Organic thermoelectric material based on cuprous vinyl tetramercaptan and preparation method thereof
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A technology of ethylene tetrathiol and thermoelectric materials, which can be used in thiol preparation, thermoelectric device node lead-out materials, organic chemistry, etc., can solve problems such as low thermal conductivity, and achieve low cost, short process flow, and excellent thermoelectricity. performance effect
Active Publication Date: 2014-04-30
INST OF CHEM CHINESE ACAD OF SCI
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However, organic thermoelectric materials have not received much attention. Organic thermoelectric materials have the adv
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Embodiment 1
[0032] The preparation of ethylene tetrathiol cuprous oxide shown in embodiment 1, formula I
[0033] In an argon atmosphere, disperse 1g of 1,3,4,6-tetrathiacyclopentene-2,5-dione in methanol, add 2.07g of sodium methoxide, and reflux for 12h; then add 3.66g of cuprous iodide , reflux for 12 hours; filter, wash the obtained solid with water, methanol and ether in sequence, and dry it in a vacuum oven (absolute pressure: 0.06Pa) at 50°C to obtain cuprous ethylene tetrathiol represented by formula I, which is marked as pristine.
[0034] Infrared spectrum: 1441cm -1 (ν(C=C)); 1121cm -1 , 897cm -1 , 621cm -1 (ν(C-S)); 470cm -1 (ν(S 2 C=CS 2 )),Such as figure 1 As shown, the identified structure is correct.
Embodiment 2、I2
[0035] Embodiment 2, I 2 Preparation of Organic Thermoelectric Materials by Oxidation
[0036] The compound prepared in Example 1 was dispersed in methanol, and 305mg I was added 2 , reacted at 20°C for 12h, filtered, washed with methanol, water, methanol and ether in turn; dried at 50°C in a vacuum oven (absolute pressure 0.06Pa) to obtain an organic thermoelectric material, and marked as 0.5eq I ox .
Embodiment 3、I2
[0037] Embodiment 3, I 2 Preparation of Organic Thermoelectric Materials by Oxidation
[0038] The compound prepared in Example 1 was dispersed in methanol, and 609mg I was added 2, reacted at 40°C for 18h, filtered, washed with methanol, water, methanol and ether in turn; dried in a vacuum oven (absolute pressure 0.06Pa) at 50°C to obtain an organic thermoelectric material, which was labeled as 1eq I ox.
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Abstract
The invention discloses an organic thermoelectric material based on cuprous vinyl tetramercaptan and a preparation method thereof. The organic thermoelectric material provided by the invention is cuprous vinyl tetramercaptan as shown in formula I. The preparation method of the cuprous vinyl tetramercaptan as shown in the formula I comprises the following steps: (1) under an inert atmosphere, letting sodium methylate have reaction with 1,3,4,6-tetrasulfide pencyclopentene-2,5-diketone under reflux in an organic solvent; (2) after the reaction is ended, adding cuprous iodide into the system after reaction, and performing reaction under reflux to obtain the organic thermoelectric material based on cuprous vinyl tetramercaptan. Cuprous vinyl tetramercaptan provided by the invention has an excellent thermoelectric performance after being treated by LiHBEt3 or I2, for instance at 400K, the electric conductivity is 314S cm<-1>, the Seebeck coefficient is 61.3 muV K<-1>, the thermal conductivity is 0.79 Wm<-1>K<-1>, and the thermoelectric figure of merit is as high as 0.060. Meanwhile, the preparation method of cuprous vinyl tetramercaptan disclosed by the invention is particularly a wet-process synthesis method, which is short in process and low in cost.
Description
technical field [0001] The invention relates to an organic thermoelectric material based on cuprous ethylene tetrathiol and a preparation method thereof. Background technique [0002] Thermoelectric materials can realize mutual conversion of heat energy and electric energy. Compared with traditional power generation, refrigeration and heating equipment, thermoelectric devices have many advantages: no moving parts, easy maintenance; stable performance; no working medium such as Freon; adaptable to various working environment; no noise. Therefore, thermoelectric materials are used in fields such as DNA synthesizers, car seat heating or cooling, microelectronic refrigeration, and outer space. At present, the research objects of thermoelectric materials are mainly inorganic materials, such as Bi-based 2 Te 3 Alloys, filled skutterudite compounds, cage compounds and semi-Hausler compounds, etc. However, organic thermoelectric materials have not received much attention. Organi...
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