Abstract: Ceria-zirconia solid solutions and barium sulfate with high thermal stability and large surface areas are of importance in catalytic applications.High-surface-area _0.6Zr_0.4O₂ solid solution nano-particles and BaSO₄ micro/nano-particles were synthesized by using hydrothermal synthesis method with hexadecyl trimethyl ammonium bromide (CTAB) , triblock poly (ethylene oxide) -poly (propylene oxide) -poly (ethylene oxide) (P123) and polyethylene glycol (PEG) as surfactants, and investigated by means of the techniques such as X-ray diffractometer, nitrogen adsorption-desorption, scanning electron microscopy, high resolution transmission electron microscopy and selected area electron diffraction. It is found that the _0.6Zr_0.4O₂ solid solutions synthesized with CTAB, P123 and PEG possess approximate spherical-shaped surface morphology with single crystalline and polycrystalline face-centered cubic-type structure and their particle diameter distributed in the range of 15~30nm, and their BET surface areas are 45~64m²/g.The BaSO₄ samples obtained with PEG and P123 as surfactants are well-ordered polyhedral morphology nano-particles with orthorhombic single-crystalline structure which side length is 80~200nm and their BET surface areas are 6~11m²/g.