Co-Fe layered double hydroxides (Co
1−xFe
x LDHs) were synthesized by a chemical co-precipitation method. It was found that the molor ratio of Co to Fe had a significant effect on the electrochemical activity. The specific capacitance of 869 F g
−1 was achieved when the molor ratio of Co to Fe was equal to 0.74:0.26. The Co
0.74Fe
0.26 LDH sample had a BET specific surface area of 202.9 m
2 g
−1 and total pore volume of 0.6 cm
3 g
−1, which led to the high liquid–solid interfacial area and further increased the utilization of the active materials. Additionally, the Co
0.74Fe
0.26 LDH electrode exhibited a good electrochemical stability with beyond 99.5% of the initial capacitance over 1000 consecutive cycles at 1 A g
−1. It is a promising electrode material for supercapacitor.
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