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Hot-pressing sintering device, bulk thermoelectric material with micro-nano porous structure and its preparation method

A technology of thermoelectric materials and porous structure, which is applied in the preparation of bulk thermoelectric materials and hot-pressing sintering devices, and can solve the problems of complex operation steps and inability to be widely used

Active Publication Date: 2019-11-29
INST OF PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the method disclosed in Chinese patent application 200910092656.X requires the use of a pore aid to form holes, and the method has complicated operation steps, which can only be applied to bismuth-tellurium-based thermoelectric material systems and cannot be widely used.

Method used

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  • Hot-pressing sintering device, bulk thermoelectric material with micro-nano porous structure and its preparation method
  • Hot-pressing sintering device, bulk thermoelectric material with micro-nano porous structure and its preparation method
  • Hot-pressing sintering device, bulk thermoelectric material with micro-nano porous structure and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0081] This embodiment is used to illustrate Zintl phase thermoelectric material Mg 3.175 mn 0.025 Sb 1.98 Bi 0.5 Te 0.02 and its preparation.

[0082] Firstly, the simple substance particles of each element are ball milled for 12 hours according to the stoichiometry to form a powder with a particle size of 200 nanometers to 10 microns. The conventional spark plasma sintering method sinters the powder into a dense block (this process is a sintering), and the sintering conditions are as follows: vacuum degree 5Pa, pressure 50MPa, heating rate 50℃ / min, sintering temperature 600℃, holding time 5 minute.

[0083] Then ball mill the primary sintered bulk material for 4 hours to form a raw material powder with a particle size of 200 nanometers to 10 microns. figure 2 Secondary sintering was performed in the device shown to obtain samples with multiscale micro-nanoporous structures. In the secondary sintering, the vacuum degree is 5Pa, the pressure is 50MPa, the heating rate ...

Embodiment 2

[0088] This embodiment is used to illustrate the Half-Heusler alloy thermoelectric material Hf 0.25 Zr 0.75 NiSn 0.99 Sb 0.01 and its preparation.

[0089] First, according to the stoichiometric ratio, the simple substances of each element are arc-melted into ingots, and then ball milled for 12 hours to form a powder with a particle size of 200-600 nanometers. figure 2 Spark plasma sintering is carried out in the device shown, the vacuum degree is 5Pa, the pressure is 60MPa, the heating rate is 40°C / min, the sintering temperature is 900°C, and the holding time is 20 minutes. Samples with scale micro-nanoporous (porous) structures.

[0090] Figure 5 and Figure 6 Representative SEM images of samples of Example 2 at different magnifications are shown. SEM results show that the sample of Example 2 has a multi-scale micro-nano pore (porous) structure. The compactness of the sample of Example 2 is 93%.

[0091] In addition, the FDS-4000 spark plasma sintering furnace joi...

Embodiment 3

[0094] This example is used to illustrate Bi 2 Te 3 Base material Bi 0.5 Sb 1.5 Te 3 and its preparation.

[0095] Firstly, ball mill the elemental particles of each element for 9 hours according to stoichiometry to form a powder with a particle size of 100-300 nanometers. figure 2 Spark plasma sintering is carried out in the device shown, the vacuum degree is 5Pa, the pressure is 50MPa, the heating rate is 70°C / min, the sintering temperature is 450°C, and the holding time is 5 minutes. Samples with scale micro-nanoporous (porous) structures.

[0096] Figure 7 and Figure 8 Representative SEM images of samples of Example 3 at different magnifications are shown. SEM results show that the sample of Example 3 has a multi-scale micro-nano pore (porous) structure. The compactness of the sample of Example 3 is 81%.

[0097] In addition, Bi 0.5 Sb 1.5 Te 3 dense material as a reference sample. Specifically, firstly, according to the stoichiometry, the simple substance...

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Abstract

The invention provides a hot pressing sintering device, which includes an upper electrode, a lower electrode, a water-cooled vacuum chamber and a mold set, wherein the mold set includes a mold main body, an upper pressing head and a lower pressing head, and the mold main body has a through hole in the height direction , the sum of the heights of the upper indenter and the lower indenter is less than the height of the mold body; when working, the mold group is placed in a water-cooled vacuum chamber, and the upper electrode and the lower electrode press the upper indenter and the lower indenter into the through hole of the mold body until The upper indenter and the lower indenter are respectively flush with the upper end surface and the lower end surface of the mold main body, and a sample chamber for accommodating samples is formed in the through hole of the mold main body. The present invention also relates to a method for preparing a thermoelectric material using the above device, and the chemical formula is Mg 3.2‑x mn x Sb 1.5‑y Bi 0.5 Te y Thermoelectric materials with multi-scale micro-nano porous structure, where 0.0125≤x≤0.1, 0.01≤y≤0.05.

Description

technical field [0001] The invention belongs to the field of thermoelectric materials. Specifically, the present invention relates to a hot-press sintering device, a bulk thermoelectric material with a micro-nano porous structure, and a preparation method for a bulk thermoelectric material with a micro-nano porous structure. Background technique [0002] Thermoelectric materials are functional materials that can directly convert heat and electricity, and have the advantages of light weight, small size, simple structure, no noise, zero emissions, and long service life. This brings hope to solve the problems of energy crisis and increasingly severe environmental pollution, as well as to develop green and environmentally friendly new energy materials. Therefore, thermoelectric materials have been highly valued by countries all over the world. [0003] With the design concepts of new materials and the development of new processes and technologies, thermoelectric materials have ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01L35/34B22F3/14
CPCB22F3/14H10N10/01
Inventor 常斯轶陈晓曦李珊王浩陈进赵怀周
Owner INST OF PHYSICS - CHINESE ACAD OF SCI
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