The present invention relates to layered ZnSb, ZnSb nanosheets and methods for their preparation. According to the present invention, ZnSb nanosheets can be formed by efficiently peeling ZnSb, which is a polymorph layered material having a structure different from that of conventional three-dimensional ZnSb. The high quality layered ZnSb nanosheets produced by the above process can be mass-produced, and thus can be applied to thermoelectric materials. According to the present invention, a layered ZnSb structure can be made by inserting and removing Na into a ZnSb three-dimensional structure, and the newly manufactured layered structure can be easily peeled off.
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