CN108017051A - A kind of high conductivity graphene powder and preparation method thereof - Google Patents
A kind of high conductivity graphene powder and preparation method thereof Download PDFInfo
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- CN108017051A CN108017051A CN201710072827.7A CN201710072827A CN108017051A CN 108017051 A CN108017051 A CN 108017051A CN 201710072827 A CN201710072827 A CN 201710072827A CN 108017051 A CN108017051 A CN 108017051A
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- high conductivity
- graphene microchip
- conductivity graphene
- crystalline flake
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/08—Intercalated structures, i.e. with atoms or molecules intercalated in their structure
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of preparation method of high conductivity graphene microchip, it is about 0.098nm using sodium ion radius, sodium atom under molten condition（Sodium ion）It can be embedded into the layer of crystalline flake graphite; recycle the characteristic of the active metal of sodium; it is easy to water; ethanol equal solvent reacts; the energy of the gas of generation is enough the Van der Waals force 16.7KJ/mol for strutting crystalline flake graphite interlamellar spacing; graphene microchip that by this method can be using prepare with scale thickness as 2 10nm, its electrical conductivity are up to 105S/cm, and preparation method is environment friendly and pollution-free.
Description
Technical field
The invention belongs to field of graphene, is related to a kind of preparation method of graphene powder, more particularly, to a kind of high
The preparation method of electric conductivity graphene powder.
Background technology
Graphene is a kind of tightly packed carbon new material into individual layer bi-dimensional cellular shape lattice structure of carbon atom, Yin Qite
Different structure, the thermal conductivity of protrusion and mechanical property, becomes material supply section educational circles research hotspot.The preparation of graphene powder
Method mainly has two kinds of mechanical stripping and chemical method.Wherein mechanical stripping method be directly by graphene platelet from larger crystal
Cut out or tear down, high-quality graphene can be obtained, and cost is low, but shortcoming is that graphene platelet size is difficult to control, nothing
Method reliably produces the graphene powder that length is applied enough, is not suitable for volume production.Chemical method is a kind of important Graphene powder
Preparation, but since preparation process uses substantial amounts of concentrated acid, environmental pollution is more serious, and the graphite reduction journey after oxidation
Degree differs, and causes the graphene powder of high conductivity to hold at high price, and greatly limit graphene answering in downstream industry
With.
The present invention efficiently uses the small metal of atomic radius or alkaline-earth metal intercalation crystalline flake graphite interlayer, utilizes chemical reaction
The energy of generation carrys out Boli scale graphite, so that zero defect on lamella is prepared, and the graphene powder that electric conductivity is high.This method
Evade the process that a large amount of oxidants are used in conventional method, process is environment friendly and pollution-free, and simple production process, reaction time is short,
The graphene powder electric conductivity prepared is up to 105S/cm, it is widely used, it is adapted to large-scale production.
The content of the invention
The object of the present invention is to provide a kind of preparation method of high conductivity graphene, and the method is prepared
Graphene powder material, the graphene powder material prepared by this method have the advantages of defect is few, and electric conductivity is high, can be extensive
Applied in terms of conductive and heat-conductive.
In order to achieve the above object, concrete technical scheme of the invention is a kind of preparation of high conductivity graphene powder
Method, specifically includes following steps：（1）Metallic sodium is melted first, weigh a certain amount of crystalline flake graphite be added to melting after
In metallic sodium, rapid stirring makes metallic sodium（Atom or ion）Fully it is intercalation into crystalline flake graphite；（2）It is added dropwise again a small amount of anti-
Solvent is answered to participate in reaction；（3）After question response, washing filters, and the graphene powder material of high conductivity is can obtain after dry
Material.
