Preparation method of Se doped skutterudite thermoelectric material

A technology of thermoelectric material and skutterudite, which is applied in the manufacture/processing of thermoelectric devices, and lead wire materials of thermoelectric device nodes, etc., can solve the problems of uneven doping of skutterudite thermoelectric materials and deviation of thermoelectric properties of thermoelectric materials, etc. Achieve the effect of excellent thermoelectric performance, excellent thermoelectric performance and convenient operation

Active Publication Date: 2018-08-28
UNIV OF JINAN
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Problems solved by technology

At present, Se-doped skutterudite thermoelectric materials can also improve the thermoelectric figure of merit of skutterudite (J Mater Sci Mater in Electronics, 29, 2018, 1264-1268; J Alloys Compd, 647, 2015, 295-302), However, whether the melting method or the solid-state reaction method is used, Se segregation will be caused, which will cause uneven doping of skutterudite thermoelectric materials, resulting in deviations in the thermoelectric properties of thermoelectric materials.

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  • Preparation method of Se doped skutterudite thermoelectric material
  • Preparation method of Se doped skutterudite thermoelectric material

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Embodiment 1

[0029] Using high-purity (99.99%) cobalt powder (Co) and antimony powder (Sb) as raw materials, the stoichiometric ratio is 1:2.98, and the Sb-deficient CoSb is prepared by melting-annealing process. 3-x Thermoelectric material powder, x=0.02. The melt annealing process is as follows: mix cobalt powder (Co) and antimony powder (Sb), heat up to 1040°C and melt for 24 hours, then anneal the molten metal at 620°C for 96 hours, and grind the annealed product to obtain Sb-deficient CoSb 3-x Thermoelectric material powder.

[0030] The resulting Sb-deficient CoSb 3-xThe thermoelectric material powder was put into a mortar and ground to 80 μm, and the obtained powder was evenly spread in a graphite crucible. Take a quartz tube, put a selenium block into the bottom of the quartz tube, then put a graphite crucible on top of the selenium block, and vacuum seal the quartz tube. After fusing, the vacuum degree in the quartz tube is 5Pa. Place the vacuum-sealed quartz tube vertically i...

Embodiment 2

[0035] Using high-purity (99.99%) cobalt powder (Co) and antimony powder (Sb) as raw materials, the stoichiometric ratio is 1:2.96, and the Sb-deficient CoSb is prepared by melting-annealing process. 3-x Thermoelectric material powder, x=0.04. The melt annealing process is as follows: mix cobalt powder (Co) and antimony powder (Sb), heat up to 1040°C and melt for 24 hours, then anneal the molten metal at 620°C for 96 hours, and grind the annealed product to obtain Sb-deficient CoSb 3-x Thermoelectric material powder.

[0036] The resulting Sb-deficient CoSb 3-x The thermoelectric material powder was put into a mortar and ground to 150 μm, and the obtained powder was evenly spread in a graphite crucible. Take a quartz tube, put a selenium block into the bottom of the quartz tube, then put a graphite crucible on top of the selenium block, and vacuum seal the quartz tube. After fusing, the vacuum degree in the quartz tube is 10Pa. Place the vacuum-sealed quartz tube verticall...

Embodiment 3

[0040] Using high-purity (99.99%) cobalt powder (Co) and antimony powder (Sb) as raw materials, according to the stoichiometric ratio of 1:2.9, the Sb-deficient CoSb was prepared by melting-annealing process 3-x Thermoelectric material powder, x=0.1. The melt annealing process is as follows: mix cobalt powder (Co) and antimony powder (Sb), heat up to 1040°C and melt for 24 hours, then anneal the molten metal at 620°C for 96 hours, and grind the annealed product to obtain Sb-deficient CoSb 3-x Thermoelectric material powder.

[0041] The resulting Sb-deficient CoSb 3-x The thermoelectric material powder was put into a mortar and ground to 200 μm, and the obtained powder was evenly spread in a graphite crucible. Take a quartz tube, put a selenium block into the bottom of the quartz tube, then put a graphite crucible on top of the selenium block, and vacuum seal the quartz tube. After fusing, the vacuum degree in the quartz tube is 8Pa. Place the vacuum-sealed quartz tube ver...

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Abstract

The invention discloses a preparation method of an Se doped skutterudite thermoelectric material. A fusion-annealing method is adopted to prepare Sb-omitted CoSb3-x thermoelectric material powder; thepowder is subjected to selenium permeation treatment; then, quick hot-pressing sintering is carried out to obtain a final product. According to the preparation method, a selenium permeation technology is used for doping the skutterudite thermoelectric material, so as to favorably realize the even doping of the Se element and avoid the uneven doping of a traditional method, and then, Se doped skutterudite thermoelectric material blocks are prepared through a quick hot-pressing sintering technology. The preparation method has the advantages of convenient and simple technology, good repeatability, high controllability and convenience in operation, the accurate control on an Se doping amount is realized through controlling technical parameters of Se permeation, and the preparation method canbe used for large batch production and has a good industrial prospect. The prepared Se doped skutterudite thermoelectric material has excellent thermoelectric properties and is suitable for mass production.

Description

technical field [0001] The invention relates to a method for preparing a doped cobalt ore thermoelectric material, in particular to a method for preparing a Se-doped skutterudite thermoelectric material, and belongs to the technical field of thermoelectric material preparation. Background technique [0002] Thermoelectric materials are energy materials that can directly convert electrical energy and heat energy. Based on the current background of a large number of resource and energy waste, environmental pollution, and excessive production capacity, thermoelectric materials have unlimited development space. Thermoelectric materials have achieved good application results in the aerospace field. In real life, a large amount of industrial waste heat and automobile exhaust heat are flooding around our production and living activities. Therefore, the emergence of thermoelectric materials provides opportunities for recycling these excess energy waste. On the other hand, in the fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L35/34H01L35/16
CPCH10N10/852H10N10/01
Inventor 赵德刚吴迪薄琳王琳
Owner UNIV OF JINAN
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