CN106542529A - A kind of method that green prepares high-quality graphene - Google Patents
A kind of method that green prepares high-quality graphene Download PDFInfo
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Abstract
The invention discloses a kind of method that green prepares high-quality graphene, pretreating graphite is prepared graphene oxide in the basic conditions, and photoreduction is carried out to graphene oxide water solution with reference to uv analyzer and obtain high-quality graphene.The present invention compared with prior art, has an advantage in that：1) graphite is pre-processed, is conducive to graphite oxidation completely and large-sized graphene oxide is obtained, furthermore contribute to uniformly graphene oxide dispersion is fully peeled off under soft mechanical agitation.2) graphene oxide is prepared under alkaline solution, it is to avoid the use of a large amount of concentrated sulfuric acids, reduce the discharge of the three wastes, environmental protection.3) present invention adopts ultraviolet lighting redox graphene, in reduction process, loaded down with trivial details operating procedure and with low cost is not needed, while it also avoid the use of toxic reducing agent, high-quality, large-sized Graphene is prepared for industrial green and is provided potential using value.
Description
Technical field
The present invention relates to a kind of environmental protection, the method that simple operation prepares high-quality graphene.
Background technology
Graphene is that carbon atom is based on sp2The hexagonal honey comb structure of hydridization composition, the two dimension of only one atomic layers thick are brilliant
Body.After its Shi Tan family relays fullerene and CNT, the new allotrope material of the another carbon being found.In carbon man
In race member, realize from the fullerene of three-dimensional diamond, graphite to one-dimensional CNT and zero dimension, only two dimension knot
The carbon crystal of structure is undiscovered always, and this blank has just been filled up in the appearance of Graphene.Although it is 2004 that mono-layer graphite is dilute
Just it is separated first, but as its unique property excites the research interest of countless scientific research authors, and past short
Extensive research has been obtained in short several years.And Andre Geim and Konstantin Novoselov is also because in terms of Graphene
Start sex work and obtain Nobel Prize in physics in 2010.
Because Graphene has unique crystal structure, present at aspects such as electricity, optics, calorifics, mechanics excellent
Performance, has extensively in fields such as nanometer electronic device, high sensitive sensor, nesa coating, functional composite material, energy storage, catalysis
Wealthy application prospect.The main preparation method of Graphene has mechanical stripping method, chemical vapour deposition technique, seal to cut transfer at present
Method for printing, SiC pyrolysismethods, oxidation-reduction method, organic synthesis method etc..Industrially generally use mechanical stripping method, SiC pyrolysismethods,
Oxidation dispersion reducing process, these methods are simply extensive, be relatively adapted to produce in enormous quantities, but shortcoming is substantially, became uneven, quality
It is not high.Graphene is due to its huge potentiality so that future is likely to by large-area applications.The scientist of various countries is exerting
Power develops graphene device.And above all raw material --- Graphene, how to prepare high-quality Graphene and be always one
Individual important research topic, and production method industrial at present can not overcome a difficult problem for low defect always.
The content of the invention
It is an object of the invention to overcome prior art to prepare the defect of Graphene presence, the present invention provide a kind of environmental protection,
Low cost, the method for preparing high-quality graphene of process is simple, are that this is significant for Graphene is prepared on a large scale.
The environmentally friendly method for preparing high-quality graphene that the present invention is provided.By pretreating graphite in alkalescence condition
Under prepare graphene oxide and avoid a large amount of concentrated sulfuric acids and use, and adopt ultraviolet lighting redox graphene, not only avoid making
With poisonous reducing agent in reduction process and simple to operate in whole reduction process, safety is easy to control, with low cost, greatly reduces
The discharge of the three wastes, provides potential using value for Graphene industrialization.
A kind of method for preparing Graphene disclosed by the invention, comprises the steps：
1) graphite raw material pretreatment：After graphite raw material and organic solvent stir process, filter, by Graphite Cake in indifferent gas
The lower high-temperature process of body protection；
2) graphite oxidation is processed：By step 1) pretreated graphite with pro-oxidant add aqueous slkali be placed in confined air
In, oxygen is filled with into confined space reacted to certain pressure, reaction carries out separation of solid and liquid after terminating, and solid phase is aoxidized
Graphene；
3) graphene oxide reduction：By step 2) graphene oxide for preparing is configured to graphene oxide water solution, adjusts
PH, ultraviolet light graphene oxide water solution are reduced；
4) post-process：Step 3) after reduction completely, filtration drying obtains graphene powder.
