CN106315571A - Method for preparing high-concentration small-diameter graphene dispersion liquid - Google Patents
Method for preparing high-concentration small-diameter graphene dispersion liquid Download PDFInfo
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- CN106315571A CN106315571A CN201610671954.4A CN201610671954A CN106315571A CN 106315571 A CN106315571 A CN 106315571A CN 201610671954 A CN201610671954 A CN 201610671954A CN 106315571 A CN106315571 A CN 106315571A
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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
- C01B2204/28—Solid content in solvents
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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
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Abstract
The invention relates to a method for preparing high-concentration small-diameter graphene dispersion liquid and belongs to the technical field of nanometer novel materials. The method includes the steps that graphite powder serves as the raw material and is oxidized through the Hummers method to obtain oxidized graphite, then the obtained oxidized graphite is reduced, and the reduced oxidized graphite is obtained; the reduced oxidized graphite and solvent are mixed and placed into a ball milling tank to be ball-milled, and the reduced oxidized graphene dispersion liquid is obtained; the dispersion liquid is dried, the obtained product can be dispersed in water and various common polar solvents, and the graphene dispersion liquid can be configured according to concentration. The method is simple in process, economical and environmentally friendly, and the prepared graphene dispersion liquid can keep high-concentration stable dispersion.
Description
Technical field
The present invention relates to nanometer new material technology field, a kind of high concentration small flake diameter graphene dispersion
Preparation method.
Background technology
Graphene is to be irrigated by Univ Manchester UK physicist An Deliehaimu and Constantine's promise for 2004
Xiao Luofu is isolated a kind of bi-dimensional cellular shape lattice structure new material piled up by monolayer carbon atom precision from graphite,
It has a lot of excellent performance, the highest electron mobility 2 × 105m2/ (V s), the heat conductivility 5000W/ of superelevation
(m K), specific surface area 2630m of super large2/ g (calculated value) etc., therefore be constantly subjected to study from physics and Material Field
The generally favor of person, the studied battery that is applied to, capacitor, field-effect transistor, sensor, electromechanical resonator, polymer nano
Emerging, the traditional field such as nano composite material, electrochemical appliance, and light emitting devices.
In recent years, preparation high dispersive, Graphene that high concentration, hydrophilic or oleophylic and conduction are excellent have huge application
Demand.The main problem that researchers run at present is exactly, due to nano effect, between lamella and the lamella of Graphene
Being easily formed van der waals force effect, this causes Graphene to be difficult in higher concentrations, and long-time stable is deposited in a liquid, Graphene
The actual application of basic material is by the most limited.Researchers constantly explore in terms of graphene dispersion problem, probing direction master
Being divided into two big classes, the directly dispersion of a class research Graphene, another big class is to study to enter after the process of Graphene initial oxidation again
The dispersion of row.This two big class method all cuts both ways.The direct scattered method of Graphene, the conjugation result complete to Graphene is broken
Bad less, the excellent properties of Graphene can be kept, but owing to lacking good Interface adhesive strength, be difficult to accomplish that high concentration is steady
Fixed scattered graphene dispersing solution, such as Umar Khan et al. (KhanU, O'Neill A, Lotya M, et al.High
Concentration Solvent Exfoliation of Graphene [J] .Small, 2010,6 (7): 864-871.) grind
Having studied carefully a kind of method preparing high concentration graphene dispersion liquid, prepared dispersion liquid concentration can reach 1.2mg/ml, and monolayer contains
Amount can reach 4%.This method depends in N-methyl-2 ketopyrrolidine long-time lower powered ultrasonic, and ultrasonic time is
Up to 460h.But analysis and observation obtains the average-size of lamella still at more than 1um, the most ultrasonic be unfavorable for industrialized
Application.Mustafa Lotya(LotyaM,King P J,Khan U,et al.High-concentration,
surfactant-stabilized graphene dispersions[J].ACS nano,2010,4(6):3155-3162.)
