We report here the synthesis of TbMnO3 nanoparticles via an acrylamide gel route. XRD, TG analysis, DSC analysis, and FTIR spectroscopy are combinatively used to investigate the thermal decomposition process of precursor xerogels and the formation of TbMnO3 phase. It is demonstrated that high-phase-purity TbMnO3 nanoparticles can be prepared by using different chelating agents at a sintering temperature of 800 degrees C. SEM observation and XRD analysis reveal that the particle size and morphology of the products have a dependence on the chelating agent. The particles prepared using citric acid as the chelating agent appear to be regularly spherical in shape and highly uniform in size with a diameter of similar to 67 nm, while the sample prepared by using the chelating agent EDTA mainly consists of sphere-, ellipsoid-, and rod-like particles and exhibits a relatively broad particle size distribution with an average particle size centered around 115 nm. The use of a combination of citric acid and EDTA generally results in sphere- and ellipsoid-like particles with an average particle size between those of the samples prepared separately by using the two chelating agents. (C) 2010 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.