CN109019577A - A kind of graphene and preparation method thereof - Google Patents
A kind of graphene and preparation method thereof Download PDFInfo
- Publication number
- CN109019577A CN109019577A CN201811147266.3A CN201811147266A CN109019577A CN 109019577 A CN109019577 A CN 109019577A CN 201811147266 A CN201811147266 A CN 201811147266A CN 109019577 A CN109019577 A CN 109019577A
- Authority
- CN
- China
- Prior art keywords
- graphene
- adhesive
- preparation
- graphite powder
- roller
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01B32/19—Preparation by exfoliation
-
- 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
Abstract
The present invention discloses a kind of graphene and preparation method thereof, comprising steps of A, graphite powder is dried；Organic solvent is added into adhesive, stirs evenly, adhesive is diluted；Then dry graphite powder is added in the adhesive after dilution, is stirred evenly, the adhesive of graphitiferous powder is made；The adhesive is biological base adhesive；B, the adhesive of graphitiferous powder is added in three-roll grinder between back roller and central roll, adjusts the distance between preliminary roller and central roll, central roll and back roller, the adhesive of graphitiferous powder is ground, removing graphite powder is made；C, purification process is carried out to get graphene to removing graphite powder.Three rollers of use grinding of the invention and the method that biological base adhesive combination technique prepares graphene are simple and quick；Required equipment is simple, and the used time is short, high-efficient, is suitble to large-scale production and practical application.
Description
Technical field
The present invention relates to technical field of graphene more particularly to a kind of graphene and preparation method thereof.
Background technique
Graphene is a kind of Two-dimensional Carbon nanometer material for forming hexagon in honeycomb lattice with sp2 hybridized orbit by carbon atom
Material；According to number of plies difference, graphene is divided into single-layer graphene, bilayer graphene, few layer graphene, multi-layer graphene.Single layer stone
Black alkene (Graphene) refers to by one layer with the periodically closelypacked carbon atom structure of benzene ring structure (i.e. hexagonal honeycomb structure)
At a kind of two-dimentional carbon material；Bilayer graphene (Bilayer or double-layer graphene) refers to by two layers with benzene
Ring structure (i.e. hexagonal honeycomb structure) periodically closelypacked carbon atom is with different way of stacking (including AB stacking, AA heap
Pile etc.) a kind of two-dimentional carbon material for constituting of stacking；Few layer graphene (Few-layer) refers to by 3-10 layers with benzene ring structure (i.e.
Hexagonal honeycomb structure) periodically closelypacked carbon atom is with different way of stacking (including ABC stacking, ABA stacking etc.) heap
A kind of two-dimentional carbon material that pile is constituted；Multi-layer graphene is called thick-layer graphene (multi-layer graphene) and refers to thickness
In the periodically closelypacked carbon atom of 10 layers or more 10nm or less benzene ring structures (i.e. hexagonal honeycomb structure) with different stackings
A kind of two-dimentional carbon material that mode (including ABC stacking, ABA stacking etc.) stacking is constituted.Graphene has high-intensitive, highly conductive
The characteristics such as rate, high-specific surface area, high-barrier and high fire-retardance have very in fields such as electronics, catalysis biological medicine, composite materials
Broad application prospect.The unique two-dimensional layered structure of graphene is in nano-dispersion in the polymer, has lamella barrier effect
Answer, can delay the transmitting of heat, the diffusion of thermal decomposition product and the diffusion of oxygen with mix, therefore material can be effectively improved
Thermal stability, barrier property and other performances.
