CN110015655A - A kind of ultra-high throughput stripping means of graphene - Google Patents
A kind of ultra-high throughput stripping means of graphene Download PDFInfo
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- CN110015655A CN110015655A CN201910057865.4A CN201910057865A CN110015655A CN 110015655 A CN110015655 A CN 110015655A CN 201910057865 A CN201910057865 A CN 201910057865A CN 110015655 A CN110015655 A CN 110015655A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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- 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
- C01B2204/32—Size or surface area
Abstract
The present invention relates to a kind of ultra-high throughput stripping means of graphene.Specifically: (1) aqueous solution or organic solvent solution of graphite or intercalated graphite and auxiliary agent are mixed, forms viscous paste；(2) the corresponding solvent of the viscous paste of formation is diluted, obtains graphene dispersing solution after stirring half an hour；(3) slurry in (1) or the dispersion liquid in (2) are dried, obtain addition agent modified graphene powder；(4) by product obtained in (3) under inert gas or vacuum condition high-temperature process, obtain pure graphene powder.Substantive characteristics of the invention is that it is removed concentration and is greater than 100 mg/mls, reaches as high as 600 mg/mls, is 10-100 times of conventional stripping methods.Safe preparation process of the present invention is controllable, high-efficient, is easy to industrial amplification, and not can cause environmental pollution.The method of the present invention is at low cost, efficiently solves the critical issue of graphene prepare with scale, to realize that the large-scale application of graphene is laid a good foundation.
Description
Technical field
The invention belongs to field of material technology, are related to a kind of ultra-high throughput stripping means of graphene.
Background technique
Since 2004 are found, graphene has caused academia and industrial circle with its excellent comprehensive performance
Extensive concern.The unique structural advantage of graphene imparts the properties such as its electricity abundant, optics, mechanics, energy conversion with
The fields such as storage, high-performance composite materials, biology have wide practical use.In order to realize the large-scale application of graphene, open
Issue it is a kind of be simple and efficient, low cost, low pollution preparation method seem most important.The preparation method of graphene can be divided into
Major class is measured from top to bottom and from bottom to top.It wherein, is that one kind is considered to have by the liquid phase stripping means of raw material of graphite ontology
The method from top to bottom of fine industrial prospect.This method is usually that graphite composite powder is dispersed in suitable organic solvent or surface-active
In agent aqueous solution, under the strong external force such as ultrasound, shearing or ball milling, the removing of graphene is realized.However, traditional liquid phase is shelled
Low from method flux, i.e., it is removed the lot of essential factors such as concentration, removing yield, dispersion concentration and is unable to satisfy industrialized needs.Mesh
Before, the highest of reported graphene removing concentration be 50 mg/mls (Nature Communications, (2018) 9:
76, DOI:10.1038/s41467-017-02580-3), and last handling process needs to expend a large amount of organic solvent, so that
Production cost is excessively high, it is difficult to realize volume production.Thus, the stone for developing high-throughput, low cost, being simple and efficient and being easy to industry amplification
Black alkene preparation method seems most important.
Summary of the invention
It is an object of the invention to overcome above-mentioned difficulties, a kind of ultra-high throughput stripping means of graphene is provided.The present invention
Using ball milling or the mode of action is sanded, removing concentration is high, and yield is close to 100 % and is able to maintain the complete crystal structure of graphene,
It is easy to industrial amplification.Graphene prepared by the present invention can be dispersed in water and other organic solvents, be can apply to energy storage, urged
The fields such as change, composite material.
The invention proposes a kind of ultra-high throughput stripping means of graphene, the specific steps are as follows:
(1) graphite composite powder or intercalated graphite are mixed with the organic solution of the aqueous solution of auxiliary agent or auxiliary agent, in ball mill or sand milling
It is reacted in machine, forms viscous paste；The graphite composite powder or intercalated graphite removing concentration are 100-600 mg/ml；Auxiliary agent
Dosage is 0.1-2 times of graphite composite powder or intercalated graphite quality；
(2) the viscous paste water obtained step (1) or the dilution of corresponding organic solution, stir 30 minutes, are formed stable
Graphene dispersing solution；
(3) viscous paste that step (1) obtains or the graphene dispersing solution that step (2) obtains are dried, are helped
The graphene powder of agent modification；
(4) product for obtaining step (3) high-temperature process under inert gas or vacuum condition, obtains pure graphene powder.
