Efficient preparation method for skutterudite thermoelectric material through laser

A technology of thermoelectric materials and skutterudite, which is applied in the field of efficient preparation of skutterudite thermoelectric materials, can solve problems such as the difficulty in accurately controlling the composition content of the final block sample, fluctuations in material performance, and volatilization of large Sb phases, and shorten the preparation cycle , low equipment requirements, and the effect of reducing preparation costs

Active Publication Date: 2016-12-07
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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Problems solved by technology

The patent (CN101693962) discloses a preparation method of p-type filled skutterudite material. The raw material is weighed in a glove box, packaged and pressed into tablets, placed in a melt spinning equipment, heated by high-frequency induction for ~5 seconds, and repeated for 3 ~5 times to ensure that the melt composition is uniform, and the melt is spun to obtain a ribbon-shaped product with an amorphous / nanocrystalline composite structure, which is powdered and pressed into tablets, and then SPS (530 ° C, 5 minutes) to obtain a pure-phase bulk material; Both methods require expensive melt spinning equipment, and in the process of master alloy remelting, the sample is heated and melted as a whole, and there is a large volatilization of Sb phase, so it is difficult to accurately control the final block test during large-scale preparation. The composition content of the sample, resulting in fluctuations in material properties

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  • Efficient preparation method for skutterudite thermoelectric material through laser
  • Efficient preparation method for skutterudite thermoelectric material through laser
  • Efficient preparation method for skutterudite thermoelectric material through laser

Examples

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Effect test

Embodiment 1

[0035] Sutterudite (CoSb 3 ) rapid preparation method of thermoelectric material laser melting / SPS, the specific steps are as follows:

[0036] (1) Use 200-mesh sieve powdered Co and Sb as raw materials, according to the chemical formula CoSb 3 Weighing; mix the weighing raw materials evenly in the grinding bowl, then spread the powder on the graphite substrate with a depth of 1mm, and place it in the processing chamber;

[0037] (2) Use argon-hydrogen mixed gas to wash the processing chamber, repeat 3 times, and finally the air pressure in the chamber is 0.12MPa;

[0038] (3) Adjust the laser process parameters, utilize the laser to melt the powder, and as the laser spot moves, the molten powder solidifies; due to the rapid cooling of the above-mentioned melt (10 4 ~10 5 K / s), the ingot grain structure is fine after condensation, and the segregation size is effectively controlled. The segregation size of different samples is similar, about 10 μm, which is much smaller tha...

Embodiment 2

[0041] Tellurium-doped skutterudite (expressed as CoSb 2.85 Te 0.15 、 Te 0.15 CoSb 2.85 or CoTe 0.15 Sb 2.85 ) rapid preparation method of thermoelectric material laser melting / SPS, the specific steps are as follows:

[0042] (1) Use 200-mesh sieve powdered Co, Sb, and Te simple substances as raw materials, according to the chemical formula CoTe 0.15 Sb 2.85 Weighing; mix the weighing raw materials evenly in the grinding bowl, then spread the powder on the graphite substrate with a depth of 1mm, and place it in the processing chamber;

[0043] (2) Use argon-hydrogen mixed gas to wash the processing chamber, repeat 3 times, and finally the air pressure in the chamber is 0.12MPa;

[0044] (3) Adjust the laser process parameters, utilize the laser to melt the powder, and as the laser spot moves, the molten powder solidifies; due to the rapid cooling of the above-mentioned melt (10 4 ~10 5 K / s), the ingot grain structure is fine after condensation, and the segregation siz...

Embodiment 3

[0047] Indium filled skutterudite (In 0.1 co 4 Sb 12 ) rapid preparation method of thermoelectric material laser melting / SPS, the specific steps are as follows:

[0048] (1) Using 200-mesh sieve powdered Co, Sb, and In simple substances as raw materials, according to the chemical formula In 0.1 co 4 Sb 12 weighing. Mix the weighing raw materials evenly in the grinding bowl, then spread the powder on the graphite substrate with a depth of 1mm, and place it in the processing chamber;

[0049] (2) Use argon-hydrogen mixed gas to wash the processing chamber, repeat 3 times, and finally the air pressure in the chamber is 0.12MPa;

[0050] (3) Adjust the laser process parameters, utilize the laser to melt the powder, and as the laser spot moves, the molten powder solidifies; due to the rapid cooling of the above-mentioned melt (10 4 ~10 5 K / s), the ingot grain structure is fine after condensation, and the segregation size is effectively controlled. The segregation size of d...

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Abstract

The invention relates to an efficient preparation method for a skutterudite thermoelectric material through laser. The efficient preparation method comprises the steps that 1, according to the chemical formula of the skutterudite thermoelectric material, pure metal powder is weighed to serve as raw material powder and is put into a graphite matrix after being uniformly mixed; 2, the graphite matrix loaded with the raw material powder is put into an inert atmosphere, and the raw material powder is heated through the laser melting technology, melted along with movement of laser spots and then condensed, so that a cast ingot is obtained; and 3, the cast ingot prepared in the step 2 is ground into powder, the cast ingot powder is sintered through spark plasmas, and thus the skutterudite thermoelectric material is obtained. According to the efficient preparation method for the skutterudite thermoelectric material through the laser, the local powder is heated through the high-energy laser, rapid melting is achieved, and the loss of Sb phases is reduced; then, small-capacity melt is rapidly condensed, and the segregation size is decreased; and subsequently, the SPS short-time heat treatment process is combined, so that efficient preparation of the skutterudite thermoelectric material is achieved.

Description

technical field [0001] The invention belongs to the field of new energy materials and relates to a method for efficiently preparing skutterudite thermoelectric materials. Background technique [0002] Thermoelectric power generation technology uses the Seebeck effect of semiconductor materials to directly convert heat energy into electrical energy. It has the characteristics of small system size, compact structure, no moving parts, maintenance-free, no noise, no emissions, high reliability and long life. The detection power supply and special military power supply have obtained important applications, and have broad application prospects and potential economic and social benefits in solar photoelectric-thermoelectric compound power generation, industrial waste heat—especially in the thermoelectric power generation of automobile exhaust waste heat recovery, and may become today's An important part of the solution to the world's energy crisis (Science 283:804, 1999). [0003]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22C12/00C22C1/04B22F3/105B33Y10/00
CPCC22C12/00B22F3/105B33Y10/00B22F2998/10B22F2003/1051B22F10/00B22F10/36B22F10/28B22F12/41C22C1/047B22F9/04Y02P10/25
Inventor 陈立东姚铮李小亚唐云山王超
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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