Though predominantly staying in micro laboratory system mostly currently, existing number of ways or method obtain graphene
In the standby stage, specifically include that micromechanics stripping method, graphite oxide reduction method, surface epitaxial growth method, chemical vapor deposition (CVD)
The methods of method, liquid phase stripping method and graphite intercalation stripping method.Micromechanics stripping method is inefficient, and controllability is not strong, cleannes
Not enough, be not suitable for large-scale production, the needs of basic research experiment can only be met.Graphite oxide reduction method is main there are two
Problem: first is that can generate a large amount of during preparing graphite oxide and have supervirulent waste liquid, have for human body and natural environment
Huge potential hazard, and liquid waste processing after completion of the reaction also becomes problem；Another is precisely due to be difficult to completely also
Original, restores in the graphene-structured of acquisition that there are more defects, causes the performances such as its electronics, mechanics deviation occur, thus answering
It is limited with aspect.The shortcomings that surface epitaxial growth method, is that being difficult to large area prepares, and film forming is uneven, the harsh temperature of condition
> 1100 DEG C of degree, preparation cost is larger.The single-layer graphene that CVD method obtains homoepitaxial is highly difficult, while through CVD method system
The electronic property of standby graphene is influenced very big by substrate.Ultrasound may destroy the knot of graphene to liquid phase stripping method for a long time
Structure, resulting lamella size is also smaller, and also uses a large amount of solvents, generates a large amount of waste liquids.Graphite intercalation stripping method is mostly multilayer
Structure, single layer rate is lower, and the structure of ring graphite may be broken during intercalation, influences the performance of product.In short, graphene exists
Still there is also problems in industrial application field: such as environmental issue, the large-scale production technology problem, cost in preparation process
Problem, development problem of specific aim application technology etc..
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene and preparation method thereof, purports
Solve the problems, such as existing for existing technology of preparing it is inconvenient for use, preparation cost is high, pollute environment and is unfavorable for large-scale production.
Technical scheme is as follows:
A kind of preparation method of graphene, wherein comprising steps of
A, graphite powder is dried；Organic solvent is added into adhesive, stirs evenly, adhesive is diluted；Then
Dry graphite powder is added in the adhesive after dilution, is stirred evenly, the adhesive of graphitiferous powder is made；The adhesive
For biological base adhesive；
B, the adhesive of graphitiferous powder is added in three-roll grinder between back roller and central roll, adjust preliminary roller and central roll, in
The distance between roller and back roller grind the adhesive of graphitiferous powder, and removing graphite powder is made；
C, purification process is carried out to get graphene to removing graphite powder.
The preparation method of the graphene, wherein in the step A, in terms of mass fraction, dry graphite powder is
0.1 ~ 4 part, organic solvent is 1 ~ 15 part, and adhesive is 10 ~ 50 parts.
The preparation method of the graphene, wherein in the step A, the graphite powder is selected from expanded graphites, natural
One of graphite.
The preparation method of the graphene, wherein in the step A, the specification of the graphite powder is 50 ~ 800 mesh.
The preparation method of the graphene, wherein in the step A, it is described biology base adhesive be selected from soybean protein,
One of starch, lignin, pyrolysis bio-oils are a variety of.
The preparation method of the graphene, wherein in the step A, the organic solvent is selected from dehydrated alcohol, acetone
One or both of.
The preparation method of the graphene, wherein in the step B, between the preliminary roller and central roll, central roll and back roller
Distance be 0.1 ~ 1mm.
The preparation method of the graphene, wherein the distance between the preliminary roller and central roll, central roll and back roller are identical.
The preparation method of the graphene, wherein in the step C, the specific steps of the purification process include: pair
It removes graphite powder and carries out ultrasound, then filtering is washed 3 times, then be washed with deionized with dehydrated alcohol, dry.
A kind of graphene, wherein the graphene is made by the preparation method of graphene as described above.
The utility model has the advantages that the grinding of three rollers is introduced the preparation process of graphene by the present invention with biological base adhesive combination technique,
Provide a kind of simple and quick method for preparing graphene.Adhesive used in the preparation method belongs to one kind of natural glue,
Meeting resource-conserving and environmentally friendly idea, and equipment needed for the preparation method is simple, the used time is short, and it is high-efficient, it is suitble to
Large-scale production.The lamella quality of graphene made from preparation method of the present invention is good, remains original crystal form of graphite
Structure has very strong application.
