Preparing method of high-performance multi-sized nanostructure skutterudite material

A nanostructure, multi-dimensional technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of reduced performance of bulk materials, decreased performance or activity, poor repeatability, etc., to achieve High thermoelectric figure of merit, good shape and performance, and high utilization

Inactive Publication Date: 2016-09-14
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of traditional mechanical grinding to prepare large quantities of nanopowders, a large amount of heat will be generated during the mechanical grinding process, which will cause phase change or decomposition of the material, especially for those multi-component thermoelectric materials (such as multi-component alloys, multi-doped compounds, clathrate, cage compound, etc.), which reduces the performance or activity of the material itself, resulting in a decrease in the performance of the prepared bulk material
Chemical synthesis includes hydrothermal or solvothermal synthesis, which is only suitable for a small amount of synthesis in the laboratory, and has high oxygen content and poor repeatability

Method used

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  • Preparing method of high-performance multi-sized nanostructure skutterudite material
  • Preparing method of high-performance multi-sized nanostructure skutterudite material
  • Preparing method of high-performance multi-sized nanostructure skutterudite material

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Effect test

Embodiment 1

[0031] Homemade Yb by melting method 0.3 Co 4 Sb 12 Polycrystalline materials are used as raw materials, and nano-scale powders are prepared by freezing and grinding methods, and the thermoelectric material blocks are obtained by spark plasma sintering technology. The specific process flow is as follows figure 1 The specific steps are as follows: first crush the crystal material in a steel mold into coarse particles less than 5mm, weigh 20g of the sample and the stainless steel ram into the central cylinder, and then fix it on a freezing grinder filled with liquid nitrogen. Set the starting pre-cooling time to 20min, the frequency to 10cps, the single grinding time to 3min, the single cooling time to 3min, and the cycle to be 20. This not only guarantees the grinding, and at the same time, recooling can also bring out the heat generated by the grinding to avoid occurrence. Phase change or chemical decomposition. After 60 minutes of freezing and grinding, it was raised to room te...

Embodiment 2

[0033] Ba made by melting method 0.3 Co 4 Sb 12 The crystal material is the raw material. Firstly, the crystal material is crushed into coarse particles less than 5mm in a steel mold, and 15g of the sample is weighed into the central cylinder together with the stainless steel ram, and then fixed on a freezing grinder filled with liquid nitrogen. Set the starting pre-cooling time to 10min, the frequency to 7cps, the single grinding time to 2min, the single cooling time to 2min, and the cycle to be 60. This not only ensures the grinding, while re-cooling can also bring out the heat generated by the grinding to avoid occurrence Phase change or chemical decomposition. After 120 minutes of freezing and grinding, it was raised to room temperature and then sampled, and then vacuum-dried to obtain nano-sized powder. Put the powder into a graphite mold and put it into the SPS sintering furnace. Under the protection of argon-hydrogen mixture, the temperature is rapidly raised to 670°C an...

Embodiment 3

[0035] Yb made by melting method 0.2 In 0.1 Co 4 Sb 12 The crystal material is the raw material. First, the crystal material is crushed into coarse particles smaller than 5mm in a steel mold, and 15-20g of the sample is weighed into the central cylinder with the stainless steel ram, and then fixed on the freezing grinder filled with liquid nitrogen. Set the starting pre-cooling time to 15min, the frequency to 9cps, the single grinding time to 3min, the single cooling time to 3min, and the cycle to 50. This not only ensures the grinding, while re-cooling can also bring out the heat generated by the grinding to avoid occurrence Phase change or chemical decomposition. After 150 minutes of freezing and grinding, it was raised to room temperature and then sampled, and then vacuum-dried to obtain nano-sized powder. Put the powder into a graphite mold, put it into an SPS sintering furnace, and quickly raise the temperature to 600°C under an Ar gas shield and keep it at 65MPa for 3 min...

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Abstract

The invention provides a preparing method of a high-performance multi-sized nanostructure skutterudite material. Firstly, a high-temperature melting quenched method is adopted to prepare a thermoelectric material ingot casting, then, a simple and easily-controlled low-temperature refrigeration-grinding method is adopted to prepare nanoscale thermoelectric powder, and refrigeration-grinding is a novel grinding method. Liquid nitrogen is adopted to serve as a refrigeration medium, and the material is ground at the ultralow temperature of -195.6 DEG C. The method has the beneficial effects that the material can be ground at the temperature lower than the temperature of the brittle point of the material, and refining of powder is facilitated; inert nitrogen atmosphere provides protection atmosphere for the material, and oxidization of the material is reduced; the low-temperature liquid nitrogen can bring out a large amount of heat generated in the grinding process, and phase changes or decomposition of the material due to temperature rise is avoided; and finally, through the discharge plasma sintering technology, the high-performance nanostructure skutterudite thermoelectric material is obtained.

Description

Technical field [0001] The invention relates to a method for preparing a high-performance multi-size nanostructure skutterudite thermoelectric material, which belongs to the field of new energy materials. Background technique [0002] Thermoelectric materials, also known as thermoelectric materials, are functional materials that utilize the Seebeck effect and Peltier effect of semiconductors to achieve direct conversion between heat and electrical energy. At the same time, devices made of thermoelectric materials have outstanding advantages such as small size, no noise, no pollution, no moving parts, and maintenance-free. They are used in electric refrigeration and thermoelectric power generation (such as beverage coolers and laser diode coolers, and spacecraft power generation Etc.) have important application prospects. [0003] CoSb 3 The base-filled skutterudite thermoelectric material has large carrier mobility, high conductivity and large Seebeck coefficient. It is a thermoel...

Claims

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Application Information

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IPC IPC(8): C22C12/00C22C1/02C22C1/04B22F9/04B22F3/14B82Y40/00B82Y30/00
CPCC22C1/007C22C1/02C22C12/00B82Y30/00B82Y40/00B22F3/14B22F9/04B22F2009/049C22C1/047
Inventor 王连军周振兴侯殿坤顾士甲江莞
Owner DONGHUA UNIV
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