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A preparation method for antimonide molybdenum base thermoelectric material

A technology of molybdenum antimonide-based and thermoelectric materials is applied in the preparation of molybdenum antimonide-based materials and the field of preparation of molybdenum antimonide-based thermoelectric materials, and can solve the problems of undesired practical application, unsuitable for large-scale production, troublesome practical operation, and the like, Achieve low cost, inhibit raw material volatilization, and save energy.

Active Publication Date: 2008-07-09
江苏先进无机材料研究院
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Problems solved by technology

[0004] D. Badurski et al. synthesized single-crystal molybdenum antimonide (Solid State Communications, 123, 283, 2002) by using the peritectic reaction between metal molybdenum and liquid antimony. Although a pure molybdenum antimonide single crystal was obtained, the process was complicated. And the output is very low, which brings no small trouble to actual operation, and is not suitable for large-scale production; Enkhtsetseg Dashjav etc. have made molybdenum antimonide (J.Mater.Chem.12,345,2002) with multiple reactions, and this method first It needs to carry out solid-state reaction, heat preservation at 750°C for 10 days, and then anneal for 7-10 days at the corresponding temperature for a long time. The process is complicated and the preparation cycle is long; Solid-state reaction was carried out at 750°C for 7 days, quenched in cold water, and then annealed at 750°C for 7 days. Although a single phase of molybdenum antimonide was finally obtained (Journal of Alloys and Compounds 427, 325, 2007), the process time It is very long and consumes a lot of energy, so it is not advisable for practical use

Method used

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  • A preparation method for antimonide molybdenum base thermoelectric material
  • A preparation method for antimonide molybdenum base thermoelectric material
  • A preparation method for antimonide molybdenum base thermoelectric material

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Embodiment 1

[0034] Example 1: Mo 3 Sb 7 material preparation

[0035] A. The high-purity metal elemental raw materials Mo (99%) and Sb (99.999%) are formulated according to the molar ratio of Mo:Sb=3:7, mixed evenly, put into the arc melting furnace, and filled with high Melting with pure argon, the time is 2-3 minutes, repeated 2-3 times. Grind the obtained material into powder and sinter with SPS at about 580°C (heating rate is 50°C / min, heat preservation is 5-10 minutes, pressure is 80-100MPa.

[0036] B. With high-purity metal elemental raw materials Mo (99%) and Sb (99.999%), according to the molar ratio batching of Mo: Sb=3: 7, after mixing evenly, tablet (ф10 mold, pressure is 50-60MPa), Vacuum packaged in a quartz tube (vacuum degree less than 10Pa), placed in a muffle furnace for solid phase reaction at 750°C for 7 days (heating rate 2-3°C / min), and repeated solid phase reaction 2-3 times. Finally, the obtained material is ground into powder, and hot-pressed at 720-750° C. an...

Embodiment 2

[0037] The Mo obtained by the two methods is illustrated from the X-ray diffraction pattern (Fig. 1). 3 Sb 7 The materials are all in pure phase, and the ZT value of the material prepared by the method provided by the invention is higher than that of the material prepared by the traditional method (Fig. 2). Example 2: Mo 3 Sb 5.2 Te 1.8 material preparation

[0038] A. The high-purity metal elemental raw materials Sb (99.999%) and Te (99.999%) are mixed according to the molar ratio of 2:3, and packed into a quartz tube in a vacuum (vacuum degree is less than 10Pa), at about 650°C-700°C Melt for 6-12 hours, then quench in water. Will get Sb 2 Te 3 With the elemental Mo powder of 99% purity and Sb (99.999%) powder, be Mo: Sb: The amount batching of Te=3: 5.2: 1.8 by final chemical formula molar ratio, put into the electric arc melting furnace after mixing, after vacuumizing ( Vacuum degree is less than 10Pa) filled with high-purity argon for smelting, the time is 2-3 min...

Embodiment 3

[0040] Example 3: Mo 3 Sb 6 Preparation of Se materials

[0041] A. The high-purity metal elemental raw materials Sb (99.999%) and Se (99.999%) are mixed according to the molar ratio of 2:3, and packed into a quartz tube in a vacuum (vacuum degree is less than 10Pa), at about 650°C-700°C Melt for 6-12 hours, then quench in cold water. will get Sb 2 Se 3 With 99% purity elemental Mo powder and Sb (99.999%) powder according to the final chemical formula molar ratio of Mo: Sb: Se = 3: 6: 1 batching, after mixing evenly put into the arc melting furnace, vacuumize and fill Enter high-purity argon for smelting, the time is 2-3 minutes, repeat 2-3 times. The obtained material is ground into powder and sintered with SPS at about 580°C (heating rate is 50°C / min, heat preservation is 5-10 minutes, pressure is 80-100MPa).

[0042] B. with high-purity metal elemental raw material Mo (99%), Sb (99.999%) and Se (99.999%), according to the molar ratio batching of Mo: Sb: Se=3: 6: 1, af...

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Abstract

The invention relates to a doping molybdenum antimonide-based thermoelectric material and the preparation method, which is characterized in that the invention adopts arc melting and discharging plasma rapid sintering method for combination. The preparation method which is provided by the invention is the arc melting and the discharging plasma rapid sintering; Sb and Te / Se are firstly melted to form Sb2Te3Sb2Se3 and then are treated with the arc melting with the stoichiometric ratio of Mo and Sb; finally, the discharging plasma rapid sintering technology is introduced for preparing a dense single-phase material. The invention provides the rapid, simple and effective preparation method of the molybdenum antimonide-based thermoelectric material, which has good practical prospect.

Description

technical field [0001] The invention relates to a method for preparing a molybdenum antimonide-based thermoelectric material, more precisely, relates to a method for preparing a molybdenum antimonide-based material with high symmetry and good thermoelectric performance, and belongs to the field of thermoelectric materials. Background technique [0002] Thermoelectric materials (also known as thermoelectric materials) are functional materials that convert heat and electricity. It has the characteristics of small size, high reliability, and long life. It plays an important role in technical fields such as aviation, military affairs, and waste heat power generation. . Now people are accustomed to use the dimensionless performance index ZT (ZT = α 2 σT / K, where α is the Seebeck coefficient; σ is the electrical conductivity; κ is the thermal conductivity, κ=electronic thermal conductivity + lattice thermal conductivity, T is the absolute temperature) as an important measure of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L35/34C22C1/02C22C1/04B22F9/04B22F3/16B22F3/105H10N10/01
CPCY02P10/25
Inventor 陈立东史啸亚柏胜强裴艳中吴汀
Owner 江苏先进无机材料研究院
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