Three-dimensionally　ordered　macroporous　(3DOM)　praseodymium　oxide　and　terbium　oxide　with　mesoporous　walls　and　cubic　crystal　structures　have　been　successfully　fabricated　with　polymethyl　methacrylate　(PMMA)　as　hard　template　and　F127,　sucrose,　and　L-lysine　as　surfactant.　Physicochemical　properties　of　the　materials　were　characterized　by　means　of　numerous　techniques.　It　is　shown　that　the　Pr6O11　and　Tb4O7　samples　displayed　a　3DOM　architecture　with　polycrystalline　wormhole-like　mesoporous　walls.　The　nature　of　surfactant　and　solvent　and　calcination　condition　had　important　effects　on　the　pore　structure　and　surface　area　of　the　final　product.　The　introduction　of　surfactant　and　the　partial　carbonization　of　sucrose　or　L-lysine　favored　the　enhancement　in　surface　area　of　the　3DOM-structured　materials,　with　the　3DOM　Pr6O11　and　Tb4O7　samples　derived　with　F127　showing　the　highest　surface　areas　of　32.0　and　25.2　m(2)/g,　respectively.　The　low-temperature　reducibility　of　the　Pr6O11　and　Tb4O7　samples　decreased　according　to　the　sequences　of　Pr6O11-F127　＞　Pr6O11-Sucrose　＞　Pr6O11-Lysine　and　Tb4O7-F127　＞　Tb4O7-Sucrose　＞　Tb4O7-Lysine,　coinciding　with　the　order　in　surface　oxygen　vacancy　density.　The　improved　physicochemical　properties　associated　with　the　generation　of　3DOM　skeletons　and　wormhole-like　mesoporous　walls　rendered　the　Pr6O11-F127　and　Tb4O7-F127　samples　to　perform　the　best　in　the　oxidation　of　CO.　(C)　2014　Elsevier　B.V.　All　rights　reserved.