A novel heterostructure of NiO/Ni3S2 nanoflake is synthesized and composited with carbon nanofibers (CNF) membrane. NiO/Ni3S2 nanoflakes are homogeneously dispersed in CNF network, herein, NiO/Ni3S2 like leaf and CNF like branch. Carbon nanofibers network efficiently prevents the pulverization and buffers the volume changes of NiO/Ni3S2, meanwhile, NiO/Ni3S2 nanoflakes through the conductive channels of carbon nanofibers own improved Li+ diffusion ability and structural stability. The capacity of NiO/Ni3S2/CNF reaches to 519.2 mA g (1) after 200 cycles at the current density of 0.5 A g 1 while NiO/Ni3S2 fades to 71 mAh g (1) after 40 cycles. Owing to the synergetic structure, the resultant binder-free electrode NiO/Ni3S2/carbon nanofibers shows an excellent reversible lithium storage capability. (C) 2018 Elsevier B.V. All rights reserved.