In this work, a fast method for synthesizing TiNb 2 O 7 nanoparticles was developed by combining colloidal sol-gel and microwave-assisted hydrothermal synthesis. The synthesis conditions and the subsequent thermal treatments were evaluated analyzing their effect on morphological, structural, and photocatalytic properties of the synthesized nanoparticles. The results indicated that the hybrid synthesis requires heating at temperature as low as 180°C for only 10 minutes. Therefore, this process is a feasible alternative method for obtaining nanoparticles with sizes ranging from 10 to 50 nm. Subsequent thermal treatments led to the direct crystallization of the TiNb 2 O 7 in the monoclinic phase, observing a direct correlation between the crystallinity and the photocatalytic activity: the higher the better. K E Y W O R D S microwave-assisted synthesis, nanoparticles, sol-gel, TiNb 2 O 7 How to cite this article: Falk GS, Rodrigues Neto JB, Borlaf M, Gómez SY, Novaes de Oliveira AP, Hotza D. Fast microwave-assisted hydrothermal synthesis of TiNb 2 O 7 nanoparticles. Int J Ceramic Eng Sci.