Method for preparing high thermoelectrical antimony telluride micro-nano crystal and block material thereof

A technology of antimony telluride micro-nano, thermoelectric properties, applied in the direction of nanotechnology, nanotechnology, binary selenium/tellurium compounds, etc., can solve the problem of large-scale production of antimony telluride micro-nano crystals, low conversion efficiency, equipment Complicated problems, low cost, good thermoelectric performance, and simple preparation method

Inactive Publication Date: 2015-01-28
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the main disadvantage of thermoelectric technology is that the conversion efficiency between heat and electricity is still relatively low, usually only about 10%, which is still low compared with traditional power generation and refrigeration technologies, so it still needs to be improve

Method used

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  • Method for preparing high thermoelectrical antimony telluride micro-nano crystal and block material thereof
  • Method for preparing high thermoelectrical antimony telluride micro-nano crystal and block material thereof
  • Method for preparing high thermoelectrical antimony telluride micro-nano crystal and block material thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Weigh 1.3950g antimony trichloride (M(SbCl 3 ) / M(TeO 2 )=0.679, molar ratio) in 50ml of ethylene glycol heated to 50 ~ 100 ℃, stirring completely dissolved and then transferred to a flask containing 1.4364g of tellurium dioxide (0.009mol) and supplemented with ethylene glycol up to 150ml, then It is placed on a heating mantle, heated to 140-180°C, and stirred for 20-40 minutes to obtain a clear and transparent solution. After cooling to 100-120°C, add 4ml of hydrazine hydrate (M(N 2 h 4 ·H 2 O) / M(TeO 2 )=8.962, molar ratio), heated to reflux at 180°C for 48h to obtain a gray precipitate. The obtained product was washed with absolute ethanol and dried in a vacuum environment at 80°C for 8 hours to obtain pure and well-crystallized antimony telluride micro-nanocrystals, whose XRD characterization is shown in figure 1 (a). The antimony telluride micro-nano crystals were cold-pressed into sheet-like blocks under a pressure of 500 MPa, and placed in a tube furnace unde...

Embodiment 2

[0047] Referring to Example 1, the difference is that after adding hydrazine hydrate, the mixture was heated to reflux at 120° C. for 24 hours to obtain a gray precipitate. The obtained product was washed with absolute ethanol and dried in a vacuum environment at 80°C for 8 hours to obtain pure and well-crystallized antimony telluride micro-nanocrystals, whose XRD characterization is shown in figure 1 (c). The antimony telluride micro-nano crystals were cold-pressed into sheet-like blocks under a pressure of 500 MPa, and placed in a tube furnace under 92% Ar + 8% H 2 Annealing at 300°C for 24h under a mixed atmosphere of a protective gas was set at 0.15 L / min, and the annealing heating rate was 5°C / min.

Embodiment 3

[0049] Weigh 1.3950g antimony trichloride (M(SbCl 3 ) / M(TeO 2 )=0.679, molar ratio) in 50ml of ethylene glycol was heated to 50 ~ 100 ℃, stirring completely dissolved and then transferred to a solution containing 1.4364g tellurium dioxide and 4.0g CTAB (M(CTAB) / M(TeO 2 ) = 1.220, molar ratio) and supplemented with ethylene glycol up to 150ml, then placed it on a heating mantle, heated to 140-180°C, stirred for 20-40min to obtain a clear and transparent solution, and cooled to 100-120 After adding 4ml hydrazine hydrate (M(N 2 h 4 ·H 2 O) / M(TeO 2 )=8.962, molar ratio), heated to reflux at 180°C for 24h to obtain a gray precipitate. The obtained product was washed with absolute ethanol and dried in a vacuum environment at 80°C for 8 hours to obtain pure antimony telluride micro-nanocrystals with good crystallinity. For the SEM characterization, see figure 2 (a).

[0050] The antimony telluride micro-nano crystals were cold-pressed into sheet-like blocks under a pressure o...

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Abstract

The invention discloses a method for preparing a high thermoelectrical antimony telluride micro-nano crystal and a block material thereof. The method comprises the following steps: dissolving an antimony precursor into polyol, then mixing the obtained solution with a tellurium precursor and a complexing agent, heating the mixed solution at a temperature of 140 to 180 under stirring, cooling to a temperature of 100 to 120 DEG C, adding a reducing agent, carrying out reactions at a temperature of 120 to 180 DEG C for 6 to 48 hours so as to obtain precipitate, washing the obtained precipitate by waterless ethanol until the washing liquid is neutral, drying the washed precipitate in vacuum so as to obtain antimony telluride micro-nano crystal, cold-pressing the obtained antimony telluride crystal into a sheet, and then carrying out annealing for 2 to 24 hours at a temperature of 300 to 400 DEG C in an atmosphere of mixed gas composed of Ar and H2 with a volume ratio of 92%:8% so as to obtain an antimony telluride block material. The obtained antimony telluride micro-nano crystal and block material thereof have the characteristics of high purity and good thermoelectrical property. Moreover the preparation method has the advantages of simpleness, low cost, easiness in repeating, and suitability for massive production, and thus has a good commercialization prospect.

Description

Technical field: [0001] The invention belongs to the technical field of semiconductor thermoelectric power generation and refrigeration around room temperature, and specifically relates to a method for preparing antimony telluride micro-nano crystals with high thermoelectric properties and bulk materials thereof. Background technique: [0002] With the increasingly prominent problems of energy crisis and environmental pollution, thermoelectric technology, as one of the clean energy technologies, has rapidly received widespread attention in the fields of waste heat power generation and refrigeration. Using the principle of directional movement of carriers inside the semiconductor in the temperature field and electric field, the direct mutual conversion between heat energy and electric energy is realized, which is the so-called semiconductor thermoelectric power generation and refrigeration technology. Compared with traditional power generation and refrigeration equipment, the...

Claims

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Application Information

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IPC IPC(8): C01B19/04B82Y30/00
CPCC01B19/007C01P2002/72C01P2004/03C01P2004/62C01P2006/32C01P2006/40
Inventor 苗蕾杨恒全刘呈燕周建华
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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