In the present invention, graphite raw material described in step (1) is having a size of 30-15000 mesh；The intercalated graphite includes Gao Meng
Sour potassium/sulfuric acid intercalated graphite, potassium permanganate/sulfuric acid/phosphoric acid intercalated graphite, nitric/sulfuric acid intercalated graphite or persulfate/sulfuric acid
It is any in intercalated graphite.
In the present invention, step (1) described auxiliary agent includes any in polyvinylpyrrolidone, polyethylene glycol or polyvinyl alcohol
Kind.
In the present invention, organic solvent described in step (1) includes ethyl alcohol, methanol, n,N dimethylformamide, N- methyl pyrrole
It is any in pyrrolidone or ethylene glycol.
In the present invention, sand mill revolving speed described in step (1) is 150-1600 revs/min, and it is that 0.5-24 is small that the time, which is sanded,
When；Drum's speed of rotation is 150-600 revs/min, and Ball-milling Time is 1-24 hours.
In the present invention, drying process described in step (3) includes spray drying, super closes on that carbon dioxide is dry, freezing is dry
It is any in dry, vacuum drying or forced air drying.
In the present invention, inert gas described in step (4) includes nitrogen or argon gas.
In the present invention, high-temperature process described in step (4) is the nitrogen by the addition agent modified graphene powder of gained at 700 DEG C
It anneals 1 hour in gas atmosphere, the heating rate in annealing process is 10 DEG C/min, and initial temperature is room temperature.
In view of the deficienciess of the prior art, the present inventor passes through long-term practice and research, skill of the invention is proposed
Art scheme, the program can realize the high throughput, low cost, large scale preparation of graphene, solve graphene prepare with scale
Critical issue, to realize practical application of the graphene in every field (such as energy storage material, composite material, catalysis, super lubrication)
Provide a kind of effective way.
The beneficial effects of the present invention are:
(1) the ultrahigh concentration removing of the achievable graphene of the present invention, removing concentration are greater than 100 mg/mls, and highest removes concentration
Greater than 600 mg/mls；
(2) present invention is able to achieve being completely exfoliated for graphene, and removing yield is handled close to 100% without further method classification.And
Stripping process will not destroy the lattice structure of graphene；
(3) the obtained graphene of present invention removing can in various solvents stable dispersion, store over 6 months still under normal temperature condition
It undergoes no deterioration, convenient for further application；
(4) the invention is simple and feasible, it can be achieved that graphene is completely exfoliated, and is easy to industrial amplification.And stripping process of the invention
It not can cause environmental pollution, be a kind of green stripping means；
(5) directly purchase business transition gold sulfide powders are raw material, and raw material sources are extensive, low in cost；
(6) present invention solves the critical issue of graphene prepare with scale, is that preparation is removed in the scale of two-dimension nano materials
Full technical strategies are provided, by the very big practical application for pushing graphene.
Detailed description of the invention
Fig. 1 is removing gained graphene transmission electron microscope photo.As seen from the figure, the size of obtained graphene film is 500
Nanometer or more, transparent appearance illustrates that obtained is few layer graphene.
Fig. 2 is the high-resolution-ration transmission electric-lens photo of removing gained graphene.As seen from the figure, the obtained graphene film number of plies
Less than 5 nanometers.
Fig. 3 is the number of plies statistical chart of removing gained graphene.As seen from the figure, the number of plies of graphene is at 5 nanometers hereinafter, super
The graphene film for crossing 80% is layer 2-4 structure.
