CN110002435A - A kind of graphene and its preparation method and application - Google Patents
A kind of graphene and its preparation method and application Download PDFInfo
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- CN110002435A CN110002435A CN201910309276.0A CN201910309276A CN110002435A CN 110002435 A CN110002435 A CN 110002435A CN 201910309276 A CN201910309276 A CN 201910309276A CN 110002435 A CN110002435 A CN 110002435A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention belongs to electrode material preparation technical fields, and in particular to a kind of graphene and its preparation method and application.Include the following steps: that (1) uses graphite type material to do cathode as anode, I A race or II A race metal, forms battery system, carry out charge and discharge；(2) material will be obtained after electric discharge be placed in liquid to impregnate, dry, the material with graphene-structured can be obtained.The present invention does cathode by using I A race or II A race metal, and there is the material of graphene-structured with preparation after graphite type material composition battery system charge and discharge, considerably reduce the production cost and operation difficulty of graphene, meanwhile the graphene prepared as cell negative electrode material when it is with good performance.
Description
Technical field
The invention belongs to electrode material preparation technical fields, and in particular to a kind of graphene and its preparation method and application.
Background technique
In background of invention, it is only intended to increase understanding of the overall background of the invention for disclosed information, without
Necessarily it is considered as recognizing or imply that information composition has become in any form to show well known to persons skilled in the art
There is technology.
Graphene has high specific surface (2630m2·g-1), high thermal conductivity (5000WmK-1), it is high intensity, high
The advantages that electric conductivity, high Young's modulus (125GPa), therefore have in energy storage field, Materials with High Strength field and heat transfer field etc.
Greatly use prospect.
The existing method for preparing graphene specifically includes that electrolysis method, solvent-thermal method, solvent stripping method, chemical vapor deposition
Method, oxidation-reduction method, micromechanics stripping method and ultrahigh vacuum graphene epitaxial growth method etc..In above-mentioned method, oxidation-
Reduction method is one of widely used method in the method for current production graphene.However, it is considered herein that: use oxygen
When change-reduction method method preparation, need using high vacuum, the atmosphere of high temperature, therefore equipment cost is higher.In addition, the life in reaction
It is also higher to produce cost, so that when preparing graphene using this method, higher cost limits the application of graphene.Therefore, having must
Further to explore the preparation method of graphene.
Summary of the invention
In view of the above problems, the present invention provides a kind of graphene and its preparation method and application.The present invention proposes
Method the production cost and operation difficulty of graphene can be greatly lowered, promote being widely used for graphene.
For achieving the above object, the invention discloses following technical proposals:
The first object of the present invention: a kind of preparation method of graphene is provided, is included the following steps:
(1) it uses graphite type material to do cathode as anode, I A race or II A race metal, forms battery system, carry out charge and discharge
Electricity；
(2) material will be obtained after electric discharge be placed in liquid to impregnate, dry, the material with graphene-structured can be obtained.
In step (1), the graphite type material includes any one in graphite paper, Graphite cloth, graphite flake, graphite fibre etc.
Kind.
In step (1), I A race metal includes the alloy of Li, Na, any one or several compositions in K element.
In step (1), II A race metal includes the alloy of any one or several compositions in Ca, Mg element.
In step (1), the charge and discharge number of the battery is 1-50 times.
In step (1), the electrolyte in the battery system includes: lithium-ion battery electrolytes, sodium-ion battery electrolysis
Liquid, kalium ion battery electrolyte, Magnesium ion battery electrolyte, any one in calcium ion battery electrolyte.
Further, the electrolyte includes: LiPF6-EC/DEC、KPF6-EC/DEC、NaPF6Appointing in-EC/DEC etc.
It anticipates one kind.
In step (2), the liquid are as follows: water, alcohol, acetonitrile, toluene, methanol, tetrahydrofuran, petroleum ether, pyridine, just oneself
Any one or a few mixture in alkane, chlorobenzene, N,N-dimethylformamide or benzonitrile.By liquid to product into
Row impregnate, can remove between graphite linings I A race or II A race metallic element, to obtain high-purity graphene.
In step (2), the soaking time is 0.1-24h.
For graphite type material as electrode material, the metals such as lithium/sodium/potassium/magnesium/calcium do cathode, form battery system, are filled
Electric discharge, is then impregnated with liquid, dries, graphene can be obtained, and this method is simple and easy, stable structure, is easily mass produced.
The second object of the present invention, the preparation method for being to provide the graphene obtain graphene.
