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The mechanochemical synthesis of PbTe nanostructures via the high-energy milling (HEM) process is proposed, as a synergistic approach, to minimize the thermal conductivity of this semiconductor material at room temperature. In this study, the effect of process control agent (PCA) addition on the microstructure and thermal properties of the as-milled PbTe nanostructures was also investigated. The synthesis design is based on a solid-state technique which allows enhancing the grain boundary scattering and consequently, decreases the thermal conductivity in the PbTe nanostructures. Moreover, the challenging part is the formation of coarse particles with embedded quantum dots and nanoparticles, which are expected to scatter long- and mid-wavelength phonons. In this sense, via the HEM-process, it is feasible to activate other phonon scattering modes by introducing rough-surfaced grains and nanoroughness to the particle surfaces. Overall, the thermal conductivity is decreased in the PbTe nanostructures by two means; namely, adding scattering processes and phonon group velocity, which were heightened due to the PCA added during milling. To elucidate the role of these components of the phonon thermal conductivity, atomic force microscopy and high-resolution transmission electron microscopy were used. On the other hand, photoacoustic (PA) and photopyroelectric (PP) techniques were applied to study the thermal properties of the PbTe nanostructures obtained by the HEM-process. The total thermal conductivity values of the PbTe nanostructures obtained by the PA and PP techniques were at least a half lower (1.06 W m−1 K−1) than that of bulk PbTe value counterpart (∼2.13 W m−1 K−1) and lower than those from PbTe nanomaterials (ranging from 1.5 to 2.2 W m−1 K−1) obtained via other means. The thermal conductivity values of the as-milled PbTe nanostructures were closely related to the carrier concentration experimental findings. We inferred that this strategy can be widely applicable to enhance existing thermoelectric compounds into their nanoforms by a scalable and a simple low-cost route.