Detailed description of the invention
Fig. 1 is a kind of preparation flow schematic diagram of the preparation method preferred embodiment of graphene of the present invention.
Fig. 2 is the positive SEM figure of expanded graphites used in the embodiment of the present invention 1.
Fig. 3 is the side SEM figure of expanded graphites used in the embodiment of the present invention 1.
Fig. 4 is the positive SEM figure of graphene made from the embodiment of the present invention 1.
Fig. 5 is the side SEM figure of graphene made from the embodiment of the present invention 1.
Fig. 6 is expanded graphites and graphene XRD comparison diagram obtained used in the embodiment of the present invention 1.
Fig. 7 is expanded graphites and graphene TGA comparison diagram obtained used in the embodiment of the present invention 1.
Specific embodiment
The present invention provides a kind of graphene and preparation method thereof, to make the purpose of the present invention, technical solution and effect more
Clear, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only used to
It explains the present invention, is not intended to limit the present invention.
The present invention provides a kind of preparation method preferred embodiment of graphene, and preparation flow is as shown in Figure 1, wherein packet
Include step:
A, it is dried to graphite powder；Organic solvent is added into adhesive, stirs evenly, adhesive is diluted；So
Dry graphite powder is added in the adhesive after dilution afterwards, is stirred evenly, the adhesive of graphitiferous powder is made；The gluing
Agent is biology and adhesive；
B, the adhesive of graphitiferous powder is added in three-roll grinder between back roller and central roll, adjust preliminary roller and central roll, in
The distance between roller and back roller grind the adhesive of graphitiferous powder, and removing graphite powder is made；
C, purification process is carried out to removing graphite powder, obtains graphene.
It should be noted that it is exactly graphite that graphene gathers into folds from level to level, the graphite of thick 1mm comprises about 3,000,000 layers of stone
Black alkene；Pencil gently streaks on paper, and the trace left may be several layers of or even only one layer of graphene.The present invention is by three rollers
Grinding introduces the preparation process of graphene with biological base adhesive combination technique, provides a kind of simple and quick graphene for preparing
Method.Specifically, which is that will be dispersed in the stone of adhesive using the different steerings between three-roll grinder roller and roller
Ink powder constantly carries out quickly horizontal " shearing "；And the viscosity of adhesive is borrowed, make constantly stripping between layers in graphite powder
From.Adhesive used in the preparation method is biological base adhesive, belongs to one kind of natural glue, meets resource-conserving and ring
Border friendly idea；And equipment needed for the preparation method is simple, and the used time is short, and it is high-efficient, it is suitble to large-scale production.The present invention is logical
Adjustment milling time is crossed, can be obtained the graphene of the required number of plies.
It should be noted that carrying out the grinding rate of setting three-roll grinder according to instrument model；Three used in the present invention
Roller mill is use for laboratory, model S65.
Further, the preparation method of the graphene, wherein described that graphite powder is dried in the step A
Condition is 60 ~ 120 DEG C (preferably 80 DEG C), 12 ~ for 24 hours.
Further, the preparation method of the graphene, wherein in the step A, in terms of mass fraction, dry
Graphite powder is 0.1 ~ 4 part, and organic solvent is 1 ~ 15 part, and adhesive is 10 ~ 50 parts.
Further, the preparation method of the graphene, wherein in the step A, the graphite powder can be selected from but
It is not limited to one of expanded graphites, natural graphite.
Further, the preparation method of the graphene, wherein in the step A, the specification of the graphite powder is 50
~ 800 mesh.
Further, the preparation method of the graphene, wherein in the step A, the adhesive can be selected from but
It is not limited to one of soybean protein, starch, lignin, pyrolysis bio-oils or a variety of.
Further, the preparation method of the graphene, wherein in the step A, the organic solvent can be selected from
One or both of but be not limited to dehydrated alcohol, acetone.Solvent for use of the present invention is nontoxic, safety and environmental protection.