Utilize surfactant sodium cholate, in water the most ultrasonic dispersed graphite alkene of peeling off of low-power, gained graphene dispersing solution
Concentration can reach 0.3mg/ml, and the concentration of the graphene dispersing solution that this method obtains still is difficult to meet application demand, and
The interpolation of surfactant have impact on graphene conductive performance.
And the method for Graphene initial oxidation redispersion is had a big advantage, after oxidation, the surface of Graphene is contained and is much contained
The polar group of oxygen, the existence of these polar groups can make graphene sheet layer and solvent produce stronger interaction force, with
High concentration is disperseed in a solvent.This method drawback can produce more defect exactly, affects the heat-conductivity conducting that Graphene is excellent
Energy.Such as Folke Johannes experimental group (FJ, Fabritius M, M ü lhaupt R.Emulsifier Free
Graphene Dispersions with High Graphene Content for Printed E lectronics and
Freestanding Graphene Films[J].Advanced Functional Materials,2012,22(6):1136-
1144.) under conditions of not using any surfactant, through peroxidating, high temperature reduction, the process of high pressure homogenizer, it is possible to
Obtain the redox graphene dispersion liquid at concentrations up to 15mg/ml, and dispersion liquid can prepare the thin film of conduction flexible.But its
Thin film prepared by dispersion liquid is affected by defect, does not show the due excellent electric property of Graphene.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of high concentration small flake diameter graphene dispersion, by the method system
The dispersion liquid obtained can either reach high concentration, meets application demand, ensure that again the satisfactory electrical conductivity of Graphene.
To achieve these goals, the present invention adopts the following technical scheme that
The preparation method of a kind of high concentration small flake diameter graphene dispersion, is achieved by the steps of:
1) first graphite powder Hummers method is oxidized and obtains graphite oxide；
2) then this graphite oxide is reduced, obtain reduction-oxidation graphite；
3) the above-mentioned reduction-oxidation graphite prepared and solvent are mixed that to obtain concentration be 0.01-10mg/ml's
Reduction-oxidation graphite suspension, loads this reduction-oxidation graphite suspension in the ball grinder of ball mill and carries out ball milling, pass through ball
Grind to peel off reduction-oxidation graphite flake layer and crush；Wherein, drum's speed of rotation controls at 30-500 rev/min, Ball-milling Time be 2～
300 hours；
4), after ball milling terminates, the redox graphene dispersion liquid of stable dispersion is i.e. obtained；By this redox graphene
Dispersion liquid is centrifuged, centrifugal rotational speed 100～15000 revs/min, the graphene film thick to remove unstripped sufficient comparison, and then
Obtain the sheet footpath redox graphene dispersion liquid less than 1um；
5) by 4) the abundant washing and drying of redox graphene dispersion liquid that step obtains, products therefrom is according to concentration requirement
It is scattered in common polar solvent, i.e. obtains high concentration small flake diameter graphene dispersion.
The raw material of above-mentioned graphite powder is native graphite, expansible graphite, expanded graphite, highly oriented graphite and thermal cracking graphite
In the mixture of one or more.
The method reduced by graphite oxide is the Microwave reduction method with thermal reduction as mechanism or high temperature reduction method, wherein, institute
The reaction temperature stating high temperature reduction method is 150～400 DEG C.
Above-mentioned solvent is METHYLPYRROLIDONE.
Above-mentioned solvent is by METHYLPYRROLIDONE and water, Methanamide, dimethyl sulfoxide, acetonitrile, N, N-dimethyl methyl
Amide, hexamethyl phosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butyl alcohol,
Dioxane, oxolane, methyl formate, tri-n-butylamine, butanone, ethyl acetate, trioctylamine, dimethyl carbonate, diisopropyl ether, three
The mixing that one or more in vinyl chloride, diphenyl ether, dichloromethane, chloroform, dichloroethanes are made into the ratio of 1～99:1 is molten
Agent.
The type of ball mill includes various planetary ball mill, agitating ball mill, tank abrading-ball grinding machine and horizontal ball mill.
The abrading-ball that ball mill is used is zirconium oxide balls, steel ball, Achates abrading-ball, aluminium oxide abrading-ball or silicon nitride abrading-ball.
