Nanocrystalline ytterbia powders have been synthesized using different precursors prepared by precipitation from nitrate solutions: ytterbium carbonates, oxalates, and hydroxides. The powders have been characterized by X-ray diffraction and scanning electron microscopy. The nature of the precursor has no effect on the crystallization temperature of ytterbia but influences its microstructure. The particles range in shape from spherical to platelike. The average crystallite size of the Yb₂O₃ powders is 20–25 nm. Raising the heat-treatment temperature from 600 to 1000°C increases the crystallite size to 33–46 nm. The highest thermal stability is offered by the ytterbia powders prepared through carbonate decomposition.