Specific embodiment
Illustrate technical solution of the present invention below by way of specific example.It should be understood that the one or more that the present invention mentions
Step do not repel before and after the combination step there is also between other method and steps or these specifically mentioned steps also
Other method and steps can be inserted.It should also be understood that these examples are merely to illustrate the present invention rather than limitation is of the invention
Range.Unless otherwise indicated, the number of various method steps is only the purpose of identification various method steps, rather than to limit each method
Arrangement order or limit practical range of the invention, relativeness is altered or modified, in no substantial technological content alteration
Under conditions of, when being also considered as the enforceable scope of the present invention.
Embodiment 1
(1) 5 grams of polyvinylpyrrolidones are dissolved under agitation in 25 ml deionized waters, it until completely dissolved, will be molten
(1000 mesh of graphite raw material, 95%) phosphorus content, which is higher than, to be added in ball grinder, after ball milling pearl is added, 300 for liquid and 5 grams of powder graphites
20 h of ball milling, obtains viscous paste under the conditions of rpm；
(2) after diluting viscous paste obtained in (1) with 480 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(3) by dispersion liquid freeze-drying process obtained in (2), polyvinyl pyrrolidon modified graphene powder is obtained, it will
Gained powder is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process
For 10 DEG C/min, initial temperature is room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 2
(1) 30 grams of potassium permanganate are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
It places reaction liquid into 35 C water baths, 30 grams of crystalline flake graphites are added into reaction solution, and (30 mesh of graphite raw material, phosphorus content are higher than
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) 5 grams of polyvinylpyrrolidones are dissolved under agitation in 25 ml deionized waters, it until completely dissolved, will be molten
(5000 mesh of graphite raw material, 95%) phosphorus content is higher than to be added in ball grinder intercalated graphite in liquid and 10 grams (1), and ball milling pearl is added
Afterwards, ball milling 20 hours under the conditions of 350 revs/min, viscous paste is obtained；
(3) after diluting viscous paste obtained in (1) with 600 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(4) by dispersion liquid freeze-drying process obtained in (2), polyvinyl pyrrolidon modified graphene powder is obtained, it will
Gained powder is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process
For 10 DEG C/min, initial temperature is room temperature；After taking off fire, sample natural cooling in nitrogen atmosphere.
Embodiment 3
(1) 5 grams of polyethylene glycol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 10
(15000 mesh of graphite raw material, 95%) phosphorus content, which is higher than, to be added in ball grinder, after ball milling pearl is added, at 300 revs/min for gram powder graphite
Ball milling 10 hours, obtain viscous paste under the conditions of clock；
(2) after diluting viscous paste obtained in (1) with 800 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(3) by dispersion liquid freeze-drying process obtained in (2), polyethyleneglycol modified graphene powder is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 4
(1) 30 grams of ammonium persulfates are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
It places reaction liquid into 35 DEG C of water-baths, 30 grams of crystalline flake graphites are added into reaction solution, and (100 mesh of graphite raw material, phosphorus content are higher than
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) 5 grams of polyethylene glycol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 10
(5000 mesh of graphite raw material, 95%) phosphorus content is higher than to be added in sand mill intercalated graphite in gram (1), after mill pearl is added, 1600
Ball milling 20 hours, obtain viscous paste under the conditions of rev/min；
(3) after diluting viscous paste obtained in (1) with 600 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(4) by dispersion liquid freeze-drying process obtained in (2), polyethyleneglycol modified graphene powder is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 5
(1) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 5 grams
(1000 mesh of graphite raw material, 95%) phosphorus content is higher than to be added in ball grinder powder graphite, after ball milling pearl is added, at 150 revs/min
Under the conditions of ball milling 20 hours, obtain viscous paste；
(2) after diluting viscous paste obtained in (1) with 480 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(3) by dispersion liquid freeze-drying process obtained in (2), the graphene powder of polyvinyl alcohol modification is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 6
