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Composite electrocatalysts of carbon and metals or metal compounds with homogeneous active sites can be obtained through the carbonization of metal organic framework (MOF) materials under inert atmosphere. In this work, a three-phase composite electrocatalysts NiFe2O4/Ni@C were prepared via pyrolysis from self-assembled MOF nanosheets aggregates. The excellent electrocatalytic activity of the obtained electrocatalysts with various Ni:Fe ratios is demonstrated. Especially, the NiFe2O4/Ni@C sample with the mole ratio of Ni:Fe = 1:1 can use the overpotential (η) of 330 and 423 mV to drive 10 and 50 mA cm−2 respectively. After 80 000 s/22 h, the current density could retained 90% of the initial current density. The excellent activity and stability of the electrocatalysts are attributed to nickel and iron ions with uniform dispersion at atomic level in the NiFe2O4 phase and the synergistic effect of nickel and NiFe2O4 nanoparticles with amorphous carbon atoms or nanoparticles around. [ABSTRACT FROM AUTHOR]