The graphene powder that the above method is prepared is thin with lamellar spacing, and uniformity is good, and fault of construction is few, leads
The advantages that conductance is hot good.Specifically evaluation criterion is：（1）Graphene powder body thickness, is tested with AFM, is about 2-10nm；（2）
The electrical conductivity of graphene microchip, it is about 10 to test its electrical conductivity with powder resistivity5s/cm；（3）SEM, can observe graphene
The surface topography of microplate is in lamellar structure.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：Present invention gas is swollen
Swollen method prepares graphene powder, has evaded the process that a large amount of oxidants are used in conventional method, and process is environment friendly and pollution-free, produces work
Skill is simple, and reaction time is short, and almost zero defect, electric conductivity are up to 10 on the graphene powder surface prepared5S/cm, can be wide
It is general to be applied on conductive and heat-conductive, it is adapted to large-scale production.
Brief description of the drawings
Fig. 1 is that the SEM of graphene powder schemes.
Fig. 2 is the atomic force microscope of graphene powder（AFM）Figure.
Embodiment
The embodiment of the present invention is described in further detail below in conjunction with attached drawing.It should be noted that following examples
The present invention is only limitted to, but the practical range being not intended to limit the invention.
Embodiment 1：
（1）20g metallic sodiums are weighed first, are placed on melting in high temperature and pressure stove, are weighed 10g crystalline flake graphites and be added to melting
In metallic sodium afterwards, rapid stirring makes metallic sodium fully be intercalation into crystalline flake graphite；
（2）Lid is opened, the deionized water that 50ml is added dropwise again under conditions of well-ventilated participates in reaction；
（3）After question response, suction filtration is washed with a large amount of deionized waters, the Graphene powder of high conductivity is can obtain after dry
Body；
（4）A small amount of powder body material is taken to be dispersed in absolute ethyl alcohol, it is about 12 ~ 15 nm that its thickness is obtained after being tested with AFM.
Embodiment 2：
（1）40g metallic sodiums are weighed first, are placed on melting in high temperature and pressure stove, are weighed 10g crystalline flake graphites and be added to melting
In metallic sodium afterwards, rapid stirring makes metallic sodium fully be intercalation into crystalline flake graphite；
（2）Lid is opened, the deionized water that 100ml is added dropwise again under conditions of well-ventilated participates in reaction；
（3）After question response, suction filtration is washed with a large amount of deionized waters, the Graphene powder of high conductivity is can obtain after dry
Body；
（4）A small amount of powder is taken to be dispersed in absolute ethyl alcohol, it is about 5 ~ 10 nm that its thickness is obtained after being tested with AFM.
Embodiment 3：
（1）60g metallic sodiums are weighed first, are placed on melting in high temperature and pressure stove, are weighed 10g crystalline flake graphites and be added to melting
In metallic sodium afterwards, rapid stirring makes metallic sodium（Atom or ion）Fully it is intercalation into crystalline flake graphite；
（2）Lid is opened, the deionized water that 200ml is added dropwise again under conditions of well-ventilated participates in reaction；
（3）After question response, suction filtration is washed with a large amount of deionized waters, graphene powder is can obtain after dry；
（4）By its above-mentioned dried powder body material repeat step（1）（2）（3）, i.e. secondary response prepares graphene powder material
Material；
（5）A small amount of graphene powder for passing through secondary response is taken to be dispersed in absolute ethyl alcohol, its thickness is obtained after being tested with AFM is about
2~5 nm。
Embodiment 4：The SEM tests of graphene powder.
The SEM figures of the graphene microchip of the present invention are scanned with the Nova NanoSEM450 types Flied emission of FEI Co. of the U.S.
What Electronic Speculum was measured, test sample is graphene powder prepared by 3 method of embodiment, refer to attached drawing 1；The figure is graphene
The scanning electron microscope (SEM) photograph of powder：Picture shows graphene powder in the form of sheets, and monolayer area is big, and surface topography is regular.
Embodiment 5：The atomic force microscope test of graphene powder.
Tested on Dimension Edge type testers, test sample is graphene prepared by 3 method of embodiment
Powder, sample drop is on mica sheet, drying；Test uses tapping-mode.It is graphene powder that test result, which refer to attached drawing 2,
Atomic force microscopy diagram, it can be seen that a large amount of tablets in irregular shape, sheet surfaces are more smooth, by measuring it in figure
Thickness, analysis draw thickness about between 2 ~ 5 nm.