Described common polar solvent is water, METHYLPYRROLIDONE, Methanamide, dimethyl sulfoxide, acetonitrile, N, N-bis-
Methylformamide, hexamethyl phosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine,
N-butyl alcohol, dioxane, oxolane, methyl formate, tri-n-butylamine, butanone, ethyl acetate, trioctylamine, dimethyl carbonate, second
The mixing of one or more in ether, diisopropyl ether, n-butyl ether, trichloro ethylene, diphenyl ether, dichloromethane, chloroform, dichloroethanes
Thing.
After using such scheme, compared with prior art, the invention have the advantages that
1) the inventive method prepares graphene dispersing solution technique simply, and equipment is simple, low cost, is suitable for large-scale production.
2) the scattered graphene dispersing solution of high-concentration stable can be obtained by the inventive method.We have prepared
Concentration is the dispersion liquid of 10mg/ml, fully meets application demand.Stability aspect, without substantially reunion, lamination in 1 year；
3) graphene dispersing solution prepared by the present invention, has peeled off into major part sheet by the structure of the graphite powder of three-dimensional order
The footpath monolayer 100～1000nm or the graphene film less than 5 layers.Product electric conductivity is excellent.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of the present invention；
Fig. 2 is the transmission electron micrograph of high concentration small flake diameter graphene dispersion.
Detailed description of the invention
The preparation method of the high concentration small flake diameter graphene dispersion of the present invention, its preparation flow is as shown in Figure 1.By this
The high concentration small flake diameter graphene dispersion that inventive method prepares, its transmission electron micrograph is as shown in Figure 2.
Embodiment 1:
2.0g natural graphite powder Hummers method is oxidized and obtains graphite oxide；By the graphite oxide that makes 45
Dry at a temperature of DEG C, take the 0.3g graphite oxide after drying and put into reaction 20 seconds in microwave reactor, obtain oxygen reduction fossil
Ink.Weigh 0.075g reduction-oxidation graphite, by itself and the mixing of 30ml METHYLPYRROLIDONE, obtain reduction-oxidation graphite and hang
Supernatant liquid.Take the Zirconia beads of zirconium content more than 97%, reduction-oxidation graphite suspension is loaded the ball grinder of planetary ball mill
In carry out ball milling, drum's speed of rotation controls the speed at 320 revs/min, peels off broken by reduction-oxidation graphite flake layer, during ball milling
Between be set to 5 hours.After ball milling terminates, i.e. obtain the reduced graphene dispersion liquid of the stable dispersion of black.For obtaining sheet footpath relatively
Little Graphene, redox graphene dispersion liquid is centrifuged by further, centrifugal rotational speed 6000 revs/min, set of time
It is 15 minutes, the graphene film thick to remove unstripped sufficient comparison, obtain the sheet footpath redox graphene less than 1um and divide
Dissipate liquid.Dispersion liquid derived above abundant washing and drying products therefrom, is dispersed among in water, and can be configured to according to needed for concentration
5.0mg/ml dispersion liquid.
Embodiment 2:
2.0g expansible graphite powder Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 that will make
DEG C dry, take 0.3g graphite oxide and put in the Muffle furnace being warming up to 150 DEG C 30 minutes, obtain reduction-oxidation graphite, many
The secondary reduction-oxidation graphite preparing q.s.Weigh 10g reduction-oxidation graphite, by its with 1000ml by N-methyl-2-pyrrole
The mixed solvent that pyrrolidone and water mix with the volume ratio of 9:1 mixes, and obtains reduction-oxidation graphite suspension.Take
Steel ball pearl, loads reduction-oxidation graphite suspension in the ball grinder of agitating ball mill and carries out ball milling, and drum's speed of rotation controls
The speed of 350 revs/min, being peeled off by reduction-oxidation graphite flake layer broken, Ball-milling Time is set to 300 hours.Ball milling terminates
After, i.e. obtain the reduced graphene dispersion liquid of the stable dispersion of black.The Graphene less for obtaining sheet footpath, we further will
Redox graphene dispersion liquid is centrifuged, and centrifugal rotational speed 2000 revs/min, set of time is 30 minutes, to remove unstripped filling
Point the thick graphene film of comparison, obtain the sheet footpath redox graphene dispersion liquid less than 1um.Dispersion liquid derived above fills
Divide washing and drying products therefrom, be dispersed among in METHYLPYRROLIDONE, and can be according to being configured to 10.0mg/ needed for concentration
Ml dispersion liquid.
