Preparation method of copper, cobalt and sulfur micropowder

A copper-cobalt-sulfur ultra-fine powder technology, applied in electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of no copper-cobalt-sulfur ultra-fine powder reports, limited copper-cobalt-sulfur research reports, cumbersome experimental procedures, etc. , to achieve the effects of easy large-scale industrial production, large reversible charge and discharge capacity, and simple product separation operation

Inactive Publication Date: 2016-02-24
SOUTHWEST UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2011, Wang Taihong's research group from Hunan University prepared a cabbage-shaped ternary composite sulfide copper tin sulfur Cu 2 SnS 3 , but its preparation method is obtained by calcining the reaction intermediate at high temperature in an argon atmosphere, and the economic cost is relatively high (Nanoscale, 2011, 3, 4389-4393)
In 2013, Jiang Jianjun's research group at Huazhong University of Science and Technology prepared nickel-cobalt-sulfur NiCo 2 S 4 Hollow nanotubes, but many steps are required and the experimental process is cumbersome (CrystEngComm2013, 15, 7649-7651)
But so far, the research reports on copper-cobalt-sulfur (Cu-Co-S) ternary composites are very limited, and there is no report on nano-scale copper-cobalt-sulfur ultrafine powder.

Method used

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  • Preparation method of copper, cobalt and sulfur micropowder
  • Preparation method of copper, cobalt and sulfur micropowder
  • Preparation method of copper, cobalt and sulfur micropowder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of copper cobalt sulfur superfine powder, it comprises the following steps:

[0038] (1) Weigh 0.1997g copper acetate hydrate (Cu(CH 3 COO) 2 ·H 2 O, purity ≥99.0%), 0.4982g of cobalt acetate hydrate (Co(CH 3 COO) 2 4H 2 O, purity ≥99.5%) and 0.3045g of thiourea (CH 4 N 2 S, purity ≥ 99.0%), dissolved in 60ml of ethylene glycol, stirred to form a solution;

[0039] (2) Transfer the solution obtained in step (1) to a 100ml stainless steel reaction kettle lined with polytetrafluoroethylene, and react for 12 hours at 200°C to obtain a black product after the reaction;

[0040] (3) Wash the obtained black product with absolute ethanol, centrifuge and wash it three times, and then dry it under vacuum at 80°C for 12 hours, so as to obtain black copper-cobalt-sulfur ultrafine powder.

[0041] As attached to the manual Figure 1-7 As shown, the obtained copper-cobalt-sulfur ultrafine powder is tested and it can be seen that: the copper-cobalt-sulfu...

Embodiment 2

[0043] A preparation method of copper cobalt sulfur superfine powder, it comprises the following steps:

[0044] (1) Weigh 0.2491g copper nitrate hydrate (Cu(NO 3 ) 2 ·3H 2 O, purity ≥99.5%), 0.5821g of cobalt nitrate hydrate (Co(NO 3 ) 2 ·6H 2 O, purity ≥99.0%) and 0.3045g of thiourea (CH 4 N 2 S, purity ≥ 99.0%), dissolved in 60ml of ethanol, stirred to form a solution;

[0045] (2) Transfer the solution obtained in step (1) to a 100ml stainless steel reactor lined with polytetrafluoroethylene, and react at 220°C for 6 hours;

[0046] (3) The product obtained in step (2) was washed with absolute ethanol and centrifuged for three times, and then dried under vacuum at 80°C for 12 hours to obtain black copper-cobalt-sulfur ultrafine powder.

[0047] As attached to the manual Figure 8 As shown, the copper-cobalt-sulfur ultrafine powder prepared in this example is a nano-flower morphology composed of nano-sheets.

Embodiment 3

[0049] A preparation method of copper cobalt sulfur superfine powder, it comprises the following steps:

[0050] (1) Weigh 0.1997g copper acetate hydrate (Cu(CH 3 COO) 2 ·H 2 O, purity ≥99.0%), 0.4982g of copper acetate hydrate (Co(CH 3 COO) 2 4H 2 O, purity ≥99.5%) and 0.4846g of L-cysteine ​​(C 3 h 7 NO 2 S, purity ≥ 98.5%), dissolved in 60ml of ethylene glycol, stirred to form a solution;

[0051] (2) Transfer the solution obtained in step (1) to a 100ml stainless steel reaction kettle lined with polytetrafluoroethylene, and react at 180°C for 20 hours;

[0052] (3) The product obtained in step (2) was washed with absolute ethanol and centrifuged for three times, and then dried under vacuum at 80°C for 12 hours to obtain black copper-cobalt-sulfur ultrafine powder.

[0053] As attached to the manual Figure 9 As shown, the copper-cobalt-sulfur ultrafine powder prepared in this example has the morphology of nanoparticle stacking.

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Abstract

The invention relates to a preparation method of copper, cobalt and sulfur micropowder. The copper, cobalt and sulfur micropowder is copper, cobalt and sulfur ternary composite sulfide CuCo2S4 solid powder, the color is black brown or black, the shape is amorphous or in cubic crystalline phase, the powder dimension is 10<-5> to 10<-8>m; the preparation method is as follows: divalent copper salt, divalent cobalt salt and an organic sulfur compound are synthesized by a one-step hydrothermal method. The preparation method is simple and is easy to realize industrial production, the prepared copper, cobalt and sulfur micropowder has excellent electrochemical properties, higher specific capacity and good cycle stability.

Description

technical field [0001] The invention relates to the technical field of electrochemistry and new energy materials, in particular to a preparation method of copper-cobalt-sulfur ultrafine powder. Background technique [0002] At present, the related research on lithium-ion batteries has attracted people's attention and interest, among which, how to obtain high-performance lithium-ion battery anode materials is particularly concerned. As we all know, the negative electrode materials of lithium-ion batteries must have the essential characteristics of high output voltage, high energy density, stable discharge voltage, and long cycle life. However, the theoretical specific capacity of existing commercial carbon-based graphite anode materials is only 372mAh / g, and poor cycle stability and low Coulombic efficiency also make carbon-based graphite anode materials unable to meet today's energy needs. Therefore, the development of a new lithium-ion battery anode material with high capa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525
CPCH01M4/5815H01M10/0525Y02E60/10
Inventor 刘胜袁若聂龙英
Owner SOUTHWEST UNIVERSITY
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