Used as a kind of more specifically commercial Application, a kind of specific scheme of the present invention is：One kind prepares high-quality graphene
Method, at relatively high temperatures, under normal pressure or high pressure, use organic solvent pretreatment graphite, under inert gas shielding, high temperature burn
Burn pretreating graphite；Add alkali soluble agent to be placed in closed container the graphite of pretreatment, pro-oxidant, held with replacement of oxygen
Gas oxygen being filled with to certain pressure and being reacted in uniform temperature in device, reaction takes out product soft after terminating
Mechanism under be again stirring for so as to fully peel off and form separation of solid and liquid after uniform graphene oxide dispersion, gained is solid
Mutually wash and dry graphene oxide solid product, the graphene oxide for weighing certain mass is configured to the aqueous solution, with inorganic
Strong acid adjusts its pH value<7, fixed wave length irradiation graphene oxide water solution is pressed using uv analyzer, until reduction reaction is complete
Entirely, high-quality graphene powder is obtained after filtration drying.
Used as a kind of more specifically commercial Application, present invention one kind more specifically scheme is：One kind prepares high-quality graphite
The method of alkene, comprises the following steps that：
1) graphite raw material and organic solvent are added into autoclave, uniform temperature is set and heating stirring number is little
When, controlling reaction temperature；
2) mixture in reactor is taken out after cooling down, is filtered, by Graphite Cake under inert gas shielding and advance
Certain hour is processed at a temperature of setting；
3) weighing the above-mentioned pretreated graphite of certain mass, pro-oxidant adds aqueous slkali to be placed in closed container
It is interior, with replacement of oxygen gas in container and oxygen is filled with to certain pressure, is reacted at a temperature of pre-setting, react
Take out product to be again stirring under soft mechanism after end so as to fully peel off and form uniform graphene oxide
Separation of solid and liquid after dispersion liquid, gained solid phase are washed and are dried, and obtain high-quality graphene oxide solid product, and liquid phase is reclaimed at Jing
Reason Posterior circle is used；
4) graphene oxide for weighing the certain mass of above-mentioned preparation is configured to graphene oxide water solution, adjusts oxidation stone
The pH value of black aqueous solution, fixes ultraviolet wavelength irradiation graphene oxide water solution using uv analyzer, until reduction is anti-
Should be complete；
5) by above-mentioned reduction reaction completely graphene aqueous solution, it is vacuum dried after filtration, obtains high-quality graphene powder.
Graphite raw material used by the present invention can be one or more in existing any kind of graphite as raw material,
Such as native graphite, artificial synthesized graphite, micro crystal graphite, highly oriented pyrolytic graphite etc., in order to preferably realize the present invention, preferably
Graphite raw material of the graphite specification for 50-1000 mesh, more preferably 200-700 mesh, most preferably 300-600 mesh.
Organic solvent used by the present invention, can be any organic solvent not reacted with graphite raw material, such as replace
Or unsubstituted amides compound, sulfoxide compound, ester type compound etc.；It is preferred that N-METHYLFORMAMIDE, gamma-butyrolacton,
Dimethyl sulfoxide (DMSO), dimethyl sulfoxide (DMSO), N,N-dimethylformamide, N, any one or a few in N- DEFs.
In the present invention, graphite raw material is not specially required with pressure during organic solvent stir process, normal pressure or condition of high voltage
Under be capable of achieving, in order to shorten the stir process time, preferred condition of high voltage, such as 20-60mPa, more preferably pressure be 40mPa.
Temperature in the present invention when graphite raw material and organic solvent stir process is 100～260 DEG C, preferred 110-220 DEG C,
The time of process is 2～5h.
In the present invention under inert gas shielding process when temperature be 200-700 DEG C, preferred 300-550 DEG C, during process
Between be 1-3h.
