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TiO2 - x N x nanoparticles were prepared by employing the direct amination of 6−10-nm-sized titania particles. Doping on the nanometer scale led to an enhanced nitrogen concentration of up to 8%, compared to ≤2% in thin films and micrometer-scale TiO2 powders. The synthesized TiO2 - x N x nanocrystals are catalytically active and absorb well into the visible region up to 600 nm, thus exemplifying the use of a nanostructure-based synthesis as a means of producing novel photocatalytic materials.