Further, the preparation method of the graphene, wherein in the step B, the preliminary roller and central roll, central roll
The distance between back roller is 0.1 ~ 1mm；In the spacing range, effective peeling effect can be played to graphite powder.More
Further, the distance between the preliminary roller and central roll, central roll and back roller are identical；Preferably, the preliminary roller and central roll, central roll and after
The distance between roller is 0.4mm.
Further, the preparation method of the graphene, wherein in the step B, time of the grinding is 0.5 ~
8h.The preparation process used time of the present invention is short, high-efficient, is suitble to large-scale production.
Further, the preparation method of the graphene, wherein in the step C, the specific step of the purification process
Rapid includes: to carry out ultrasound to removing graphite powder, and then filtering is washed 3 times with dehydrated alcohol, then be washed with deionized completely,
It is dry.Preferably, described pair of removing graphite powder carries out 10 ~ 120 min of ultrasound.
The present invention provides a kind of graphenes, wherein the graphene by graphene as described above preparation method system
?.The lamella quality of graphene made from preparation method of the present invention is good, remains original crystalline structure of graphite, has
Very strong application.
Below by embodiment, the present invention is described in detail.
Embodiment 1
(1) appropriate 80 mesh expanded graphites is taken to dry for 24 hours under the conditions of 80 DEG C；In terms of mass fraction, 5 parts of dehydrated alcohols are added
Into 20 parts of lignin, is stirred evenly with glass plate, lignin is diluted；0.8 part of graphite powder after dry is added to
It in lignin after dilution, is stirred evenly with glass plate, obtains the adhesive of graphitiferous powder.
(2) adhesive of graphitiferous powder is added in three-roll grinder (model S65) between back roller and central roll, it will
The distance between preliminary roller and central roll, central roll and back roller are adjusted to 0.4mm, carry out grinding 2h to the adhesive of graphitiferous powder, are made
Remove graphite powder.
(3) 30 min of ultrasound are carried out to removing graphite powder, then filtering is washed 3 times, then use deionized water with dehydrated alcohol
Washing, it is dry to get graphene.
The expanded graphites and graphene obtained used with scanning electron microscope (SEM) to the embodiment carry out respectively
Test, it is as shown in Figure 2,3 to the test result of expanded graphites, to the test result of graphene as shown in 4,5.The result shows that
Raw material expanded graphites thickness is very thick, is laminated by tens of thousands of layers of graphene；Graphene very thin thickness made from the embodiment, only
Including 2 ~ 3 layers, and the lamella quality of the graphene is good, remains original crystalline structure of graphite.
The expanded graphites and graphene obtained use to the embodiment carry out X-ray diffraction (XRD) test respectively, survey
Test result is as shown in fig. 6, the XRD curve of expanded graphites occurs a sharp high-intensitive characteristic peak, this category at 26.6 °
In 001 region feature peak of expanded graphites interlayer；And equally there is a weak peak here in graphene, apparent position does not occur
It moves, this illustrates that the removing of three-roller only changes the distance between lamella in graphite, and there is no quilts for the original crystalline structure of graphite
It destroys；It is stripped to obtain graphene.
The expanded graphites and graphene obtained use to the embodiment carry out thermogravimetric analysis (TGA) respectively, measure knot
Fruit is as shown in fig. 7, the initial thermal degradation of expanded graphites at 235 DEG C, and terminates, the mainly sulfuric acid of interlayer at 400 DEG C or so
The loss of hydroxyl and carboxyl on radical ion and graphite flake layer, final carbon left are 47.7%；And the initial thermal degradation of graphene exists
317 DEG C, then slowly weightless, final remaining carbon is 86.4%；It may be during the preparation process, to be lost a large amount of sulfate ions,
Cause only to exist on a small quantity in the high temperature process, therefore in high temperature section, expanded graphites can be expanded, and heating surface area becomes larger,
It is more sensitive to heat source, and graphene more has thermal stability.
