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In this work, p-type 20%Bi2Te3–80%Sb2Te3 bulk thermoelectric (TE) materials were prepared by mechanical deformation (MD) of pre-melted ingot and by mechanical alloying (MA) of elemental Bi, Sb, and Te granules followed by cold-pressing. The dependence on annealing time of changes of microstructure and TE properties of the prepared samples, including Seebeck coefficient, electrical resistivity, thermal conductivity, and figure-of-merit, was investigated. For both samples, saturation of the Seebeck coefficient and electrical resistivity were observed after annealing for 1 h at 380°C. It is suggested that energy stored in samples prepared by both MA and MD facilitated their recrystallization within short annealing times. The 20%Bi2Te3–80%Sb2Te3 sample prepared by MA followed by heat treatment had higher a Seebeck coefficient and electrical resistivity than specimens fabricated by MD. Maximum figures-of-merit of 3.00 × 10−3/K and 2.85 × 10−3/K were achieved for samples prepared by MA and MD, respectively.

The effects of mechanical deformation and subsequent annealing on the thermoelectric properties and microstructure have been investigated for p-type (Bi0.25Sb0.75)2Te3 alloys prepared by melting followed by quenching. The mechanically deformed pellets were prepared by repetition of cold-pressing of quenched samples at room temperature. Cold-pressed pellets were then annealed at 300°C in vacuum, and the thermoelectric properties and microstructure were traced through the course of the heat treatment. For the heavily deformed samples, the Seebeck coefficient rapidly increased at the very early stage of annealing and did not change as the annealing time increased, due to recrystallization of a new δ-phase which equilibrated at the annealing temperature of 300°C (δ300-phase). At the initial stage of annealing (recovery stage), the electrical resistivity sharply increased, probably due to the interaction of antistructural defects with vacancies produced during the cold-pressing treatment. However, for the lightly deformed samples, recrystallization occurred only at some portion of the grain boundaries, and the newly generated δ300-phase slowly replaced the original, as-solidified δingot-phase.