Single-phase b-Zn 4 Sb 3 materials were prepared by mechanical grinding (MG). Source materials for the Zn 4 Sb 3 ingots were prepared using three different processes after the direct melting of constituent elements. In process 1, the ingot was obtained by quenching the melt in water within an evacuated quartz ampoule. In process 2, the ingot was heat-treated for 100 h at 723 K after process 1. In process 3, the ingot was heat-treated for a total of 200 h in two stages at 723 K and 673 K after process 1. The resultant ingots were mechanically ground and sintered at 623 K by hot pressing. The sintered materials were characterized by x-ray diffraction, differential thermal analysis (DTA), and thermoelectric property measurements. The thermal conductivity of the sintered materials was 0.88 W m À1 K À1 at room temperature, being slightly lower than that reported for the materials prepared by a conventional method. Results indicate that the dimensionless figure of merit of the single-phase b-Zn 4 Sb 3 ranged from 1.06 to 1.31 at 573 K.