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Graphite intercalation compound preparation method

A graphite interlayer and compound technology, applied in the direction of graphite, zinc halide, copper halide, etc., can solve the problems of different physical and chemical properties, different application fields, etc., achieve good process repeatability, reduce production costs, and improve electronic conductivity Effect

Active Publication Date: 2017-08-11
HUNAN UNIV
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  • Abstract
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Problems solved by technology

[0004] In addition, according to the different inserts, the physical and chemical properties of graphite interlayer compounds are different, and their application fields are also different.
At present, there are many researches on graphite intercalation compounds with metal halides as intercalation agents (Adv.EnergyMater.2014, 4, 1300600), but the method of converting metal halide intercalation agents into metal sulfides or metal phosphides is still unknown. not yet reported

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Examples

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Embodiment 1

[0016] A kind of preparation method of the graphite intercalation compound of metal salt as intercalation agent, comprises: 1g particle size is the natural graphite of 10 μ m after drying 4h at 120 ℃, after adding 3.4g anhydrous ferric chloride rapidly, then stirring and mixing in the air, Then vacuum-dried at 120° C. for 1 hour and then transferred to a reaction kettle. After sealing the reaction kettle in the air, it was placed in a heating furnace and heated to 450° C. and kept for 48 hours. The obtained product was washed with deionized water, alcohol and acetone and dried at 80 °C for 12 h to obtain a first-order FeCl 3 -graphite intercalation compound (as attached figure 1 Shown), the sample is named FG-1 (F ferric chloride, -2 first order). Take 0.3g of the FG-1 prepared above in CS 2 Heating it to 550°C at a heating rate of 5°C / min in the mixture with nitrogen gas and holding it for 2 hours to prepare a graphite intercalation compound intercalated with iron sulfide, ...

Embodiment 2

[0020] Dry 1g of natural graphite with a particle size of 10μm at 100°C for 4h, then quickly add 1.7g of anhydrous ferric chloride, stir and mix in the air, then dry it in vacuum at 100°C for 1h, and then transfer it to the reactor. After the gloves are sealed in the air, place them in a heating furnace and heat them to 450°C and keep them warm for 24 hours. The obtained product was washed with deionized water, alcohol and acetone and dried at 80 °C for 12 h to obtain the second-order FeCl 3 - Graphite interlayer compound, the sample is named FG-2 (F ferric chloride, -2 second order);

[0021] Take 0.5g of FG-2 and treat it under the mixed gas of hydrogen and argon at 450°C for 4 hours to obtain RFG-2 (R hydrogen reduction). Take 0.3g of RFG-2 and 0.6g of elemental sulfur in the air and mix them in the reaction kettle. Heat to 155°C and keep it for 12h, then raise the temperature to 350°C and keep it for 2h to make sulfur react with elemental metal to form sulfide. Finally, ...

Embodiment 3

[0023] Dry 1g of natural graphite with a particle size of 10μm at 120°C for 4h, then quickly add 6.8g of anhydrous ferric chloride, stir and mix in the air, then dry it in vacuum at 120°C for 1h, and then transfer it to the reactor. After sealing in the air, place it in a heating furnace and heat it to 450°C and keep it warm for 12 hours. The obtained product was washed with deionized water, alcohol and acetone, dried at 80°C for 12 hours, and collected for later use. The sample was named FG-1 (F ferric chloride, -1 first order). Take 0.3g of the above-prepared FNG-1 and heat it to 550°C at a heating rate of 5°C / min in a mixed atmosphere of hydrogen sulfide and nitrogen, and keep it warm for 2 hours to prepare an iron sulfide intercalated graphite intercalation compound.

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Abstract

The invention discloses a graphite intercalation compound preparation method. The method includes: mixing graphite with metal halides in air, sealing in a reactor, heating to a certain temperature, keeping the temperature for a period of time to allow the metal halides to diffuse to graphite intercalation so as to form a graphite intercalation compound with the metal halides as an intercalator, and converting the metal halide type intercalator into metal sulfide or metal phosphide to obtain a graphite intercalation compound with the metal sulfide / phosphide as the intercalator, so that the metal sulfide / phosphide can exist in graphite intercalation in a molecular level. Insertion of different substances in graphite intercalation can be realized, so that different characteristics of products can be achieved; a preparation process has advantages of low material consumption, low energy consumption, product quality stability, high technical repeatability and the like, the method is suitable for large-scale industrial production, and final products are applied to fields of next-generation energy storage materials, solar cell materials, electro-catalysis and the like.

Description

technical field [0001] The invention relates to a preparation method of graphite intercalation compound with metal sulfide or metal phosphide as intercalation agent. Background technique [0002] Graphite intercalation compound is a new material that has been paid more and more attention in recent years. Graphite is a hexagonal crystal system, which is a typical C layered structure substance. The carbon atoms on the layer plane are combined by strong covalent bonds, and the layers are combined by weak van der Waals force, and the interlayer distance is relatively large. Therefore, under appropriate conditions, various chemical substances such as acids, alkali metals, and salts can be inserted into the graphite interlayer, and combine with carbon atoms to form a new chemical phase-graphite interlayer compound. Graphite intercalation compounds not only maintain the excellent physical and chemical properties of graphite, but also exhibit unique physical and chemical properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/22C01G49/10C01G3/05C01G9/04H01M4/36H01M4/58H01M4/587H01M4/62H01M10/0525
CPCC01G3/05C01G9/04C01G49/10C01P2002/72C01P2006/40H01M4/366H01M4/5805H01M4/5815H01M4/587H01M4/625H01M10/0525Y02E60/10
Inventor 韩飞张成智刘金水李轩科张福全
Owner HUNAN UNIV
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