Method for preparing skutterudite base thermoelectric block body material

A technology of bulk materials and thermoelectric materials, applied in the field of materials

Inactive Publication Date: 2009-04-01
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the product contains more or less elemental Sb and CoSb 2 phase, and this method only proposes CoSb 3 and CoSb 3 Synthetic process of doped

Method used

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  • Method for preparing skutterudite base thermoelectric block body material
  • Method for preparing skutterudite base thermoelectric block body material
  • Method for preparing skutterudite base thermoelectric block body material

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0022] In 0.1 co 4 Sb 12 Preparation of thermoelectric materials

[0023] 1. Synthesis process

[0024] 1. Ingredients

[0025] Add about 40ml of absolute ethanol to a 100ml polytetrafluoroethylene tank, add 4.48g of KOH or NaOH, stir slightly, and calculate the theoretical output as 2g, according to In 0.1 co 4 Sb 12 Stoichiometric addition of CoCl in sequence 2 ·6H 2 O, SbCl 3 , InCl 3 4H 2 O, KBH 4 1.114g, 3.205g, 0.034g, 2.8g, respectively, and then stir evenly, and finally add absolute ethanol to a total volume of about 80-85ml, cover it, and put it into an autoclave.

[0026] 2. Solvothermal reaction

[0027] Put the high-pressure reaction kettle into the heating furnace and raise the temperature to 180-200°C at a rate of 5-10°C / min for 48 hours, and then naturally cool to room temperature.

[0028] 3. Washing

[0029] Pour off the clarified solvent in the upper layer of the reaction kettle, stir the black product with an appropriate amount of deionized wa...

example 2

[0044] In 0.1 co 3.7 Ni 0.3 Sb 12 Preparation of thermoelectric materials

[0045] 1. Synthesis process

[0046] 1. Ingredients

[0047] Add about 40ml of absolute ethanol to a 100ml polytetrafluoroethylene tank, add 4.48g of KOH or NaOH, stir slightly, and calculate the theoretical output as 2g, according to In 0.1 co 3.7 Ni 0.3 Sb 12 Add the corresponding amount of CoCl sequentially in the stoichiometric ratio 2 ·6H 2 O, SbCl 3 , InCl 3 4H 2 O, NiCl 2 ·6H 2 O, KBH 4 About 1.03g, 3.205g, 0.034g, 0.083g, 2.8g respectively, then stir evenly, and finally add absolute ethanol until the total volume reaches 80-85ml, cover it, and put it into the autoclave.

[0048] 2. Constant temperature reaction

[0049] Put the high-pressure reaction kettle into the heating furnace and raise the temperature to 180-200°C at a rate of 5-10°C / min for 48 hours, and then naturally cool to room temperature.

[0050] 3. Washing

[0051] Pour off the clarified solvent in the upper la...

specific example 3

[0057] In 0.2 co 4 Te 0.2 Sb 11.8 Preparation of thermoelectric materials

[0058] 1. Synthesis process

[0059] 1. Ingredients

[0060] Add about 40 ml of absolute ethanol to a 100ml polytetrafluoroethylene tank, add 4.48 grams of KOH or NaOH, stir slightly, and calculate the theoretical output as 2 grams, according to In 0.2 co 4 Te 0.2 Sb 11.8 Stoichiometric addition of CoCl in sequence 2 ·6H 2 O, SbCl 3 , InCl 3 4H 2 O, Na 2 TeO 3 , KBH 4 They are 1.106g, 3.129g, 0.068g, 0.028g, 2.8g respectively, stir evenly, and finally add absolute ethanol until the total volume reaches 80-85ml, cover it, and put it into the autoclave.

[0061] 2. Constant temperature reaction

[0062] Put the closed autoclave into the heating equipment, react at a constant temperature of 180-200°C for 48 hours, and then cool down to room temperature naturally.

[0063] 3. Washing

[0064] Pour off the clarified solvent in the upper layer of the reaction kettle, stir the black product w...

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Abstract

The invention discloses a preparation method of a skutterudite group thermoelectricity lump material, which adopts the combination of solvent thermosynthesis and vacuum melting. In the skutterudite MSb3, M equals to Co, Rh, and Ir, comprising the skutterudite MSb3; M bits or Sb bits-doped MSb3; Ag, Cu, Zn, Cd, Pb, Sn, Ga or In-filled MSb3; doped and filled MSb3 and MSb3 which is compounded with a second phase. The preparation method comprises the steps of: material blending, thermal reaction of the solvent, washing, thermal treatment and sealing melting. The invention discloses a preparation method of a skutterudite group thermoelectricity lump material compounded with the second phase, when adopting the method, second phase nano powder such as ZrO2 with the mass percentage of 0.05 percent to 5 percent is added for supplement in the step of the material blending. Compared with the existing commonly used spark plasma sintering or hot pressed sintering after simple substance mechanical alloying, or the plasma sintering or the hot pressed sintering after long-time high temperature solid phase reaction of the simple substance materials, the obtained materials are more compact and lower in cost.

Description

technical field [0001] The invention belongs to the technical field of materials, and relates to a preparation method of a skutterudite-based thermoelectric block material. Background technique [0002] The general formula of skutterudite-like compounds is MX 3 , (where M can be Co, Ir, Rh, etc., X can be P, As or Sb atoms), has a cubic crystal structure, and contains 8 ABs in a unit cell 3 Molecules, a total of 32 atoms, there are two larger cage-like pores in each unit cell. Due to CoSb 3 Superior electrical conductivity and high Seebeck coefficient have become a research hotspot, but CoSb 3 The thermal conductivity of the bulk thermoelectric material is relatively high. With the concept of "electronic crystal-phonon glass", in CoSb 3 The two larger cage-like pores in the unit cell are filled with other atoms to reduce the CoSb 3 efficient approach to thermal conductivity. [0003] CoSb filled with lanthanides, actinides and alkaline earth metal atoms with smaller a...

Claims

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Application Information

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IPC IPC(8): C22C1/04B22F3/16C22C12/00
Inventor 蔡克峰王玲
Owner TONGJI UNIV
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