Inert gas used by the present invention not only includes that (IUPAC newly specifies, i.e., for the gas of 18 races on the periodic table of elements
0 race originally), also including other any gases for being difficult to react with raw material, such as nitrogen, hydrogen etc., preferred nitrogen, argon gas
Or the mixing of one or more in hydrogen.
Pro-oxidant used by the present invention is nitrate, such as potassium nitrate, sodium nitrate, ammonium nitrate, calcium nitrate, plumbi nitras etc.,
It is preferred that potassium nitrate, sodium nitrate.
Aqueous slkali of the present invention is hydroxide, such as potassium hydroxide, NaOH, lithium hydroxide or calcium hydroxide.
During graphite oxidation of the present invention, it is to realize more preferable oxidation effectiveness, is preferably first fallen in container with replacement of oxygen
Gas, then proceedes to be filled with oxygen and is reacted to certain pressure；Preferred pressure is 3～20MPa, more preferably 4～15MPa,
Further preferred 5～10MPa.
During graphite oxidation of the present invention, the post-reacted temperature of oxygen is filled with for 100～700 DEG C, preferably 400～550 DEG C,
More preferably 450～500 DEG C.
Graphene oxide can be peeled off by mechanism after terminating and uniformly be disperseed by graphite oxidation reaction of the present invention
Carry out separation of solid and liquid after liquid again；The preferably soft mechanism of the mechanism, such as stirring at low speed, preferred stir speed (S.S.) is
150-250r/min, more preferably stir speed (S.S.) are 200r/min.
Liquid phase after separation of solid and liquid of the present invention can be to reclaim Jing after processing, and recovery and treatment method is preferably by liquid phase
The concentration of alkali is adjusted to after before reaction, the concentration of alkali is identical in aqueous slkali, is used as caustic solution circulation.
In the inventive method, the concentration of the graphene oxide water solution configured by reduction process does not have particular/special requirement, but is
More preferable effect, preferred concentration are 0.5～1.5mg/mL, more preferably 1mg/mL.
It is the reagent that can be used for adjusting pH in chemistry that the present invention adjusts graphene oxide water solution pH agents useful for same, such as without
Machine strong acid, preferably phosphoric acid, sulfuric acid or hydrochloric acid.
The present invention adjusts graphene oxide water solution pH<7, preferred pH are 3～5.
The wavelength of ultraviolet light of the present invention is 200-300nm, preferred 254nm.
For achieving the above object, the present invention further specifically discloses a kind of method that green prepares high-quality graphene,
Comprise the steps：
Step 1：The graphite raw material for weighing certain preparation is mixed with the organic solvent of certain volume in addition autoclave,
A few hours are processed at pre-set temperature, is graphite layers away from having expanded.Described organic solvent can be N- first
Base formamide, gamma-butyrolacton, dimethyl sulfoxide (DMSO), dimethyl sulfoxide (DMSO), N,N-dimethylformamide, N, in N- DEFs
Any one or a few.The mesh number of graphite powder is 50～1000 mesh；
Step 2：Take out the graphite that step 1 is handled well with organic solvent, cooled and filtered, by Graphite Cake in inert gas
Protection under high-temperature process a few hours, remove may residual organic solvent or catabolite；
Step 3：Weigh graphite, pro-oxidant and the aqueous slkali solute of certain mass step 2 pretreatment and load reactor
In, and add the deionized water stirring certain hour capping kettle of certain volume.Repeatedly replaced with oxygen after reactor sealing
Gas reactor, then fill oxygen to certain pressure, it is warming up to the temperature stirring a few hours for pre-setting；
Step 4：Take out step 3 reactant and certain hour is again stirring under soft mechanism so as to fully peel off
Separation of solid and liquid after uniform graphene oxide dispersion is formed, gained solid phase is washed and is dried, and obtains high-quality graphene oxide
Solid product, aqueous slkali reclaim Jing and process Posterior circle use；
Step 5：The graphene oxide for weighing certain mass is configured to the aqueous solution, and adjusts graphene oxide with inorganic acid
The pH value of the aqueous solution, fixes ultraviolet wavelength irradiation graphene oxide water solution using uv analyzer, until reduction is complete.
Step 6：By above-mentioned reduction reaction completely graphene aqueous solution, it is vacuum dried after filtration, obtains high-quality graphene
Powder.
