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In this study, we demonstrate the feasibility of Bi-doped tetrahedrite Cu 12 Sb 4-x Bi x S 13 (x = 0.02-0.20) synthesis in an industrial eccentric vibratory mill using Cu, Sb, Bi and S elemental precursors. High-energy milling was followed by spark plasma sintering. In all the samples, the prevailing content of tetrahedrite Cu 12 Sb 4 S 13 (71-87%) and famatinite Cu 3 SbS 4 (13-21%), together with small amounts of skinnerite Cu 3 SbS 3 , have been detected. The occurrence of the individual Cu-Sb-S phases and oxidation states of bismuth identified as Bi 0 and Bi 3+ are correlated. The most prominent effect of the simultaneous milling and doping on the thermoelectric properties is a decrease in the total thermal conductivity ( κ ) with increasing Bi content, in relation with the increasing amount of famatinite and skinnerite contents. The lowest value of κ was achieved for x = 0.2 (1.1 W m -1 K -1 at 675 K). However, this sample also manifests the lowest electrical conductivity σ , combined with relatively unchanged values for the Seebeck coefficient ( S ) compared with the un-doped sample. Overall, the lowered electrical performances outweigh the benefits from the decrease in thermal conductivity and the resulting figure-of-merit values illustrate a degradation effect of Bi doping on the thermoelectric properties of tetrahedrite in these synthesis conditions.

Bismuth Doping in Nanostructured Tetrahedrite: Scalable Synthesis and Thermoelectric Performance