Multicomponent metal sulfide materials with a yolk–shell structure and a single phase were studied for the first time as anode materials for sodium-ion batteries. Yolk–shell-structured Fe–Ni–O powders with a molar ratio of iron and nickel components of 1/1 were prepared via one-pot spray pyrolysis. The prepared Fe–Ni–O powders were transformed into yolk–shell-structured (Fe 0.5 Ni 0.5 ) 9 S 8 solid-solution powders via a sulfidation process. The initial discharge and charge capacities of the (Fe 0.5 Ni 0.5 ) 9 S 8 powders at a current density of 1 A·g −1 were 601 and 504 mA·h·g −1 , respectively. The discharge capacities of the (Fe 0.5 Ni 0.5 ) 9 S 8 powders for the 2 nd and 100 th cycle were 530 and 527 mA·h·g −1 , respectively, and their corresponding capacity retention measured from the 2 nd cycle was 99%. The (Fe 0.5 Ni 0.5 ) 9 S 8 powders had high initial discharge and charge capacities at a low current density of 0.1 A·g −1 , and the reversible discharge capacity decreased slightly from 568 to 465 mA·h·g −1 as the current density increased from 0.1 to 5.0 A·g −1 . The synergetic effect of the novel yolk–shell structure and the multicomponent sulfide composition of the (Fe 0.5 Ni 0.5 ) 9 S 8 powders resulted in excellent sodium-ion storage performance.
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