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Filled antimony-based square cobalt mineral compound and its production

A compound and skutterudite technology, which is applied in the field of preparation of filled antimony-based skutterudite thermoelectric materials, can solve the problems of low cost, no filled antimony-based skutterudite compound, etc., achieves low cost, avoids peritectic Decomposition temperature, the effect of reducing production cost

Inactive Publication Date: 2007-11-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrothermal / solvothermal method is a novel preparation method for low-temperature synthetic materials. Due to its low cost, large output and high efficiency, it has been widely used in the preparation of nanomaterials; however, no hydrothermal / solvothermal method has yet been used. A report on filled antimony-based skutterudite compounds

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, a preparation method of filled antimony-based skutterudite compound, the following steps are carried out in sequence:

[0020] 1), the analytically pure LaCl 3 ·nH 2 O, CoCl 2 ·6H 2 O, SbCl 3 And high-purity tellurium (Te) powder (>99.99%), according to La 0.3 co 4 Sb 11.5 Te 0.5 Stoichiometric batching, each 0.6mmol LaCl 3 ·nH 2 O, 8 mmol CoCl 2 ·6H 2 O, 23 mmol SbCl 3 and 1 mmol tellurium powder, the above four raw materials were dissolved in 400 mL of absolute ethanol as a base material, and mixed uniformly to obtain a mixed solution.

[0021] 2) Place the prepared mixed solution in an autoclave (WDF-0.5 type), and the volume of the autoclave is 500mL. Then add the reducing agent NaBH in the autoclave 4 100mmol, and then immediately seal the autoclave. The autoclave was heated to 240°C and reacted for 24 hours.

[0022] 3), after the reaction is finished, the autoclave is naturally cooled to room temperature, and the reaction product is...

Embodiment 2

[0025] Embodiment 2, a preparation method of filled antimony-based skutterudite compound, the following steps are carried out in sequence:

[0026] 1), the analytically pure LaCl 3 ·nH 2 O, CoCl 2 ·6H 2 O, SbCl 3 and Na 2 TeO 3 , press La 0.3 co 4 Sb 11.5 Te 0.5 Stoichiometric batching, each 0.6mmol LaCl 3 ·nH 2 O, 8 mmol CoCl 2 ·6H 2 O, 23 mmol SbCl 3 and 1 mmol Na 2 TeO 3 , the above four raw materials were dissolved in 250mL of benzene as a base material, and mixed uniformly to obtain a mixed solution.

[0027]2) Place the prepared mixed solution in an autoclave (WDF-0.5 type), and the volume of the autoclave is 500mL. Then add the reducing agent NaBH in the autoclave 4 160mmol and organic complexing agent ethylenediaminetetraacetic acid 16mmol, then immediately seal the autoclave. The autoclave was heated to 300°C and reacted for 10 hours.

[0028] 3), after the reaction is finished, the autoclave is naturally cooled to room temperature, and the reacti...

Embodiment 3

[0032] Embodiment 3, a preparation method of filled antimony-based skutterudite compound, the following steps are carried out in sequence:

[0033] 1), the analytically pure LaCl 3 ·nH 2 O, CoCl 2 ·6H 2 O, SbCl 3 and Na 2 TeO 3 , press La 0.2 Yb 0.8 Fe 3 CoSb 10 Te 2 Stoichiometric batching, each 0.4mmol LaCl 3 ·nH 2 O, 1.6 mmol YbCl 3 , 6 mmol FeCl 3 ·6H 2 O, 2 mmol CoCl 2 ·6H 2 O, 20 mmol SbCl 3 and 4 mmol Na 2 TeO 3 , the above six kinds of raw materials were dissolved in 350mL deionized water as base materials, and mixed uniformly to obtain a mixed solution.

[0034] 2) Place the prepared mixed solution in an autoclave (WDF-0.5 type), and the volume of the autoclave is 500mL. Then add the reducing agent KBH in the autoclave 4 130mmol and organic complexing agent citric acid 33mmol, then immediately seal the autoclave. The autoclave was heated to 150°C and reacted for 100 hours.

[0035] 3), after the reaction is finished, the autoclave is naturally...

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Abstract

The structural formula of filled antimony-based square cobalt mineral compound is RxM4Sb12-yDy; R represents filled atom element, M represents VIII-B family transient metal elements, D represents doped elements, 0 C22C 12 / 00 C22C 1 / 00 B22F 9 / 16 0 6 2 2007 / 4 / 13 101074463 2007 / 11 / 21 000000000 Zhejiang Univ. 310027 Zhao Xinbing Mi Jianli Zhu Tiejun tangyin yi 33212

Description

technical field [0001] The invention relates to a novel semiconductor refrigeration and thermoelectric power generation material and a preparation method thereof, in particular to a preparation method of a filled antimony-based skutterudite thermoelectric material. Background technique [0002] Thermoelectric materials are functional materials that directly convert heat and electricity through carrier transport in solids. Since the energy conversion process realized by thermoelectric materials does not require the operation of mechanical parts or chemical fluid media, thermoelectric power generation and refrigeration devices made of thermoelectric materials have the advantages of no pollution, no noise, no wear, and high reliability. Thermoelectric materials have been widely used in industrial waste heat, waste heat power generation, deep space spacecraft power generation devices and mobile small power generation devices, as well as small refrigeration devices and portable r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C12/00C22C1/00B22F9/16
Inventor 赵新兵糜建立朱铁军
Owner ZHEJIANG UNIV
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