Uniquely structured FeSex-reduced graphene oxide (rGO) composite powders, in which hollow FeSexnanoparticles are uniformly distributed throughout the rGO matrix, were prepared by spray pyrolysis applying the nanoscale Kirkendall diffusion process. Iron oxide-rGO composite powders were transformed into FeSex-rGO composite powders by a two-step post-treatment process. Metallic Fe nanocrystals formed during the first-step post-treatment process were transformed into hollow FeSexnanoparticles during the selenization process. The FeSex-rGO composite powders had mixed crystal structures of FeSe and FeSe2 phases. A rGO content of 33% was estimated from the TG analysis of the FeSex-rGO composite powders. The FeSex-rGO composite powders had superior sodium-ion storage properties compared to those of the Fe2O3-rGO composite powders with similar morphological characteristics. The discharge capacities of the FeSex- and Fe2O3-rGO composite powders for the 200th cycle at a constant current density of 0.3 A g-1 were 434 and 174 mA h g-1, respectively. The FeSex-rGO composite powders had a high discharge capacity of 311 mA h g-1 for the 1000 th cycle at a high current density of 1 A g-1.
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