In sum, the invention provides a kind of environmentally friendly method for preparing Graphene.The present invention will pre-process stone
Ink prepares graphene oxide in the basic conditions, and carries out photoreduction to graphene oxide water solution with reference to uv analyzer and obtain
High-quality graphene.The present invention is pre-processed to graphite first, and reason is that the interlamellar spacing for making graphite increases, and is conducive to graphite
Oxidation completely and is obtained large-sized graphene oxide, furthermore contributes to fully to peel off under soft mechanical agitation equal
Even graphene oxide dispersion.The present invention prepares graphene oxide under alkaline solution, it is to avoid the use of a large amount of concentrated sulfuric acids,
Reduce the discharge of the three wastes, environmental protection.Additionally, the oxygen-containing functional group that hydroxide ion is easy to graphite oxide forms chemical bond,
Intercalation is formed, graphene oxide is equally also contributed to and is peeled off under follow-up gentle mechanical agitation effect.In addition, adjusting oxidation stone
Black aqueous solution pH value<7, it is because in pH value<Under conditions of 7, the lamella of graphene oxide will not be destroyed.The present invention relates to
Graphene is prepared to ultraviolet lighting redox graphene, its principle is that ultraviolet lighting is to provide energy, irradiation oxidation
Graphene aqueous solution can form electronics, and an electrons wrap up four hydrones, or 8 hydrones, form aqueous electron, water
Closing electronics has very strong reproducibility, so as to redox graphene.In redox graphene process, it is not necessary to loaded down with trivial details operation
Step and with low cost, while it also avoid the use of toxic reducing agent, is that industrial green prepares high-quality, large-sized
Graphene provides strong using value.
Specific embodiment
Below by way of specific concrete example explanation technical scheme.It should be understood that these embodiments are only used for
The bright present invention rather than restriction the scope of the present invention.It should be noted that to those skilled in the art, not
On the premise of departing from present inventive concept, some deformations and improvement can also be made.These belong to protection scope of the present invention.
Embodiment 1
The 400 mesh natural flake graphites for weighing 0.5g and the N,N-dimethylformamide solvent for measuring 10mL add high pressure anti-
In answering kettle, high-temperature is risen to 170 DEG C, control reaction temperature and add stirring 4h.The mixture taken out after cooling in reactor enters
Row is filtered, by Graphite Cake in N2Under protection, 500 DEG C of process 2h, to remove the organic solvent or catabolite of residual.Weigh
The pretreating graphite of 0.3g, 4gKOH, 0.3gNaNO3It is placed in reactor, adds 30ml deionized waters, stirs 15mins.Sealing
With replacement of oxygen gas reactor 3 times after reactor, then oxygen is rushed to 5MPa, rise high-temperature to 500 DEG C, stir 40h.Will after cooling
Take out reactant and separation of solid and liquid after 2h is stirred under soft mechanical agitation, solid product is first washed with 5% Jing watery hydrochloric acid, then
After deionized water is washed till neutrality, 100 DEG C are vacuum dried to obtain graphene oxide solid.Weigh 0.1g graphene oxides and be configured to water
Solution, the pH value that graphene oxide water solution is adjusted with HCL is 3, is measured in the vial of 3ml graphene aqueous solutions to 5ml,
Horizontal lying-type is put into the uv analyzer of dark box type four, adjusts ultraviolet wavelength and is 254nm and is shone apart from fluorescent lamp 5cm positions
Penetrate reduction 40h.Finally by the graphene aqueous solution of reaction reduction, it is vacuum dried after filtration, obtains high-quality graphene powder.