Embodiment 3:
2.0g expansible graphite powder Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 that will make
DEG C dry, take 0.3g graphite oxide and put in the Muffle furnace being warming up to 300 DEG C 30 minutes, obtain reduction-oxidation graphite, many
The secondary reduction-oxidation graphite preparing q.s.Weigh 5g reduction-oxidation graphite, by its with 1000ml by N-methyl-2-pyrroles
The mixed solvent that alkanone and ethanol mix with the volume ratio of 9:1 mixes, and obtains reduction-oxidation graphite suspension.Take
Agate ball pearl, loads reduction-oxidation graphite suspension in tank abrading-ball grinding machine and carries out ball milling, and drum's speed of rotation controls 250
Rev/min speed reduction-oxidation graphite flake layer is peeled off broken, Ball-milling Time is set to 24 hours.After ball milling terminates, to obtain final product
Reduced graphene dispersion liquid to the stable dispersion of black.The Graphene less for obtaining sheet footpath, we are further by oxygen reduction
Functionalized graphene dispersion liquid is centrifuged, and centrifugal rotational speed 3000 revs/min, set of time is 15 minutes, to remove unstripped sufficient ratio
Thicker graphene film, obtains the sheet footpath redox graphene dispersion liquid less than 1um.Dispersion liquid derived above fully washs
Dry products therefrom, be dispersed among in DMF, and can be according to being configured to 10.0mg/ml dispersion needed for concentration
Liquid.
Embodiment 4:
2.0g expanded graphite Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 DEG C baking that will make
Dry, take 0.3g graphite oxide and put in the Muffle furnace being warming up to 400 DEG C 30 minutes, obtain reduction-oxidation graphite, repeatedly make
The standby reduction-oxidation graphite obtaining q.s.Weigh 3.75kg reduction-oxidation graphite, by its with 500L by N-methyl-2-pyrrolidine
The mixed solvent that ketone and acetone mix with the volume ratio of 9:1 mixes, the reduction-oxidation graphite suspension obtained.Take
Aluminium oxide pearl, loads in horizontal ball mill carry out ball milling by reduction-oxidation graphite suspension, drum's speed of rotation control 35 turns/
Minute speed, reduction-oxidation graphite flake layer is peeled off broken, Ball-milling Time is set to 72 hours.After ball milling terminates, i.e. obtain
The reduced graphene dispersion liquid of the stable dispersion of black.The Graphene less for obtaining sheet footpath, we are further by reduction-oxidation
Graphene dispersing solution is centrifuged, centrifugal rotational speed 4000 revs/min, and set of time is 15 minutes, unstripped sufficiently compares to remove
Thick graphene film, obtains the sheet footpath redox graphene dispersion liquid less than 1um.Dispersion liquid derived above fully washs baking
Dry products therefrom, is dispersed among in oxolane, and can be according to being configured to 1.0mg/ml dispersion liquid needed for concentration.
Embodiment 5:
Highly oriented for 2.0g graphite Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 DEG C that will make
Dry, take 0.3g graphite oxide and put into reaction 20 seconds in microwave reactor, obtain reduction-oxidation graphite.Weigh 0.3mg oxygen reduction
Graphite, mixes its mixed solvent mixed with the volume ratio of 9:1 by METHYLPYRROLIDONE and chloroform with 30ml
Together, reduction-oxidation graphite suspension is obtained.Take silicon nitride abrading-ball, reduction-oxidation graphite suspension is loaded planetary ball mill
Ball grinder in carry out ball milling, drum's speed of rotation controls the speed at 350 revs/min, peels off broken by reduction-oxidation graphite flake layer
Broken, Ball-milling Time is set to 96 hours.After ball milling terminates, i.e. obtain the reduced graphene dispersion liquid of the stable dispersion of black.For
Obtaining the Graphene that sheet footpath is less, redox graphene dispersion liquid is centrifuged by further, centrifugal rotational speed 5000 revs/min
Clock, set of time is 15 minutes, the graphene film thick to remove unstripped sufficient comparison, obtains the reduction less than 1um of the sheet footpath
Graphene oxide dispersion.Dispersion liquid derived above abundant washing and drying products therefrom, is dispersed among in dichloromethane, and can
According to being configured to 1.0mg/ml dispersion liquid needed for concentration.
