Although TiNb2O7 is regarded as a material with high application potential in lithium-ion batteries (LIBs) and solid-oxide fuel cells (SOFCs), it has been difficult to find suitable cost-effective conditions for synthesizing it on a commercial scale. In this study, TiNb2O7 compounds were synthesized by a solid state synthesis process. For stoichiometrically precise synthesis of the TiNb2O7 phase, the starting materials, TiO2 and Nb2O5 were taken in a 1:1 molar ratio. Activation energy and reaction kinetics of the system were investigated at various synthesis temperatures (800,1000,1200, and 1400°C) and for various holding durations (1,5,10, and 20 h). Furthermore, change in the product morphology and particle size distribution were also evaluated as a function of synthesis temperature and duration. Additionally, quantitative phase analysis was conducted using the Rietveld refinement method. It was found that increases in the synthesis temperature and holding time lead to increase in the mean particle size from 1 to 4.5 μm. The reaction rate constant for the synthesis reaction was also calculated.