Embodiment 2
During the 400 mesh natural flake graphites for weighing 0.5g and the gamma-butyrolacton solvent for measuring 10mL add autoclave,
High-temperature is risen to 210 DEG C, reaction temperature is controlled and is added stirring 3h.The mixture taken out after cooling in reactor is filtered,
By Graphite Cake in N2Under protection, 450 DEG C of process 2h, to remove the organic solvent or catabolite of residual.Weigh 0.2g's
Pretreating graphite, 4gKOH, 0.2gNaNO3It is placed in reactor, adds 30ml deionized waters, stirs 15mins.Sealed reactor
Afterwards with replacement of oxygen gas reactor 3 times, then oxygen is rushed to 6MPa, rise high-temperature to 500 DEG C, stir 40h.To take out after cooling anti-
Answer thing that separation of solid and liquid after 2h is stirred under soft mechanical agitation, solid product first washed with 5% Jing watery hydrochloric acid, then spend from
After son is washed to neutrality, 100 DEG C are vacuum dried to obtain graphene oxide solid.Weigh 0.1g graphene oxides and be configured to the aqueous solution, use
It is 4 that HCL adjusts the pH value of graphene oxide water solution, is measured in the vial of 3ml graphene aqueous solutions to 5ml, horizontal lying-type
Be put into the uv analyzer of dark box type four, adjust ultraviolet wavelength and be 254nm and be irradiated reduction apart from fluorescent lamp 5cm positions
42h.Finally by the graphene aqueous solution of reaction reduction, it is vacuum dried after filtration, obtains high-quality graphene powder.
Embodiment 3
The 350 mesh micro crystal graphites for weighing 0.5g and the N,N-dimethylformamide solvent for measuring 10mL add autoclave
In, high-temperature is risen to 180 DEG C, control reaction temperature and add stirring 2h.The mixture taken out after cooling in reactor was carried out
Filter, by Graphite Cake in N2Under protection, 550 DEG C of process 2h, to remove the organic solvent or catabolite of residual.Weigh 0.1g
Pretreating graphite, 4gKOH, 0.1gNaNO3It is placed in reactor, adds 30ml deionized waters, stirs 15mins.Sealing reaction
With replacement of oxygen gas reactor 3 times after kettle, then oxygen is rushed to 7MPa, rise high-temperature to 450 DEG C, stir 38h.To take out after cooling
Reactant stirs separation of solid and liquid after 2h under soft mechanical agitation, solid product is first washed with 5% Jing watery hydrochloric acid, then is spent
After ion is washed to neutrality, 100 DEG C are vacuum dried to obtain graphene oxide solid.Weigh 0.1g graphene oxides and be configured to the aqueous solution,
The pH value that graphene oxide water solution is adjusted with HCL is 3, measures in the vial of 3ml graphene aqueous solutions to 5ml, lies low
Formula is put into the uv analyzer of dark box type four, adjusts ultraviolet wavelength and is 254nm and is irradiated also apart from fluorescent lamp 5cm positions
Former 40h.Finally by the graphene aqueous solution of reaction reduction, it is vacuum dried after filtration, obtains high-quality graphene powder.
Embodiment 4
During the 500 mesh micro crystal graphites for weighing 0.5g and the dimethyl sulfoxide solvent for measuring 10mL add autoclave, rise
High-temperature is controlled reaction temperature and adds stirring 5h to 120 DEG C.The mixture taken out after cooling in reactor is filtered, will
Graphite Cake is in N2Under protection, 300 DEG C of process 2h, to remove the organic solvent or catabolite of residual.Weigh the pre- of 0.1g
Process graphite, 4gKOH, 0.1gKNO3It is placed in reactor, adds 30ml deionized waters, stirs 15mins.After sealed reactor
With replacement of oxygen gas reactor 3 times, then oxygen is rushed to 10MPa, rise high-temperature to 500 DEG C, stir 48h.To take out after cooling anti-
Answer thing that separation of solid and liquid after 2h is stirred under soft mechanical agitation, solid product first washed with 5% Jing watery hydrochloric acid, then spend from
After son is washed to neutrality, 100 DEG C are vacuum dried to obtain graphene oxide solid.Weigh 0.1g graphene oxides and be configured to the aqueous solution, use
It is 5 that HCL adjusts the pH value of graphene oxide water solution, is measured in the vial of 3ml graphene aqueous solutions to 5ml, horizontal lying-type
Be put into the uv analyzer of dark box type four, adjust ultraviolet wavelength and be 254nm and be irradiated reduction apart from fluorescent lamp 5cm positions
50h.Finally by the graphene aqueous solution of reaction reduction, it is vacuum dried after filtration, obtains high-quality graphene powder.
