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A kind of in-situ synthesis method of transition metal oxide/graphene composite material

A composite material and in-situ synthesis technology, applied in active material electrodes, electrochemical generators, structural parts, etc., can solve volume expansion and other problems

Active Publication Date: 2021-06-22
HUIBO NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing graphene composite material preparation method includes the use of metal simple substance placed in the graphene oxide aqueous solution, the black solid product generated after standing is freeze-dried to obtain the metal oxide / graphene composite, etc., but in the lithium There is a common problem of volume expansion in the negative electrode of ion batteries

Method used

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  • A kind of in-situ synthesis method of transition metal oxide/graphene composite material
  • A kind of in-situ synthesis method of transition metal oxide/graphene composite material
  • A kind of in-situ synthesis method of transition metal oxide/graphene composite material

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Embodiment 1

[0035] (1) Dissolve ferric nitrate, cobalt nitrate, and cerium nitrate in deionized water at a molar ratio of 1:0.1:0.02, mix well and stir to obtain a uniform solution; (2) add ammonia water to the solution at 100 drops / min, Until the pH reaches 10, continue to stir for 2 hours to complete the precipitation. After standing and aging at room temperature for 4 hours, put it in a hydrothermal reaction kettle, react with water at 160°C for 6 hours, filter and wash with water until neutral, and dry to obtain Fe 2 o 3 -Co 2 o 3 -CeO 2 Composite hydroxide precipitation; (3) use improved Hummers method to prepare graphene oxide: take a certain amount of graphite and potassium permanganate and mix evenly, add in the there-necked flask that 98% concentrated sulfuric acid and phosphoric acid mixed acid solution are housed, Continue to stir the reaction for 12h. After the obtained gray-green solution, put it in an ice-water bath for 2h, add hydroxide precipitate (the mass percentage ...

Embodiment 2

[0037] (1) Dissolve ferric chloride, manganese sulfate, and cerium chloride in deionized water at a molar ratio of 1:0.5:0.06, mix well and stir to obtain a uniform solution; (2) add ammonia water to the solution at 300 drops / min until the pH reaches 10, continue to stir for 2 hours to complete the precipitation, put it into a hydrothermal reaction kettle after standing for 4 hours at room temperature, and conduct a hydrothermal reaction at 180°C for 4 hours, filter and wash until neutral, and dry get Fe 2 o 3 -MnO 2 -CeO 2Composite hydroxide precipitation; (3) Use improved Hummers method to prepare graphite oxide: take a certain amount of graphite and potassium permanganate and mix evenly, add in the there-necked flask that 98% concentrated sulfuric acid and phosphoric acid mixed acid solution are housed, continue Stirring and reacting for 12 h, the gray-green solution obtained was then bathed in ice water for 2 h, and precipitated by adding hydroxide (the mass percentage ...

Embodiment 3

[0039] (1) Dissolve iron sulfate, titanium sulfate, and cerium chloride in deionized water at a molar ratio of 1:0.3:0.03, mix well and stir to obtain a uniform solution; (2) add ammonia water to the solution at 400 drops / min , until the pH reaches 10, continue to stir for 2 hours to complete the precipitation, put it into a hydrothermal reaction kettle after standing and aging at room temperature for 4 hours, and conduct a hydrothermal reaction at 140°C for 5 hours, filter and wash with water until neutral, and dry to obtain Fe 2 o 3 -TiO 2 -CeO 2 Composite hydroxide precipitation; (3) Use improved Hummers method to prepare graphite oxide: take a certain amount of graphite and potassium permanganate and mix evenly, add in the there-necked flask that 98% concentrated sulfuric acid and phosphoric acid mixed acid solution are housed, continue Stirring and reacting for 12 h, the gray-green solution obtained was then ice-water bathed for 2 h, and precipitated by adding hydroxid...

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Abstract

A kind of in-situ synthesis method of transition metal oxide / graphene composite material of the present invention, the steps are: dissolving soluble iron salt, transition metal salt and cerium salt in deionized water, mixing to obtain a uniform solution; adding a precipitant, When the pH reaches above 10, stir until the precipitation is complete, let it stand for aging, after the hydrothermal reaction, filter and wash to neutrality, and dry to obtain the hydroxide compound precipitation; weigh graphite and potassium permanganate, mix and Add the mixed acid solution of concentrated sulfuric acid and phosphoric acid, continue to stir the reaction, then take an ice-water bath, add the precipitate, and add the corresponding amount of H 2 o 2 , continue to stir and ultrasonically disperse; the product is washed, centrifuged, dried and sintered to obtain a transition metal oxide / graphene composite material. In the present invention, hydroxide precipitation is directly added in the process of preparing graphite oxide, so that graphene oxide grows on the hydroxide matrix in situ, so as to alleviate the volume expansion effect existing when metal oxide is used in the negative electrode of lithium ion battery.

Description

technical field [0001] The invention belongs to the technical field of negative electrode materials for lithium ion batteries, and in particular relates to an in-situ synthesis method of a transition metal oxide / graphene composite material. Background technique [0002] Compared with traditional secondary batteries, lithium-ion batteries have attracted widespread attention due to their advantages such as high energy density, safety and pollution-free, small self-discharge, wide operating temperature, long cycle life, and no memory effect. Lithium-ion batteries are widely used in portable electronic devices (such as mobile phones, digital cameras, video cameras, notebook computers, etc.) and power tools, and are gradually expanding to electric bicycles, electric vehicles, new energy storage and other fields. [0003] At present, graphite is the most commonly used material for the negative electrode of lithium-ion batteries. Although it has the advantages of high electronic co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/485H01M4/505H01M4/525H01M10/0525
CPCH01M4/364H01M4/38H01M4/485H01M4/505H01M4/525H01M10/0525H01M2004/027Y02E60/10
Inventor 高波朱广林杨东升王艺璇涂赣峰
Owner HUIBO NEW MATERIAL CO LTD