P-CuSe2 (pyrite CuSe2) and preparation method thereof

A technology of pyrite type, copper selenide, applied in binary selenium/tellurium compounds, metal selenide/telluride and other directions, can solve the problem of difficulty in obtaining pure metastable pyrite type copper diselenide, safety hazards The problem of uneven environment and reducibility, to achieve the effect of suitable large-scale production, high safety and suitable reducibility

Active Publication Date: 2019-02-26
QINGHAI UNIV FOR NATITIES
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Problems solved by technology

However, when copper diselenide is prepared by the hot injection method at present, the reaction aids used are reagents such as triethylenetetramine, ethylenediamine, and hydrazine hydrate. These reagents have strong alkalinity and strong reducing properties. will be reduced to Se 2 2- Lower valence state, not easy to control, there is a problem of uneven reducibility in the preparation, there are impurities such as marcasite copper diselenide and copper selenide in the final product, it is difficult to obtain pure metastable pyrite-type diselenide Copper; more importantly, this kind of chemical is highly toxic, and there will be safety hazards and environmental pollution problems when applied to large-scale production

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  • P-CuSe2 (pyrite CuSe2) and preparation method thereof

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[0026] The invention provides a kind of preparation method of pyrite type copper diselenide, comprises the following steps:

[0027] (1) Copper chloride is mixed with triethylene glycol to obtain a cationic precursor solution;

[0028] (2) heating glucose, selenium powder, polyvinylpyrrolidone and triethylene glycol after mixing to obtain anion precursor solution;

[0029] (3) performing a displacement reaction after mixing the cation precursor solution in the step (1) with the anion precursor solution in the step (2), to obtain pyrite-type copper diselenide;

[0030] The mol ratio of described cupric chloride and selenium powder is 1:2;

[0031] The steps (1) and (2) have no chronological relationship.

[0032] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0033] The invention mixes copper chloride and triethylene glycol to obtain a cationic precursor solution....

Embodiment 1

[0050] Dissolve 0.5 mmol of copper chloride dihydrate in 10 mL of triethylene glycol, stir at 40°C for 30 min until dissolved, and the stirring rate is 200 r / min to obtain a cationic precursor solution with a concentration of 0.05 mol / L;

[0051] Add 0.10 g of glucose, 1.0 mmol of selenium powder and 0.20 g of polyvinylpyrrolidone into the three-necked flask, then add 35 mL of triethylene glycol, stir for 5 min at a speed of 400 r / min, and then place the three-necked flask in a thermal reaction reflux device , the system is evacuated first, and then nitrogen gas is introduced, so that it is alternately carried out 3 times, and nitrogen gas is fed after the last vacuum pumping, and the continuous feeding of nitrogen gas is maintained; wherein, the vacuum degree during the vacuum pumping is 0.08MPa, The vacuuming time is 2min; the flow rate of the nitrogen gas is 60mL / min; the above-mentioned mixed solution is heated at a heating rate of 8°C / min, and stirred at a speed of 400r / mi...

Embodiment 2

[0056] Dissolve 1.0 mmol of copper chloride dihydrate in 8 mL of triethylene glycol, stir at 60°C for 30 min until dissolved, and the stirring rate is 200 r / min, to obtain a cationic precursor solution with a concentration of 0.125 mol / L;

[0057] Add 0.20 g of glucose, 2.0 mmol of selenium powder and 0.15 g of polyvinylpyrrolidone into the three-necked flask, then add 40 mL of triethylene glycol, stir for 5 min at a speed of 400 r / min, and then place the three-necked flask in a thermal reaction reflux device , the system is first vacuumed, and then nitrogen is introduced, so that it is alternately carried out 5 times, and nitrogen is introduced after the last vacuuming, and the continuous introduction of nitrogen is kept until the end of the replacement reaction; wherein, the vacuum during the vacuum The temperature is 0.08MPa, and the time of vacuuming is 2min; the flow rate of the nitrogen gas is 60mL / min; Stir at a rotating speed until the temperature of the system reaches...

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Abstract

The invention belongs to the technical field of metastable crystal materials and particularly relates to p-CuSe2 (pyrite CuSe2) and a preparation method thereof. According to the preparation method ofp-CuSe2, CuCl is used as a Cu source, triethylene glycol is used as a solvent and a reducing agent, CuCl and triethylene glycol are mixed, and a cationic precursor solution is obtained. Glucose is used as an auxiliary reducing agent and matched with triethylene glycol, Se powder is reduced to Se2<2-> under the action of polyvinylpyrrolidone, an anionic precursor solution is obtained, auxiliary reducing agents with higher toxicity are avoided, the glucose has proper reducibility and cannot produce Se<2-> and other impure phases due to too high reducibility, and product purity can be improved.The cationic precursor solution and the anionic precursor solution are mixed to be subjected to a replacement reaction, and the p-CuSe2 with single and stable phase is obtained.

Description

technical field [0001] The invention relates to the technical field of metastable crystal materials, in particular to a pyrite-type copper diselenide and a preparation method thereof. Background technique [0002] Copper diselenide (CuSe 2 ), as a metal chalcogenide semiconductor material, has excellent optical, electrical and magnetic properties, and has a wide range of applications in solar cells, ionic conductors, thermoelectric elements and other fields. Especially pyrite-type copper diselenide, it has superconductivity at low temperature, the critical temperature is 2.4K; it has weak ferromagnetism when the temperature is lower than 31K, it is extremely rare to have superconductivity and ferromagnetism at the same time compound. In recent years, copper indium selenide-based thin-film solar cells have developed rapidly, and the conversion efficiency can reach up to 22.6%. Copper diselenide has potential uses as a raw material for large-scale production of copper indium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04
CPCC01B19/007C01P2004/61C01P2006/80
Inventor 马元良黄雄季慧明陈许龙
Owner QINGHAI UNIV FOR NATITIES
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