Ceria-zirconia　solid　solutions　and　barium　sulfate　with　high　thermal　stability　and　large　surface　areas　are　of　importance　in　catalytic　applications.　High-surface-area　Ce0.6Zr0.4O2　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　Ce0.6Zr0.4O2　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　15~30　nm,　and　their　BET　surface　areas　are　45~64　m2/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　80~200　nm　and　their　BET　surface　areas　are　6~11　m2/g.