Yttrium oxide (Y2O3) and ytterbium (Yb)-doped Y2O3 particles were synthesized via the sol-gel method from the aqueous solution of their nitrate salts. The synthesized powders were then deposited on Corning glass substrates using an electron beam evaporation technique to examine the growth morphology of the thin films. The effect of the Yb dopant concentration on the microstructure and morphology of the Y2O3 powders and thin films was investigated using various characterization techniques. The synthesized powders and fabricated thin films have body-centered cubic structures with space group Ia-3. Based on the X-ray peak broadening, crystallite size and lattice parameters were evaluated with the Williamsom-Hall and Cohen-Wagner methods. The lattice parameter and crystallite size decrease with increasing Yb concentration. The intensities of the Raman peaks decrease due to microstructural disorder caused by the increase in the Yb dopant concentration. The band gap values of the powders also decrease depending on the dopant concentration, similar to the lattice parameter and crystallite size. While the synthesized powders have a sponge-like morphology, they exhibit different morphological structures depending on the dopant concentration when converted into thin films.