a cubic phase cu 3 sbs 3 Base thermoelectric material and preparation method thereof

A technology of thermoelectric materials and cubic phase, which is applied in the field of cubic phase Cu3SbS3-based thermoelectric materials and its preparation, can solve the problems of unavoidable monoclinic or orthorhombic stable phase transition, etc., and achieve flexible sintering method selection, stable raw materials, and low price Effect

CN107240637BInactive Publication Date: 2019-07-09HENAN POLYTECHNIC UNIV
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2019-07-09
Estimated Expiration
Not applicable · inactive patent

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Abstract

The present invention relates to a Cu 3 Sb 3 Based thermoelectric material, characterized in that it is a cubic phase with a chemical composition of Cu 3 Sb 1‑x Fe x S 3 , where x is 0.05-0.20. Its preparation method mainly comprises the following steps: 1) batching: according to chemical composition Cu 3 Sb 1‑x Fe x S 3 The stoichiometric ratio of each element in the method takes copper, antimony, iron, and sulfur as the reaction raw materials, wherein x is 0.05 to 0.30; 2) mechanical alloying: the reaction raw materials in step 1) are subjected to high-energy ball milling under an inert gas protective atmosphere , the obtained powder is subjected to spark plasma sintering or hot pressing sintering to obtain high-density and high-performance single-phase cubic phase Cu 3 Sb 3 bulk thermoelectric material. The raw material of the present invention is stable, the process is simple and controllable, the preparation cost is low, and the repeatability is good, and the prepared cubic phase Cu 3 Sb 1‑ x Fe x S 3 Thermoelectric materials have high density, pure phase, stable thermodynamic performance and excellent thermoelectric performance.
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Description

technical field

[0001] The invention belongs to the field of new energy materials, in particular to a cubic phase Cu 3 Sb 3 Based thermoelectric materials and their preparation methods. Background technique

[0002] Thermoelectric power generation technology is an energy conversion technology that uses the thermoelectric effect (Seebeck effect) of thermoelectric materials to realize direct conversion between thermal energy and electrical energy. The working efficiency and application prospects of thermoelectric devices not only depend on the performance value ZT of thermoelectric materials (the characterization parameter of the comprehensive thermoelectric performance of materials), but also are closely related to the price of raw materials and the thermodynamic stability of the materials themselves. Due to the toxicity of lead element, the current commercial medium-temperature thermoelectric material, lead telluride, is gradually withdrawing from the market. In order to ...

Examples

Embodiment 1

[0032] A preparation of cubic phase Cu 3 Sb 3 A method based on thermoelectric materials, comprising the steps of:

[0033] 1) Ingredients: According to the chemical composition Cu 3 Sb 1-x Fe x S 3 The stoichiometric ratio of each element takes copper, antimony, iron, and sulfur as the reaction raw materials, that is, the ratio of the amount of copper, antimony, sulfur, and iron is 3: (1-x): x: 3, where x = 0.10 , the mass purity of copper is better than 99.5%, the mass purity of antimony is better than 99.5%, the elemental sulfur is analytically pure, and the elemental iron purity is 99%;

[0034] 2) Mechanical alloying: Pour the reaction materials described in step 1) into a stainless steel ball mill tank, and perform high-energy ball milling under an inert gas protective atmosphere. The ball milling speed is 450rpm, the ball-to-material ratio is 20, and the ball milling time is 20h;

[0035] 3) Spark plasma sintering: put the powder obtained in step 2) into a graphit...

Embodiment 2

[0038] A preparation of cubic phase Cu 3 Sb 3 A method based on thermoelectric materials, comprising the steps of:

[0039] 1) Ingredients: According to the chemical composition Cu 3 Sb 1-x Fe x S 3 The stoichiometric ratio of each element takes copper, antimony, iron, and sulfur as the reaction raw materials, that is, the ratio of the amount of copper, antimony, sulfur, and iron is 3: (1-x): x: 3, where x = 0.05 , the mass purity of copper is better than 99.5%, the mass purity of antimony is better than 99.5%, the elemental sulfur is analytically pure, and the elemental iron purity is 99%;

[0040] 2) Mechanical alloying: Pour the reaction materials described in step 1) into a stainless steel ball mill tank, and perform high-energy ball milling under an inert gas protective atmosphere. The ball milling speed is 450rpm, the ball-to-material ratio is 20, and the ball milling time is 20h;

[0041] 3) Spark plasma sintering: put the powder obtained in step 2) into a graphit...

Embodiment 3

[0045] A preparation of cubic phase Cu 3 Sb 3 A method based on thermoelectric materials, comprising the steps of:

[0046] 1) Ingredients: According to the chemical composition Cu 3 Sb 1-x Fe x S 3 The stoichiometric ratio of each element takes copper, antimony, iron, and sulfur as the reaction raw materials, that is, the ratio of the amount of copper, antimony, sulfur, and iron is 3: (1-x): x: 3, where x = 0.20 , the mass purity of copper is better than 99.5%, the mass purity of antimony is better than 99.5%, the elemental sulfur is analytically pure, and the elemental iron purity is 99%;

[0047] 2) Mechanical alloying: Pour the reaction materials described in step 1) into a stainless steel ball mill tank, and perform high-energy ball milling under an inert gas protective atmosphere. The ball milling speed is 400 rpm, the ball-to-material ratio is 15, and the ball milling time is 25 hours;

[0048] 3) Spark plasma sintering: put the powder obtained in step 2) into a g...