The rule of thumb for improving the performance of thermoelectric materials is to reduce the thermal conduction, which attributes to electron transport and phonon transport. Phonons are characterized by different wavelength, Short wavelength phonons are scattered by impurity atoms in alloyed matels, Mid- and Long wavelength phonns are scattered by the iuinterfaces. Nanostructuring can engineer the phonon transport by introduce numerous grain boundaries, thus increasing phonon scattering, further improving thermal resistance. The aim of the present study is the nano-grains of the thermoelectric material ZnSb and the correlation with thermal transport measurements. We explored cryomilling (by ball-milling powders at Cryogenic temperature) as a technique to created nano—powders of ZnSb for pressing into pellets. The effect of cryomilling flowed by hot-pressing of undoped ZnSb was investigated.