Embodiment 6:
2.0g thermal cracking graphite Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 DEG C that will make
Dry, take 0.3g graphite oxide and put in the Muffle furnace being warming up to 200 DEG C 30 minutes, obtain reduction-oxidation graphite, repeatedly
Prepare the reduction-oxidation graphite of q.s.Weigh 1g reduction-oxidation graphite, by its with 1000ml by N-methyl-2-pyrrolidine
The mixed solvent that ketone and n-butyl alcohol mix with the volume ratio of 9:1 mixes, and obtains reduction-oxidation graphite suspension.Take
Steel ball pearl, loads reduction-oxidation graphite suspension in the ball grinder of agitating ball mill and carries out ball milling, and drum's speed of rotation controls
Being peeled off by reduction-oxidation graphite flake layer broken the speed of 210 revs/min, Ball-milling Time is set to 120 hours.Ball milling terminates
After, i.e. obtain the reduced graphene dispersion liquid of the stable dispersion of black.The Graphene less for obtaining sheet footpath, we further will
Redox graphene dispersion liquid is centrifuged, and centrifugal rotational speed 7000 revs/min, set of time is 15 minutes, to remove unstripped filling
Point the thick graphene film of comparison, obtain the sheet footpath redox graphene dispersion liquid less than 1um.Dispersion liquid derived above fills
Divide washing and drying products therefrom, be dispersed among in methanol, and can be according to being configured to 1.0mg/ml dispersion liquid needed for concentration.
Embodiment 7:
Highly oriented for 2.0g graphite Hummers method is oxidized and obtains graphite oxide；The graphite oxide 45 DEG C that will make
Dry, take 0.3g graphite oxide and put in the Muffle furnace being warming up to 240 DEG C 30 minutes, obtain reduction-oxidation graphite, repeatedly
Prepare the reduction-oxidation graphite of q.s.Weigh 10g reduction-oxidation graphite, by its with 1000ml by N-methyl-2-pyrroles
The mixed solvent that alkanone and DMF mix with the volume ratio of 9:1 mixes, and obtains reduction-oxidation
Graphite suspension.Taking agate ball pearl, loaded in tank abrading-ball grinding machine by reduction-oxidation graphite suspension and carry out ball milling, ball mill turns
Speed controls the speed at 150 revs/min, is peeled off by reduction-oxidation graphite flake layer broken, and Ball-milling Time is set to 200 hours.Ball
After mill terminates, i.e. obtain the reduced graphene dispersion liquid of the stable dispersion of black.The Graphene less for obtaining sheet footpath, Wo Menjin
Redox graphene dispersion liquid is centrifuged by one step, centrifugal rotational speed 15000 revs/min, and set of time is 15 minutes, to remove not
Peel off the thickest graphene film, obtain the sheet footpath redox graphene dispersion liquid less than 1um.Derived above divides
Dissipate liquid abundant washing and drying products therefrom, be dispersed among in methyl formate, and can divide according to being configured to 1.0mg/ml needed for concentration
Dissipate liquid.
