Two methods for preparing mesoporous CeO2/Au nanocomposites were compared: template synthesis and photochemical modification of fibrous cerium(IV) oxide with gold nanoparticles. The composition, structure, morphology of the obtained nanocomposites, as well as the specific surface area and pore size distribution were studied by a complex of physicochemical methods: X-ray phase analysis, X-ray spectral microanalysis, scanning electron microscopy, low-temperature nitrogen adsorption, and electron spectroscopy. The catalytic properties of the obtained nanocomposites were studied in methyl orange photodegradation reactions. It is shown that the CeO2/Au catalyst obtained by the photochemical modification method has the highest photocatalytic activity both under the action of UV and visible light.