The third object of the present invention is to provide the application of the graphene, is included in energy storage material, Materials with High Strength neck, heat
Application in conductive material etc., for example, being used as the preparation of lithium cell cathode material.
Method of the invention prepares the thinking of grapheme material are as follows: existing battery system has lithium, sodium, potassium, magnesium, calcium ion
Battery etc., only composition battery system could in the intercalation metallic atom of graphite type material, therefore, it is necessary to select I A race or
II A race metallic atom；In addition, the metallic atomic radius of I A race or II A race metallic atom is smaller, need lesser energy embedding
Enter the interlayer of graphite type material, therefore is conducive to the synthesis of graphene；By electrochemical reaction process, I A race is introduced in graphite
Or II A race metallic atom, increase its interlamellar spacing, to weaken the interaction force of its interlayer, then dissolves metallic atom
Fall, graphite is layers-separated to can be obtained graphene.
Compared with prior art, the present invention achieves following the utility model has the advantages that the present invention is by using I A race or II A race metal
Cathode is done, and prepares the material with graphene-structured after forming battery system charge and discharge with graphite type material, is greatly lowered
The production cost and operation difficulty of graphene, meanwhile, have when the graphene prepared is as cell negative electrode material good
Performance.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is SEM of the graphite paper under 5000 times in embodiment 1.
Fig. 2 is SEM of the graphite paper under 20000 times in embodiment 1.
Fig. 3 is SEM of the gained graphene under 5000 times in embodiment 1.
Fig. 4 is SEM of the gained graphene under 20000 times in embodiment 1.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As previously mentioned, using high vacuum, the atmosphere of high temperature, therefore the more existing method for preparing graphene needs
Equipment cost is higher；In addition, the production cost in reaction is also higher.Therefore, the present invention proposes a kind of filling using battery system
The method that electric discharge prepares graphene；The present invention is further illustrated now in conjunction with the drawings and specific embodiments.
Embodiment 1
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite paper as electrode material, with metal
Lithium is assembled into battery as cathode, and electrolyte used is 1M LiPF6- EC/DEC discharges, and product is then put into wine
0.5h is impregnated in essence, dries, graphene can be obtained.
Fig. 1 is SEM of the graphite paper under 5000 times in embodiment 1, Fig. 2 be in embodiment 1 graphite paper under 20000 times
SEM.It can be seen from the figure that the surfacing of graphite paper, corrugationless structure.
Fig. 3 is SEM of the gained graphene under 5000 times in embodiment 1, and Fig. 4 is that gained graphene exists in embodiment 1
SEM under 20000 times.It can be seen from the figure that there is apparent pleated structure on the surface of product, illustrate that graphene is successfully closed
At.
Embodiment 2
A kind of preparation method of graphene includes the following steps: to take a certain amount of Graphite cloth as electrode material, with metal
Potassium is assembled into battery as cathode, and electrolyte used is 0.8M KPF6- EC/DEC is carried out charge and discharge 2 times, then by product
2h is impregnated into the water, dries, graphene can be obtained.
Embodiment 3
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite paper as electrode material, with metal
Sodium is assembled into battery as cathode, and electrolyte used is 1M NaPF6- EC/DEC carries out electric discharge 1 time, then puts product
Enter and impregnated in n-hexane for 24 hours, graphene can be obtained in drying.
Embodiment 4
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite flake as electrode material, with metal
Calcium is assembled into battery as cathode, and electrolyte used is 1M LiPF6- EC/DEC is carried out charge and discharge 50 times, then by product
It is put into chlorobenzene and impregnates 5h, dry, graphene can be obtained.
Embodiment 5
A kind of preparation method of graphene includes the following steps: to take a certain amount of Graphite cloth as electrode material, with metal
Magnesium is assembled into battery as cathode, and electrolyte used is 0.8M KPF6- EC/DEC carries out electric discharge 30 times, then by product
It is put into methanol and impregnates 2h, dry, graphene can be obtained.
Embodiment 6
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite paper as electrode material, with metal
Sodium is assembled into battery as cathode, and electrolyte used is 1M NaPF6- EC/DEC is carried out charge and discharge 10 times, then by product
It is put into tetrahydrofuran and impregnates 10h, dry, graphene can be obtained.
Embodiment 7
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite flake as electrode material, with metal
Lithium is assembled into battery as cathode, and electrolyte used is 1M LiPF6- EC/DEC is carried out charge and discharge 20 times, then by product
It is put into alcohol and impregnates 0.5h, dry, graphene can be obtained.