Claims (8)
1. the preparation method of high concentration small flake diameter graphene dispersion, it is characterised in that be achieved by the steps of:
1) first graphite powder Hummers method is oxidized and obtains graphite oxide；
2) then this graphite oxide is reduced, obtain reduction-oxidation graphite；
3) the above-mentioned reduction-oxidation graphite prepared and solvent are mixed obtain the reduction that concentration is 0.01-10mg/ml
Graphite oxide suspension, loads this reduction-oxidation graphite suspension in the ball grinder of ball mill and carries out ball milling, will by ball milling
Reduction-oxidation graphite flake layer is peeled off broken；Wherein, drum's speed of rotation controls at 30-500 rev/min, and Ball-milling Time is 2～300
Hour；
4), after ball milling terminates, the redox graphene dispersion liquid of stable dispersion is i.e. obtained；This redox graphene is disperseed
Liquid is centrifuged, centrifugal rotational speed 100～15000 revs/min, the graphene film thick to remove unstripped sufficient comparison, and then obtains
The particle diameter redox graphene dispersion liquid less than 1um；
5) by 4) the abundant washing and drying of redox graphene dispersion liquid that obtains of step, products therefrom disperses according to concentration requirement
In common polar solvent, i.e. obtain high concentration small flake diameter graphene dispersion.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: above-mentioned stone
The raw material of powdered ink is one or more in native graphite, expansible graphite, expanded graphite, highly oriented graphite and thermal cracking graphite
Mixture.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: will oxidation
The method of graphite reduction is the Microwave reduction method with thermal reduction as mechanism or high temperature reduction method, wherein, and described high temperature reduction method
Reaction temperature is 150～400 DEG C.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: above-mentioned molten
Agent is METHYLPYRROLIDONE.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: above-mentioned molten
Agent is by METHYLPYRROLIDONE and water, Methanamide, dimethyl sulfoxide, acetonitrile, N,N-dimethylformamide, hempa
Amide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butyl alcohol, dioxane, tetrahydrochysene
Furan, methyl formate, tri-n-butylamine, butanone, ethyl acetate, trioctylamine, dimethyl carbonate, diisopropyl ether, trichloro ethylene, hexichol
The mixed solvent that one or more in ether, dichloromethane, chloroform, dichloroethanes are made into the ratio of 1～99:1.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: ball mill
Type include various planetary ball mill, agitating ball mill, tank abrading-ball grinding machine and horizontal ball mill.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: ball mill
The abrading-ball used is zirconium oxide balls, steel ball, Achates abrading-ball, aluminium oxide abrading-ball or silicon nitride abrading-ball.
The preparation method of high concentration small flake diameter graphene dispersion the most according to claim 1, it is characterised in that: described often
See that polar solvent is water, METHYLPYRROLIDONE, Methanamide, dimethyl sulfoxide, acetonitrile, N,N-dimethylformamide, pregnancy
Base phosphamide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butyl alcohol, dioxane,
Oxolane, methyl formate, tri-n-butylamine, butanone, ethyl acetate, trioctylamine, dimethyl carbonate, ether, diisopropyl ether, positive fourth
The mixture of one or more in ether, trichloro ethylene, diphenyl ether, dichloromethane, chloroform, dichloroethanes.
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Cited By (3)
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| CN109650385A (en) * | 2019-01-19 | 2019-04-19 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of high-purity high stable watersoluble plumbago alkene slurry of super-small and preparation method thereof |
| CN109761225A (en) * | 2019-03-30 | 2019-05-17 | 山东大学 | A kind of system based on Hydrodynamic cavitation and preparing grapheme through oxidation reduction |
| CN110511367A (en) * | 2019-08-20 | 2019-11-29 | 安徽神剑新材料股份有限公司 | A kind of polyester resin for powder coating of containing graphene |
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2016
- 2016-08-13 CN CN201610671954.4A patent/CN106315571A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650385A (en) * | 2019-01-19 | 2019-04-19 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of high-purity high stable watersoluble plumbago alkene slurry of super-small and preparation method thereof |
| CN109761225A (en) * | 2019-03-30 | 2019-05-17 | 山东大学 | A kind of system based on Hydrodynamic cavitation and preparing grapheme through oxidation reduction |
| CN110511367A (en) * | 2019-08-20 | 2019-11-29 | 安徽神剑新材料股份有限公司 | A kind of polyester resin for powder coating of containing graphene |
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Application publication date: 20170111 |