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3D MoS2/Graphene hybrid layer materials were prepared by in situ synthesizing molybdenum sulfide on 3D honeycomb-like structured graphene sheets via a hydrothermal approach. Furthermore, the composite materials were explored as counter electrodes for dye-sensitized solar cells (DSSCs). It was found that the DSSC with 3D MoS2/Graphene hybrid counter electrode exhibited a high energy conversion efficiency of 7.31%, which is larger than those with either MoS2 (2.81%) or graphene counter electrode (6.72%). The excellent electrocatalytic activity of the hybrid counter electrode was further demonstrated by cyclic voltammograms, namely, the MoS2/Graphene hybrid electrode showed higher peak current density and lower peak-to-peak separation positions than either MoS2 or graphene counter electrode.

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