 O 3 ) through thermal decomposition of a complex formed by Gd(NO 3 ) 3 ·6H 2 O and glycine. Decomposition of the complex occurs at temperatures about (250 ± 10)C. An ultrafine white powder of the gadolinium oxide nanocrystallites was obtained. The resulting nanocrystallites were characterized by X-ray powder diffraction analysis, which revealed the size of the gadolinium oxide nanocrystallites equal to 10 nm. The morphology of the gadolinium oxide nanocrystallites was examined by scanning electron microscopy. The elemental composition of the product was confirmed by EDS analysis.

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