(1) 30 grams of potassium permanganate are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
Place reaction liquid into 35oIn C water-bath, into reaction solution, (100 mesh of graphite raw material, phosphorus content are higher than 30 grams of crystalline flake graphites of addition
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 ml deionized waters, until completely dissolved, by solution and 10
In gram (1) intercalated graphite (5000 mesh of graphite raw material, 95%) phosphorus content, which is higher than, to be added in ball grinder, after ball milling pearl is added,
Ball milling 20 hours, obtain viscous paste under the conditions of 350 revs/min；
(3) after diluting viscous paste obtained in (1) with 600 ml deionized waters, stirring obtains graphene dispersion in 30 minutes
Liquid；
(4) by dispersion liquid freeze-drying process obtained in (2), the graphene powder of polyvinyl alcohol modification is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 7
(1) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 milliliters of ethyl alcohol, until completely dissolved, by solution and 5 grams of powder
(1000 mesh of graphite raw material, 95%) phosphorus content is higher than to be added in sand mill graphite, after mill pearl is added, under the conditions of 150 revs/min
Ball milling 20 hours, obtain viscous paste；
(2) after diluting viscous paste obtained in (1) with 480 milliliters of ethyl alcohol, stirring obtains graphene dispersing solution in 30 minutes；
(3) by dispersion liquid spray drying treatment obtained in (2), the graphene powder of polyvinyl alcohol modification is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 8
(1) 30 grams of potassium permanganate are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
Place reaction liquid into 35oIn C water-bath, into reaction solution, (100 mesh of graphite raw material, phosphorus content are higher than 30 grams of crystalline flake graphites of addition
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 milliliters of ethyl alcohol, until completely dissolved, by solution and 10 grams (1)
In intercalated graphite (5000 mesh of graphite raw material, phosphorus content be higher than 95%) be added ball grinder in, be added ball milling pearl after, 350 turns/
Ball milling 20 hours under the conditions of minute, viscous paste is obtained；
(3) after diluting viscous paste obtained in (1) with 600 milliliters of ethyl alcohol, stirring obtains graphene dispersing solution in 30 minutes；
(4) by dispersion liquid spray drying treatment obtained in (2), the graphene powder of polyvinyl alcohol modification is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 9
(1) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 milliliters of N-Methyl pyrrolidones, it until completely dissolved, will be molten
(1000 mesh of graphite raw material, 95%) phosphorus content, which is higher than, to be added in ball grinder, after ball milling pearl is added, 300 for liquid and 5 grams of powder graphites
Ball milling 20 hours, obtain viscous paste under the conditions of rev/min；
(2) after diluting viscous paste obtained in (1) with 480 milliliters of N-Methyl pyrrolidones, stirring obtains graphite in 30 minutes
Alkene dispersion liquid；
(3) dispersion liquid supercritical carbon dioxide obtained in (2) is dried, obtains the Graphene powder of polyvinyl alcohol modification
Body, by gained powder 700oIt anneals 1 hour in the nitrogen atmosphere of C, obtains pure graphene powder.Heating in annealing process
Rate is 10 DEG C/min, and initial temperature is room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Embodiment 10
(1) 30 grams of potassium permanganate are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
Place reaction liquid into 35oIn C water-bath, into reaction solution, (100 mesh of graphite raw material, phosphorus content are higher than 30 grams of crystalline flake graphites of addition
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) 5 grams of polyvinyl alcohol are dissolved under agitation in 25 milliliters of N-Methyl pyrrolidones, it until completely dissolved, will be molten
(5000 mesh of graphite raw material, 95%) phosphorus content is higher than to be added in ball grinder intercalated graphite in liquid and 10 grams (1), and ball milling pearl is added
Afterwards, ball milling 20 hours under the conditions of 350 revs/min, viscous paste is obtained；
(3) after diluting viscous paste obtained in (1) with 600 milliliters of ethyl alcohol, stirring obtains graphene dispersing solution in 30 minutes；
(4) by dispersion liquid spray drying treatment obtained in (2), the graphene powder of polyvinyl alcohol modification is obtained, by gained powder
Body is annealed 1 hour in 700 DEG C of nitrogen atmosphere, obtains pure graphene powder.Heating rate in annealing process is 10 DEG C/
Min, initial temperature are room temperature；After annealing, sample natural cooling in nitrogen atmosphere.
