The invention belongs to the technical field of
new materials, and discloses a preparation method of high-purity
bismuth antimonide, which comprises the following steps: sealing an
antimony elementary substance and a
bismuth elementary substance in a vacuumized container, and heating for melting reaction to prepare the high-purity
bismuth antimonide, the
molar ratio of the
antimony elementary substance to the bismuth elementary substance is 1: 1; the heating and melting are carried out in two steps: firstly heating to a first temperature and reacting for a period of time, then heating to a second temperature and reacting for a period of time, and keeping the container in a shaking state at the second temperature stage; the first temperature is higher than the
melting point temperature of bismuth and lower than the
melting point temperature of
antimony; the second temperature is higher than the
melting point temperature of antimony. The reaction is carried out through two-stage heating, the
reaction temperature is controlled to be below the
melting point temperature of antimony, antimony volatilization is avoided, after most of the reaction is completely carried out, heating is carried out, the reaction is thoroughly carried out, the
vapor pressure in the vacuum cavity is reduced, antimony loss is avoided, and therefore the product purity can be effectively improved. Meanwhile, the invention further provides the high-purity bismuth
antimonide prepared on the basis of the method.