Embodiment 6：The electrical conductivity test of graphene powder.
With the electrical conductivity of ST-2722 type semiconductor powders resistivity tester measurement graphene powder, test sample is real
The graphene powder of the preparation of example 3 is applied, while prepares 8 samples, horizontal survey, it is 1.98*10 to obtain its electrical conductivity average value5S/m。
It is complete by above-mentioned description, relevant staff using the above-mentioned desirable embodiment according to the present invention as enlightenment
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property scope is not limited to the content on specification, it is necessary to determines its technical scope according to right.
Claims (7)
1. a kind of preparation method of high conductivity graphene microchip, it comprises the following steps：（1）Metallic sodium is melted first, is claimed
Take in the metallic sodium that a certain amount of crystalline flake graphite is added to after melting, rapid stirring makes metallic sodium（Atom or ion）Fully insert
Layer is into crystalline flake graphite；（2）A small amount of reaction dissolvent is added dropwise again and participates in reaction；（3）After question response, washing filters, dry
It can obtain the graphene powder material of high conductivity afterwards.
A kind of 2. preparation method of high conductivity graphene microchip according to claim 1, it is characterised in that：The gold
It is only the alkali and alkaline earth metal ions that the representational material of one of which, in principle atom or ionic diameter are less than 0.14nm to belong to sodium
And its activity come hydrogen before metal all meet the method.
A kind of 3. preparation method of high conductivity graphene microchip according to claim 1, it is characterised in that：Described is anti-
It is deionized water to answer solvent, the one or more in absolute ethyl alcohol, inorganic acid.
A kind of 4. preparation method of high conductivity graphene microchip according to claim 1, it is characterised in that：Described is dry
Dry mode can be heat drying or freeze-drying.
A kind of 5. preparation method of high conductivity graphene microchip according to claim 1, it is characterised in that：It is signified
Abundant intercalation be by stirring or ultrasonic disperse at least 30min, make crystalline flake graphite intercalation uniform.
A kind of 6. preparation method of high conductivity graphene microchip according to claim 1, it is characterised in that：It is described
Preparation method repeats operation, can obtain higher-quality graphene microchip.
A kind of 7. preparation method of high conductivity graphene microchip according to claim 2, it is characterised in that：The gold
The state belonged to when participating in reacting is fluid or gas.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016109598594 | 2016-10-28 | ||
| CN201610959859 | 2016-10-28 |
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| CN108017051A true CN108017051A (en) | 2018-05-11 |
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| CN201710072827.7A Pending CN108017051A (en) | 2016-10-28 | 2017-02-10 | A kind of high conductivity graphene powder and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110740623A (en) * | 2019-10-28 | 2020-01-31 | 宁波石墨烯创新中心有限公司 | Thin-layer graphene/metal composite heat-conducting film material and preparation method thereof, preparation method of metal salt intercalated graphene and electronic device |
| CN113358428A (en) * | 2021-04-26 | 2021-09-07 | 万向一二三股份公司 | Lithium battery pole piece processing method |
-
2017
- 2017-02-10 CN CN201710072827.7A patent/CN108017051A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110740623A (en) * | 2019-10-28 | 2020-01-31 | 宁波石墨烯创新中心有限公司 | Thin-layer graphene/metal composite heat-conducting film material and preparation method thereof, preparation method of metal salt intercalated graphene and electronic device |
| CN110740623B (en) * | 2019-10-28 | 2021-02-02 | 宁波石墨烯创新中心有限公司 | Thin-layer graphene/metal composite heat-conducting film material and preparation method thereof, preparation method of metal salt intercalated graphene and electronic device |
| CN113358428A (en) * | 2021-04-26 | 2021-09-07 | 万向一二三股份公司 | Lithium battery pole piece processing method |
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