Abstract The thermal decomposition process of LiHC 2 O 4 ·H 2 O from 30 to 600 °C was investigated by the thermogravimetric and differential scanning calorimetry (TG‐DSC). The phases decomposited at different temperature were characterized by X‐ray diffraction (XRD), which indicated the decompositions at 150, 170, and 420 °C, relating to LiHC 2 O 4 , Li 2 C 2 O 4 , Li 2 C 2 O 4 , and Li 2 CO 3 , respectively. Reaction mechanisms in the whole sintering process were determined, and the model fitting kinetic approaches were applied to data for non‐isothermal thermal decomposition of LiHC 2 O 4 ·H 2 O; finally, the kinetic parameters of each reaction were also calculated herein.