Comparative example 1
(1) 20 ml deionized waters and 10 grams of powder graphites are added in ball grinder, after ball milling pearl is added, in 300 revs/min of items
Ball milling 20 hours, obtain slurry under part；
(2) after slurry obtained in (1) being diluted with 480 ml deionized waters, stratification after stirring 30 minutes.Upper layer is stripping
From graphene dispersing solution, lower layer is the graphite not being completely exfoliated.The result shows that only a small amount of graphene is peeled away.
Comparative example 2
(1) 30 grams of potassium permanganate are slowly added under the conditions of ice-water bath in the nitration mixture of 300 milliliters of concentrated sulfuric acids, after mixing,
It places reaction liquid into 35 DEG C of water-baths, 30 grams of crystalline flake graphites are added into reaction solution, and (100 mesh of graphite raw material, phosphorus content are higher than
95%) it, is reacted 1 hour under lasting stirring condition；Reaction solution is slowly added in ice water, with 3# sand core funnel in vacuum condition
Lower filtering reacting liquid, discards filtrate, and deionized water is added into filtering gained hygrometric state solid, is so repeated several times, obtains intercalation
Graphite；
(2) intercalated graphite in 20 milliliters of N-Methyl pyrrolidones and 10 grams (1) is added in ball grinder, after ball milling pearl is added,
Ball milling 20 hours, obtains slurry under the conditions of 300 revs/min；
(3) after slurry obtained in (1) being diluted with 480 ml deionized waters, stratification after stirring 30 minutes.Upper layer is stripping
From graphene dispersing solution, lower layer is the graphite not being completely exfoliated.The result shows that only a small amount of graphite is peeled away.
Claims (8)
1. a kind of ultra-high throughput stripping means of graphene, it is characterised in that specific step is as follows:
(1) graphite composite powder or intercalated graphite are mixed with the organic solution of the aqueous solution of auxiliary agent or auxiliary agent, in ball mill or sand milling
It is reacted in machine, forms viscous paste；The graphite composite powder or intercalated graphite removing concentration are 100-600 mg/ml；Auxiliary agent
Dosage is 0.1-2 times of graphite composite powder or intercalated graphite quality；
(2) the viscous paste water obtained step (1) or the dilution of corresponding organic solution, stir 30 minutes, are formed stable
Graphene dispersing solution；
(3) viscous paste that step (1) obtains or the graphene dispersing solution that step (2) obtains are dried, are helped
The graphene powder of agent modification；
(4) product for obtaining step (3) high-temperature process under inert gas or vacuum condition, obtains pure graphene powder.
2. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that the graphite is former
Material is having a size of 30-15000 mesh；The intercalated graphite includes potassium permanganate/sulfuric acid intercalated graphite, potassium permanganate/sulfuric acid/phosphoric acid
It is any in intercalated graphite, nitric/sulfuric acid intercalated graphite or persulfate/sulfuric acid intercalated graphite.
3. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that the auxiliary agent includes
It is any in polyvinylpyrrolidone, polyethylene glycol or polyvinyl alcohol.
4. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that described is organic molten
Agent includes any in ethyl alcohol, methanol, n,N dimethylformamide, N-Methyl pyrrolidone or ethylene glycol.
5. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that described in step (1)
Sand mill revolving speed is 150-1600 revs/min, and it is 0.5-24 hours that the time, which is sanded,；Drum's speed of rotation is 150-600 revs/min
Clock, Ball-milling Time are 1-24 hours.
6. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that step (3) is described dry
Dry processing includes spray drying, supercritical carbon dioxide is dry, is freeze-dried, is any in vacuum drying or forced air drying.
7. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that described in step (4)
Inert gas includes nitrogen or argon gas.
8. a kind of ultra-high throughput stripping means of graphene according to claim 1, it is characterised in that described in step (4)
High-temperature process is that the addition agent modified graphene powder of gained is annealed 1 hour in 700 DEG C of nitrogen atmosphere, in annealing process
Heating rate is 10 DEG C/min, and initial temperature is room temperature.
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| CN113817222A (en) * | 2021-09-15 | 2021-12-21 | 南京林业大学 | Method for improving dispersion degree of graphene powder and preparation of modified asphalt |
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