In conclusion the grinding of three rollers is introduced the preparation process of graphene by the present invention with biological base adhesive combination technique,
Provide a kind of simple and quick method for preparing graphene.Adhesive used in the preparation method is natural glue, meets resource
Economizing type and environmentally friendly idea, and equipment needed for the preparation method is simple, the used time is short, and it is high-efficient, it is suitble to scale metaplasia
It produces.The lamella quality of graphene made from preparation method of the present invention is good, remains original crystalline structure of graphite, has
Very strong application.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of graphene, which is characterized in that comprising steps of
A, graphite powder is dried；Organic solvent is added into adhesive, stirs evenly, adhesive is diluted；Then
Dry graphite powder is added in the adhesive after dilution, is stirred evenly, the adhesive of graphitiferous powder is made；The adhesive
For biological base adhesive；
B, the adhesive of graphitiferous powder is added in three-roll grinder between back roller and central roll, adjust preliminary roller and central roll, in
The distance between roller and back roller grind the adhesive of graphitiferous powder, and removing graphite powder is made；
C, purification process is carried out to get graphene to removing graphite powder.
2. the preparation method of graphene according to claim 1, which is characterized in that in the step A, with mass fraction
Meter, dry graphite powder are 0.1 ~ 4 part, and organic solvent is 1 ~ 15 part, and adhesive is 10 ~ 50 parts.
3. the preparation method of graphene according to claim 1, which is characterized in that in the step A, the graphite powder choosing
One of self-expansion type graphite, natural graphite.
4. the preparation method of graphene according to claim 1, which is characterized in that in the step A, the graphite powder
Specification is 50 ~ 800 mesh.
5. the preparation method of graphene according to claim 1, which is characterized in that in the step A, the biology base rubber
Glutinous agent is selected from one of soybean protein, starch, lignin, pyrolysis bio-oils or a variety of.
6. the preparation method of graphene according to claim 1, which is characterized in that in the step A, the organic solvent
Selected from one or both of dehydrated alcohol, acetone.
7. the preparation method of graphene according to claim 1, which is characterized in that in the step B, the preliminary roller is in
The distance between roller, central roll and back roller are 0.1 ~ 1mm.
8. the preparation method of graphene according to claim 7, which is characterized in that in the step B, the preliminary roller is in
The distance between roller, central roll and back roller are identical.
9. the preparation method of graphene according to claim 1, which is characterized in that in the step C, the purification process
Specific steps include: to removing graphite powder carry out ultrasound, filtering, then washed 3 times with dehydrated alcohol, then be washed with deionized water
It washs, it is dry.
10. a kind of graphene, which is characterized in that the graphene by any graphene of claim 1-9 preparation side
Method is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811147266.3A CN109019577A (en) | 2018-09-29 | 2018-09-29 | A kind of graphene and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811147266.3A CN109019577A (en) | 2018-09-29 | 2018-09-29 | A kind of graphene and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109019577A true CN109019577A (en) | 2018-12-18 |
Family
ID=64614992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811147266.3A Pending CN109019577A (en) | 2018-09-29 | 2018-09-29 | A kind of graphene and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109019577A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111717912A (en) * | 2020-06-16 | 2020-09-29 | 华侨大学 | Device and method for preparing graphene through continuous stripping |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| 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 |
| US20140154941A1 (en) * | 2012-12-05 | 2014-06-05 | Aruna Zhamu | Unitary graphene matrix composites containing carbon or graphite fillers |
| JP2015012134A (en) * | 2013-06-28 | 2015-01-19 | 株式会社都ローラー工業 | Deposition method and deposition device of carbon-based material film |