Embodiment 8
A kind of preparation method of graphene includes the following steps: to take a certain amount of graphite flake as electrode material, with metal
Magnesium is assembled into battery as cathode, and electrolyte used is 1M LiPF6- EC/DEC discharges, and product is then put into water
Middle immersion 3h, drying, can be obtained graphene.
Embodiment 9
A kind of preparation method of graphene includes the following steps: to take a certain amount of Graphite cloth as electrode material, with metal
Calcium is assembled into battery as cathode, and electrolyte used is 0.8M KPF6- EC/DEC carries out electric discharge 40 times, then by product
It is put into tetrahydrofuran and impregnates 1h, dry, graphene can be obtained.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene, which comprises the steps of:
(1) it uses graphite type material to do cathode as anode, I A race or II A race metal, forms battery system, carry out charge and discharge；
(2) material will be obtained after electric discharge be placed in liquid to impregnate, dry, the material with graphene-structured can be obtained.
2. the preparation method of graphene as described in claim 1, which is characterized in that in step (1), the graphite type material packet
Include graphite paper, Graphite cloth, graphite flake, any one in graphite fibre.
3. the preparation method of graphene as described in claim 1, which is characterized in that in step (1), I A race metal includes
The alloy of any one or several compositions in Li, Na, K element.
4. the preparation method of graphene as described in claim 1, which is characterized in that in step (1), II A race metal packet
Include the alloy of any one or several compositions in Ca, Mg element.
5. the preparation method of graphene as described in claim 1, which is characterized in that in step (1), the charge and discharge of the battery
Number is 1-50 times.
6. the preparation method of graphene as described in any one in claim 1-5, which is characterized in that in step (2), the liquid
Are as follows: water, alcohol, acetonitrile, toluene, methanol, tetrahydrofuran, petroleum ether, pyridine, n-hexane, chlorobenzene, N,N-dimethylformamide
Or any one or a few the mixture in benzonitrile.
7. the preparation method of graphene as described in any one in claim 1-5, which is characterized in that in step (2), the immersion
Time is 0.1-24h.
8. the preparation method of graphene as described in any one in claim 1-5, which is characterized in that in step (1), the battery
Electrolyte in system includes: lithium-ion battery electrolytes, sodium-ion battery electrolyte, kalium ion battery electrolyte, magnesium ion
Any one in battery electrolyte, calcium ion battery electrolyte；Preferably, the electrolyte includes: LiPF6-EC/DEC、
KPF6-EC/DEC、NaPF6Any one in-EC/DEC.
9. described as the described in any item preparation methods of claim 1-8 obtain graphene.
10. the method according to claim 1 is led, in the preparation of heat conducting material in energy storage material, Materials with High Strength
Application；Or, application of the graphene as claimed in claim 9 in energy storage material, Materials with High Strength neck, heat conducting material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050271574A1 (en) * | 2004-06-03 | 2005-12-08 | Jang Bor Z | Process for producing nano-scaled graphene plates |
| US20080048152A1 (en) * | 2006-08-25 | 2008-02-28 | Jang Bor Z | Process for producing nano-scaled platelets and nanocompsites |
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN101973544A (en) * | 2010-10-29 | 2011-02-16 | 中国科学院上海微***与信息技术研究所 | Method for preparing aqueous solution of single-layer grapheme oxide |
| CN102530930A (en) * | 2011-09-05 | 2012-07-04 | 东莞新能源科技有限公司 | Method for preparing graphene by electrochemical stripping |
| CN102815694A (en) * | 2012-03-13 | 2012-12-12 | 华东理工大学 | Graphene preparation method, and graphene prepared through using method |
-
2019
- 2019-04-17 CN CN201910309276.0A patent/CN110002435A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050271574A1 (en) * | 2004-06-03 | 2005-12-08 | Jang Bor Z | Process for producing nano-scaled graphene plates |
| US20080048152A1 (en) * | 2006-08-25 | 2008-02-28 | Jang Bor Z | Process for producing nano-scaled platelets and nanocompsites |
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN101973544A (en) * | 2010-10-29 | 2011-02-16 | 中国科学院上海微***与信息技术研究所 | Method for preparing aqueous solution of single-layer grapheme oxide |
| CN102530930A (en) * | 2011-09-05 | 2012-07-04 | 东莞新能源科技有限公司 | Method for preparing graphene by electrochemical stripping |
| CN102815694A (en) * | 2012-03-13 | 2012-12-12 | 华东理工大学 | Graphene preparation method, and graphene prepared through using method |
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Application publication date: 20190712 |