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Hot-press sintering device, block thermoelectric materials of micro-nano porous structure and manufacturing method thereof

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

Active Publication Date: 2018-12-07
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-press sintering device, block thermoelectric materials of micro-nano porous structure and manufacturing method thereof
  • Hot-press sintering device, block thermoelectric materials of micro-nano porous structure and manufacturing method thereof
  • Hot-press sintering device, block thermoelectric materials of micro-nano porous structure and manufacturing method thereof

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 present invention provides a hot-press sintering device. The device comprises a top electrode, a bottom electrode, a water-cooling vacuum chamber and a mould group. The mould group comprises a mould main body, an upper pressing head and a lower pressing head, the mould main body is provided with a through hole in a height direction, the sum of the heights of the upper pressing head and the lower pressing head is smaller than the height of the mould main body, when the hot-press sintering device is operated, the mould set is arranged in the water-cooling vacuum chamber, the top electrode and the bottom electrode press the upper pressing head and the lower pressing head into the through hole of the mould main body until the upper pressing head and the lower pressing head to be leveled with the upper end face and the lower end face of the mould main body, and the through hole of the mould main body is internally provided with a sample chamber holding samples. The present invention further relates to a method for preparing thermoelectric materials through adoption of the device mentioned above, and thermoelectric materials of a multi-scale micro-nano porous structure with a chemical formula of Mg3.2-xMnxSb1.5-yBi0.5Tey, wherein 0.0125<=x<=0.1, and 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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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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