| CN104495810A (en) * | 2014-12-10 | 2015-04-08 | 华侨大学 | Environmental-friendly method for large-scale preparation of graphene |
| CN106672951A (en) * | 2016-12-14 | 2017-05-17 | 北京化工大学 | Environment-friendly, high-efficiency and large-scale graphene preparation method |
| CN107459035A (en) * | 2017-05-25 | 2017-12-12 | 拜永孝 | A kind of large-scale preparation method of the controllable high-quality graphene of lamellar spacing |
| CN108163847A (en) * | 2018-01-12 | 2018-06-15 | 昂星新型碳材料常州有限公司 | The preparation method of large stretch of diameter graphene and large stretch of diameter graphene |
-
2018
- 2018-09-29 CN CN201811147266.3A patent/CN109019577A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| 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 |
| US20140154941A1 (en) * | 2012-12-05 | 2014-06-05 | Aruna Zhamu | Unitary graphene matrix composites containing carbon or graphite fillers |
| JP2015012134A (en) * | 2013-06-28 | 2015-01-19 | 株式会社都ローラー工業 | Deposition method and deposition device of carbon-based material film |
| CN104495810A (en) * | 2014-12-10 | 2015-04-08 | 华侨大学 | Environmental-friendly method for large-scale preparation of graphene |
| CN106672951A (en) * | 2016-12-14 | 2017-05-17 | 北京化工大学 | Environment-friendly, high-efficiency and large-scale graphene preparation method |
| CN107459035A (en) * | 2017-05-25 | 2017-12-12 | 拜永孝 | A kind of large-scale preparation method of the controllable high-quality graphene of lamellar spacing |
| CN108163847A (en) * | 2018-01-12 | 2018-06-15 | 昂星新型碳材料常州有限公司 | The preparation method of large stretch of diameter graphene and large stretch of diameter graphene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111717912A (en) * | 2020-06-16 | 2020-09-29 | 华侨大学 | Device and method for preparing graphene through continuous stripping |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10472243B2 (en) | Industrial method for preparing large-sized graphene | |
| KR101818703B1 (en) | Method for preparation of graphene by using pre-high speed homogenization and high pressure homogenization | |
| CN106185895A (en) | A kind of graphene dispersion liquid and preparation method thereof | |
| CN106410155B (en) | A kind of preparation method of graphene silica carbon negative pole material | |
| CN105590703B (en) | Can graphical three-dimensional grapheme/polyurethane flexible conductive film preparation method | |
| CN103922330A (en) | Method for preparing graphene powder by using dry process | |
| CN106276881B (en) | A kind of preparation method of graphene | |
| CN104386677B (en) | A kind of low-level oxidation Graphene and its preparation method | |
| CN104310383A (en) | Graphene nanosheet and preparation method thereof | |
| CN107628610A (en) | A kind of method that mechanical stripping method prepares graphene and graphene conductive liquid | |
| US20150133568A1 (en) | Method for preparing graphene from biomass-derived carbonaceous mesophase | |
| CN105776192B (en) | A kind of method for continuous preparation graphene microchip of being delaminated using grinding | |
| CN105858641B (en) | Graphene production method | |
| CN106882795A (en) | A kind of scale ultrasound stripping prepares the application of the method and Graphene of Graphene | |
| CN105967172A (en) | Preparation method of foldable graphene thin film of large area | |
| CN106009787A (en) | Graded dispersion method and device for preparing graphene-based waterborne dispersion liquid | |
| CN107393622B (en) | Graphene-titanium suboxide composite conductive agent and preparation method thereof | |
| Xu et al. | Exfoliation of graphite in CO2 expanded organic solvents combined with low speed shear mixing | |
| CN103466612A (en) | Method for preparing native grapheme by means of frequency mixing ultrasound | |
| CN106672951B (en) | A kind of environmental-friendly high efficiency can prepare with scale graphene method | |
| CN107032329A (en) | A kind of three-dimensional grapheme of nano-micrometre classification pore passage structure and preparation method thereof | |
| CN110203913A (en) | A method of preparing graphene | |
| CN109665518A (en) | A kind of preparation method of highly conductive graphene | |
| CN109019577A (en) | A kind of graphene and preparation method thereof | |
| CN109694056A (en) | A kind of method that liquid phase removing graphite oxide prepares graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181218 |