MnCo 2 O 4 octahedral structure with edge length about 500 nm was successfully synthesized by a simple hydrothermal route. With the use of NaOH, the chemical potential and the rate of ionic motion in the precursor solution were controlled, and the particle size was limited. The magnetization measurements revealed that the products exhibited ferrimagnetic characteristics with different saturation magnetization and coercivity at different measuring temperatures. In addition, the as-prepared MnCo 2 O 4 as anodes for lithium-ion batteries (LIBs) exhibited a reversible capacity of 1180 mA·h/g and 1090 mA·h/g at current density of 0.1 C and 1 C, respectively. The excellent cyclic performance was confirmed because the value of reversible capacity for MnCo 2 O 4 was 618 mA·h/g after 50 cycles at 0.1 C. Owing to the good rate performance, MnCo 2 O 4 octahedral products were suggested to have a promising application as anode material for LIBs.