Highly crystalline CaTaO2N nanoparticles possessing large specific surface areas were investigated as photocatalysts for the decomposition of methyl orange. Two different Ca2Ta2O7 precursors were synthesized by classical solid state synthesis and a hydrothermal soft-chemistry approach, respectively. In both cases, nitridation was carried out by thermal ammonolysis. The obtained CaTaO2N samples were compared with respect to their optical, thermal and morphological properties as well as their photocatalytic activities. In particular, the influence of ammonolysis temperature on the photocatalytic properties was studied. Using hydrothermally synthesized Ca2Ta2O7, phase pure CaTaO2N was obtained already at a relatively low ammonolysis temperature of 860 degrees C. Morphological investigations show that the CaTaO2N samples from the hydrothermally synthesized precursor consist of single-crystalline particles of 45-70 nm diameter with high specific surface areas between 12 and 19 m(2) g(-1), depending on ammonolysis temperature. A considerable photocatalytic activity for methyl orange degredation was found for the nanoscaled CaTaO2N particles prepared at lower ammonolysis temperatures. Using CoOx as co-catalyst, a further strong enhancement of the methyl orange decomposition by a factor 5-10 was achieved. (C) 2015 Elsevier Ltd. All rights reserved.