La3+ and Co2+ co-doped titania nanoparticles were prepared from reacting TiOSO4, La(NO3)3 and Co(NO3)2 with NH4OH in water/Triton X-100/n-hexanol/cyclohexane microemulsions. The structure, surface morphology and the specific surface area of the samples were characterized. The photocatalytic efficiency of as-prepared TiO2 was tested by photodegrading methyl orange. The results showed that doping with La3+ and Co2+ could suppress the growth of TiO2 grains and increase the specific surface area; When the calcination temperature increased from 300°C to 900°C, the average crystallite size of the particles increased from 7.3nm to 35.6 nm andthe specific surface area of the particles decreased rapidly from 205.5m2/g to 41.2m2/g. The synthesized amorphous particles wer transformed into anatase phase at 300°C, and further into rutile phase at 900°C. UV-Vis diffuse reflectance spectrum revealed that La3+ and Co2+ co-doped TiO2 absorbed UV light and visible light, while pure TiO2 could only absorb UV light. In the experiments of photodegrading methyl orange, it was proved that La3+ and Co2+ co-doped TiO2 had high photocatalytic activity under UV light and visible light, while pure TiO2 showed photocatalytic activity just under UV light.