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A method for preparing high-performance skutterudite by microwave rapid heating-mechanical alloying two-step synthesis

A technology of mechanical alloying and rapid heating, which is applied in the manufacture/processing of thermoelectric devices, and the material of the junction lead wires of thermoelectric devices. and other problems, to achieve the effect of inhibiting excessive grain growth, uniform heating and heating, and convenient equipment operation.

Active Publication Date: 2019-09-06
ANHUI UNIVERSITY OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the melting and long-time annealing treatment is adopted, and the synthesis time is as long as 30 hours (Acta Physica Acta, 2010, 59(10): 7219-04), the energy consumption is high, and the long-term high temperature will cause the grains to grow excessively. Seriously affect its thermoelectric properties, and because the melting points of Co and Sb differ by 864K, it is difficult to obtain single-phase CoSb by this method 3 based thermoelectric materials
For example, the application of Chinese Patent No. 201410027252.3 uses the melting method to prepare and synthesize CoSb 3 Alloy, adding 2 to 3 days of annealing at the same time, the efficiency of obtaining single crystal is low, and the properties along the growth direction are unstable
However, the solid-phase synthesis method will appear Sb and CoSb 2 Miscellaneous phases, simply using mechanical alloying method, the synthesis time is also longer, easy to generate heterogeneous phases (Thermoelectric Nanomaterials Springer Series in Materials Science,2013,182:255-285)
In addition, using the method described above to prepare synthetic CoSb 3 It is usually difficult to effectively ensure the uniformity of the filling element distribution when using ternary skutterudite thermoelectric materials, which affects its performance

Method used

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  • A method for preparing high-performance skutterudite by microwave rapid heating-mechanical alloying two-step synthesis
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Embodiment 1

[0039] For the preparation of synthetic CoSb by the existing melting method, solid phase synthesis method, mechanical alloying and vapor deposition method 3 The thermoelectric figure of merit and purity of skutterudite existing in the base skutterudite thermoelectric material are relatively low, which affects its use effect. In this embodiment, microwave rapid heating technology is combined with mechanical alloying, and microwave heating is first used to prepare Get CoSb 3 , then the CoSb3 Powder mixed with In powder for filling, mechanically alloyed, and finally sintered, so that In-filled CoSb can be prepared. 3 Cobalt-based thermoelectric materials, effectively improving the obtained CoSb 3 Thermoelectric figure of merit of cobalt-based thermoelectric materials. At the same time, by adopting microwave heating-mechanical alloying two-step synthesis process, and optimizing the specific process parameters, such as microwave heating power, time, ball milling treatment time an...

Embodiment 2

[0052] A method for preparing high-performance skutterudite by microwave rapid heating-mechanical alloying two-step synthesis of the present invention specifically comprises the following steps:

[0053] Step 1. Raw material preparation and mixing

[0054] Co and Sb elemental powders with a particle size of 400 mesh and a purity of 99.9% are used as raw materials, according to CoSb 3 Weigh the atomic mass ratio, and grind and mix, and add acetone during the grinding process;

[0055] Step 2. Cold forming

[0056] After the acetone is completely volatilized, the powder is cold-pressed, and the pressure is 6MPa;

[0057] Step 3: Vacuum fusing and microwave heating

[0058] The cold-pressed sample is sealed in a vacuum quartz tube, and the vacuum degree in the quartz tube is controlled to be 10 -3 Above MPa, then place the sealed quartz tube through a ceramic dry pot in a microwave oven for heating and synthesis. Green silicon carbide is placed inside the dry pot as an auxili...

Embodiment 3

[0064] A method for preparing high-performance skutterudite by microwave rapid heating-mechanical alloying two-step synthesis of the present invention specifically comprises the following steps:

[0065] Step 1. Raw material preparation and mixing

[0066] Co and Sb elemental powders with a particle size of 400 mesh and a purity of 99.9% are used as raw materials, according to CoSb 3 Weigh the atomic mass ratio, and grind and mix, and add acetone during the grinding process;

[0067] Step 2. Cold forming

[0068] After the acetone is completely volatilized, the powder is cold-pressed, and the pressure is 9MPa;

[0069] Step 3: Vacuum fusing and microwave heating

[0070] The cold-pressed sample is sealed in a vacuum quartz tube, and the vacuum degree in the quartz tube is controlled to be 10 -3 Above MPa, then place the sealed quartz tube through a ceramic dry pot in a microwave oven for heating and synthesis. Green silicon carbide is placed inside the dry pot as an auxili...

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Abstract

The invention discloses a microwave rapid heating-mechanical alloying two-step synthesis method for preparing high-performance skutterudite, which belongs to the technical field of thermoelectric material preparation. A method for preparing high-performance skutterudite by microwave rapid heating-mechanical alloying two-step synthesis of the present invention combines rapid microwave heating technology with mechanical alloying, and first prepares CoSb by microwave heating 3 , then the CoSb 3 CoSb powder is mixed with In powder for filling, then mechanically alloyed, and finally sintered to prepare high-purity CoSb 3 Base-filled skutterudite thermoelectric materials. CoSb that is difficult to synthesize by conventional techniques can be prepared by adopting the preparation process of the present invention 3 base-fill alloy, and effectively improved the resulting CoSb 3 Thermoelectric figure of merit and purity of base-filled thermoelectric materials.

Description

technical field [0001] The invention belongs to the technical field of preparation of thermoelectric materials, and more specifically relates to a method for preparing high-performance skutterudite through rapid microwave heating-mechanical alloying two-step synthesis. Background technique [0002] With the depletion of fossil fuels, environmental and energy issues have become increasingly prominent, which has attracted great attention from all countries in the world. Thermoelectric materials can realize the direct conversion of heat energy and electric energy, and have the characteristics of small size, light weight, environmental friendliness, strong reliability, no noise in the working process, long service life, easy integration and large-scale production, etc., so it is the most promising One of the promising new materials. Thermoelectric materials use the dimensionless thermoelectric figure of merit (ZT) to measure performance. where S is the Seebeck coefficient, ρ ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22C12/00C22C1/04B22F3/105B22F9/04H01L35/18H01L35/34H10N10/01H10N10/853
CPCC22C1/04C22C12/00B22F3/105B22F9/04B22F2003/1051B22F2003/1054B22F2009/043B22F2009/041B22F2998/10H10N10/853H10N10/01B22F3/02
Inventor 雷鹰高文圣李雨万润东马雷强郑睿
Owner ANHUI UNIVERSITY OF TECHNOLOGY