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Method of quickly preparing Mg-Si-Sn-based thermoelectric material in controllable manner

A mg-si-sn, thermoelectric material technology, which is applied in the field of rapid and controllable preparation of Mg-Si-Sn-based thermoelectric materials, can solve the problem that Mg is easily oxidized or reacts with the container and is easily adhered to the high-temperature volatilization and escape of Mg. The surface of the grinding ball and the inner wall of the ball mill tank, and the components deviate from the nominal stoichiometric ratio, etc., achieve the effect of shortening the preparation cycle, large commercial application potential, and short preparation cycle

Active Publication Date: 2014-12-24
WUHAN UNIV OF TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, since the melting point of Si is as high as 1687K, the melting method has extremely high requirements on equipment, and this preparation process cannot solve the high-temperature volatilization and dissipation of Mg caused by the high melting point difference between Mg and Si, and the easy oxidation of Mg at high temperature or contact with the container. Reaction and other problems; while the mechanical alloying method has the disadvantages of being easily mixed with impurities and oxidation, and Mg is very easy to adhere to the surface of the ball and the inner wall of the ball mill, causing the actual composition to deviate from the nominal stoichiometric ratio, so it is difficult to produce purer Mg 2 Si 1-x sn x compound; vacuum induction melting has extremely high requirements on equipment, and it is difficult to solve the problem of component segregation; adopt B 2 o 3 Although the flux method can use the liquid seal to reduce the contact between the sample and the air, but due to the Mg and B 2 o 3 It can be reacted (magnesia thermal reduction method to prepare boron powder: 3Mg+B 2 o 3 →3MgO+2B), resulting in the mixing of MgO into the Mg-Si-Sn sample; the tantalum tube packaging has problems such as high cost and complicated process; the two-step solid-state reaction has the disadvantages of long preparation period and poor repeatability

Method used

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  • Method of quickly preparing Mg-Si-Sn-based thermoelectric material in controllable manner
  • Method of quickly preparing Mg-Si-Sn-based thermoelectric material in controllable manner
  • Method of quickly preparing Mg-Si-Sn-based thermoelectric material in controllable manner

Examples

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Effect test

Embodiment 1

[0034] A, a kind of fast and controllable method for preparing Mg-Si-Sn base thermoelectric material, it comprises the following steps:

[0035] 1) In an inert gas glove box, press Mg 2.16 (Si 0.3 sn 0.7 ) 0.98 Sb 0.02 The stoichiometric ratio of each element in the method weighs Mg powder (2N, 100-200 mesh), Mg 2 Si powder (2.5N, 200 mesh), Sn powder (2.5N, 200 mesh) and Sb powder (5N, 200 mesh) are used as raw materials, and then the powder is mixed in an agate mortar; Put it into a mold with an inner diameter of 12mm, first hold the pressure at 4MPa for 5min, and then hold at 6MPa for 10min to obtain a cylinder;

[0036] 2) One-step solid phase reaction: Place the cylinder obtained in step 1) in a BN crucible, seal it under vacuum conditions (-0.1MPa) and place it in a high-purity quartz glass tube, then place the quartz glass tube in the tube In a type atmosphere furnace, heat up to 823K at a heating rate of 10K / min, hold for 5min, and then cool with the furnace;

...

Embodiment 2

[0042] A, a kind of fast and controllable method for preparing Mg-Si-Sn base thermoelectric material, it comprises the following steps:

[0043] 1) In an inert gas glove box, press Mg 2.16 (Si 0.3 sn 0.7 ) 0.98 Sb 0.02 The stoichiometric ratio of each element is weighed Mg powder, Mg 2 Si powder, Sn powder and Sb powder were used as raw materials, and then the powders were mixed in an agate mortar; Hold the pressure for 10 minutes under pressure to obtain a cylinder;

[0044] 2) One-step solid phase reaction: Place the cylinder obtained in step 1) in a BN crucible, seal it under vacuum conditions (-0.1MPa) and place it in a high-purity quartz glass tube, then place the quartz glass tube in the tube In a type atmosphere furnace, heat up to 823K at a heating rate of 10K / min, hold for 5min, and then cool with the furnace;

[0045] 3) Spark plasma activation sintering: Grind the product obtained in step 2) into powder in an inert gas glove box, then take a small amount of p...

Embodiment 3

[0049] A, a kind of fast and controllable method for preparing Mg-Si-Sn base thermoelectric material, it comprises the following steps:

[0050] 1) In an inert gas glove box, press Mg 2.16 (Si 0.5 sn 0.5 ) 0.98 Sb 0.02 The stoichiometric ratio of each element is weighed Mg powder, Mg 2 Si powder, Sn powder and Sb powder were used as raw materials, and then the powders were mixed in an agate mortar; Hold the pressure for 10 minutes under pressure to obtain a cylinder;

[0051] 2) One-step solid phase reaction: Place the cylinder obtained in step 1) in a BN crucible, seal it under vacuum conditions (-0.1MPa) and place it in a high-purity quartz glass tube, then place the quartz glass tube in the tube In a type atmosphere furnace, heat up to 833K at a heating rate of 10K / min, hold for 10min, and then cool with the furnace;

[0052]3) Spark plasma activation sintering: grind the product obtained in step 2) into powder in an inert gas glove box, then take a small amount of p...

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Abstract

The invention relates to a method of quickly preparing Mg-Si-Sn-based thermoelectric material in a controllable manner. The method comprises the following steps: 1) dosing and tabletting, namely in the presence of inert gases, weighing Mg powder, Mg2Si powder, Sn powder and Sb powder which are used as raw materials according to a stoichiometric ratio of each element in a chemical formula Mg2(1+z)Si1-xSnxSby (z is not smaller than 0 and not greater than 0.12, x is not smaller than 0 and not greater than 1.0, and y is not smaller than 0 and not greater than 0.025), and mixing and uniformly pressing the raw materials into blocks; 2) sealing the blocks in vacuum, then, heating the blocks to 823-833K, carrying out heat preservation for 5-10 minutes, and cooling the blocks along with a furnace; 3), grinding products obtained in the step 2) into powder in the presence of inert gases, and carrying out discharge plasma activated sintering to obtain the high-performance Mg-Si-Sn-based thermoelectric material. The method has the characteristics of simple process, low energy consumption, short preparation period, good repeatability, excellent thermoelectric properties of obtained block materials, and the like.

Description

technical field [0001] The invention belongs to the field of new energy materials, and in particular relates to a method for rapid and controllable preparation of Mg-Si-Sn-based thermoelectric materials. Background technique [0002] The energy issue is an important issue related to the development of human society. In recent years, with the decreasing reserves of fossil fuels such as coal, oil, and natural gas, and the resulting environmental problems such as the greenhouse effect, dust pollution, and acid rain becoming more and more serious, the development of environmentally friendly new energy has become a priority for researchers in various countries. a consensus. People's requirements for new energy technologies mainly include the following points: (1) extensive and renewable energy sources; (2) environmentally friendly; (3) simple equipment and easy to use; (4) low cost. Representatives of these new energy sources include solar energy, water energy, wind energy, tid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C1/04C22C23/00
Inventor 唐新峰尹康邱思源张强鄢永高苏贤礼
Owner WUHAN UNIV OF TECH
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