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P-type thermoelectric material and preparation method thereof

A reaction and ligand technology, applied in the field of p-type thermoelectric materials and their preparation, can solve the problems of lack of raw material sources and complicated preparation methods, and achieve the effect of simple equipment and wide sources

Active Publication Date: 2022-07-01
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the existing thermoelectric materials, although inorganic thermoelectric materials have high performance, their raw material sources are relatively scarce, and their preparation methods are relatively complicated.

Method used

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  • P-type thermoelectric material and preparation method thereof
  • P-type thermoelectric material and preparation method thereof
  • P-type thermoelectric material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1. Preparation of 1,4-dihydroxy-2,3,5,6-tetramercaptobenzene (DHTMB)

[0044] Flow chart such as figure 1 shown.

[0045] 1. Synthesis of 2,3,5,6-tetrabenzylthio-1,4-benzoquinone

[0046] 3.072g of sodium hydride was added to a 500mL two-necked bottle with a magnet, one bottle mouth was plugged with a rubber stopper, and the other bottle mouth was connected to a double-row tube. The gas in the bottle was withdrawn and argon was passed through, repeating 3 times. 300 mL of tetrahydrofuran was added, 9 mL of benzyl mercaptan was added while stirring, and 3.9 g of tetrachlorobenzoquinone was added after the reaction was performed at room temperature for 1 hour. The reaction system was heated to 60°C, and the temperature was lowered to room temperature after 12 hours of reaction. Water was added to the system, followed by extraction with dichloromethane three times, the extract was dried over anhydrous magnesium sulfate, and filtered to obtain a filtrate. The s...

Embodiment 2

[0051] Example 2. Preparation of Ag-DHTMB crystallites

[0052] Flow chart such as figure 1 shown.

[0053] 48mg DHTMB was added to a 100mL two-necked bottle with a magnet, one bottle mouth was plugged with a rubber stopper, and the other bottle mouth was connected to a double-row tube. The gas in the bottle was withdrawn and argon was passed through, repeating 3 times. 40 mL of degassed methanol and 116.8 mg of silver acetate were added sequentially (the molar ratio of DHTMB to silver acetate was 1:3.5). Heat to reflux and return to room temperature after 24 hours of reaction. The solid was obtained by filtration, washed with water, methanol and diethyl ether in turn, and dried in vacuum at 60°C to obtain Ag-DHTMB microcrystals.

Embodiment 3

[0054] Example 3. Characterization of DHTMB and Ag-DHTMB crystallites

[0055]A small amount of prepared DHTMB was dissolved in deuterated toluene solvent and subjected to 1 H-NMR characterization; Ag-DHTMB crystallites were characterized by synchrotron radiation powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, etc. , Seebeck coefficient, etc.

[0056] figure 2 for DHTMB 1 H NMR chart, it can be seen from the figure that the ratio of the number of hydroxyl groups to sulfhydryl groups is 1:2, which is the same as its theoretical value.

[0057] image 3 is the synchrotron radiation powder X-ray diffraction peak of Ag-DHTMB crystallite and its fitting diagram with the theoretical diffraction peak. It can be seen that the half width of the synchrotron radiation powder X-ray diffraction peak of Ag-DHTMB crystallite is very narrow, indicating that the The crystallinity of the crystal is very high. Compared with the theoretical diffrac...

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Abstract

The invention discloses a p-type thermoelectric material and a preparation method thereof. The p-type thermoelectric material is an Ag-based coordination polymer and is obtained by reacting a ligand as shown in a formula I with silver acetate, wherein the ligand is prepared according to a method comprising the following steps: S1, in an inert atmosphere, reacting benzyl mercaptan with sodium hydride to obtain benzyl mercaptan sodium, and reacting the benzyl mercaptan sodium with chloranil; s2, a crude product obtained after the reaction is subjected to a reaction in the presence of manganese dioxide, and 2, 3, 5, 6-tetrabenzyl thio-1, 4-benzoquinone is obtained; s3, under the inert atmosphere, 2, 3, 5, 6-tetrabenzyl thio-1, 4-benzoquinone and boron tribromide are subjected to a reaction in fluorobenzene, and 2, 3, 5, 6-tetrabenzyl thio-1, 4-benzoquinone and boron tribromide are subjected to a reaction; and reacting the obtained product in degassed methanol in an inert atmosphere. The Ag-based coordination polymer has high crystallinity, high conductivity and high Seebeck coefficient, and has important significance on synthesis of p-type thermoelectric materials.

Description

technical field [0001] The invention relates to a p-type thermoelectric material and a preparation method thereof, belonging to the field of thermoelectric materials. Background technique [0002] Electric energy is a widely used clean energy, and the main source of electricity today is the combustion of fossil fuels. However, due to the disadvantages of non-renewable fossil fuels, environmental pollution caused by combustion, and aggravation of the greenhouse effect, it has become an inevitable trend to explore environmentally friendly power generation methods. Thermoelectric materials are materials that can convert thermal energy into electrical energy. Because of the advantages of quietness, long life, and no environmental pollution, thermoelectric materials have received extensive attention because they do not require mechanical moving parts during the conversion process. Among the existing thermoelectric materials, although inorganic thermoelectric materials have high ...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C319/06C07C319/14C07C323/20C07C323/22C08G83/00H01L35/24
CPCC07C323/20C07C319/02C07C319/14C07C319/06C08G83/008C07C2601/16H10N10/856C07C323/22
Inventor 徐伟李洋
Owner INST OF CHEM CHINESE ACAD OF SCI
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