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In this study, we prepared hexagonal and monoclinic phases of La 2 O 2 CO 3 nanoparticles by different wet preparation methods and investigated their phase-related CO 2 behavior through field-emission scanning microscopy, high-resolution transmission electron microscopy, Fourier transform infrared, thermogravimetric analysis, CO 2 -temperature programmed desorption, and linear sweeping voltammetry of CO 2 electrochemical reduction. The monoclinic La 2 O 2 CO 3 phase was synthesized by a conventional precipitation method via La(OH)CO 3 when the precipitation time was longer than 12 h. In contrast, the hydrothermal method produced only the hexagonal La 2 O 2 CO 3 phase, irrespective of the hydrothermal reaction time. The La(OH) 3 phase was determined to be the initial phase in both preparation methods. During the precipitation, the La(OH) 3 phase was transformed into La(OH)CO 3 owing to the continuous supply of CO 2 from air whereas the hydrothermal method of a closed system crystallized only the La(OH) 3 phase. Based on the CO 2 -temperature programmed desorption and thermogravimetric analysis, the hexagonal La 2 O 2 CO 3 nanoparticles (HL-12h) showed a higher surface CO 2 adsorption and thermal stability than those of the monoclinic La 2 O 2 CO 3 (PL-12h). The crystalline structures of both La 2 O 2 CO 3 phases predicted by the density functional theory calculation explained the difference in the CO 2 behavior on each phase. Consequently, HL-12h showed a higher current density and a more positive onset potential than PL-12h in CO 2 electrochemical reduction.

Hexagonal and Monoclinic Phases of La2O2CO3 Nanoparticles and Their Phase-Related CO2 Behavior