Claims (10)
1. a kind of method for preparing Graphene, it is characterised in that：Comprise the steps：
1) graphite raw material pretreatment：After graphite raw material and organic solvent stir process, filter, Graphite Cake is protected in inert gas
The lower high-temperature process of shield；
2) graphite oxidation is processed：By step 1) pretreated graphite with pro-oxidant add aqueous slkali be placed in confined space
It is interior, oxygen is filled with into confined space reacted to certain pressure, reaction carries out separation of solid and liquid after terminating, and solid phase aoxidizes stone
Black alkene；
3) graphene oxide reduction：By step 2) graphene oxide for preparing is configured to graphene oxide water solution, adjusts pH, purple
Outer light irradiation graphene oxide water solution is reduced；
4) post-process：Step 3) after reduction completely, filtration drying obtains graphene powder.
2. the method for preparing Graphene according to claim 1, it is characterised in that：Step 1) described in graphite raw material be
Any one in native graphite, artificial synthesized graphite, micro crystal graphite or highly oriented pyrolytic graphite；The graphite of the graphite raw material
Specification is preferably 50-1000 mesh, more preferably 200-700 mesh, most preferably 300-600 mesh.
3. the method for preparing Graphene according to claim 1, it is characterised in that：Step 1) described in organic solvent be
N-METHYLFORMAMIDE, gamma-butyrolacton, dimethyl sulfoxide (DMSO), dimethyl sulfoxide (DMSO), N,N-dimethylformamide or N, N- diethyl formyl
Any one or a few in amine；Described inert gas is the mixing of one or more in nitrogen, argon gas or hydrogen.
4. the method for preparing Graphene according to claim 1, it is characterised in that：Step 1) in stir process temperature be
100～260 DEG C, preferred 110-220 DEG C, the time of process is 2～5h；Described high-temperature process temperature is 200-700 DEG C, preferably
300-550 DEG C, process time is 1-3h.
5. the method for preparing Graphene according to claim 1, it is characterised in that：Step 2) described in pro-oxidant be nitre
Hydrochlorate, preferred potassium nitrate or sodium nitrate；Described aqueous slkali be hydroxide, preferred potassium hydroxide, NaOH, lithium hydroxide
Or calcium hydroxide.
6. the method for preparing Graphene according to claim 1, it is characterised in that：Step 2) oxygen is filled with into confined space
Displace the gas in container during gas first, then proceed to be filled with oxygen and reacted to certain pressure；Described certain pressure
For 3～20MPa, more preferably preferably 4～15MPa, 5～10MPa；The temperature of reaction be 100～700 DEG C, preferably 400～550 DEG C,
More preferably 450～500 DEG C.
7. the method for preparing Graphene according to claim 1, it is characterised in that：Step 2) reaction terminate after by machinery
Effect carries out separation of solid and liquid after graphene oxide is peeled off uniformly dispersion liquid again.
8. the method for preparing Graphene according to claim 1, it is characterised in that：Step 2) liquid phase after separation of solid and liquid returns
Receipts process；Recovery and treatment method preferably by the concentration of alkali in liquid phase adjust to after before reaction, the concentration of alkali is identical in aqueous slkali,
Use as caustic solution circulation.
9. the method for preparing Graphene according to claim 1, it is characterised in that：Step 3) described in graphene oxide water
The concentration of solution is 0.5～1.5mg/mL, preferred 1mg/mL；It is inorganic acid to adjust pH agents useful for same, preferably phosphoric acid, sulfuric acid or
Hydrochloric acid；Adjust pH<7, preferred pH are 3～5.
10. the method for preparing Graphene according to claim 1, it is characterised in that：Step 3) wavelength of ultraviolet light is
200-300nm, preferred 254nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111892044A (en) * | 2020-08-28 | 2020-11-06 | 中南大学 | Method for large-scale preparation of graphene powder |
| CN112028061A (en) * | 2019-06-04 | 2020-12-04 | 成都中医药大学 | Graphene oxide prepared by illumination method |
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| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
| CN103496696A (en) * | 2013-10-16 | 2014-01-08 | 盐城工学院 | Method for preparing reduction-state graphene |
| CN103738952A (en) * | 2013-12-16 | 2014-04-23 | 湖南大学 | Method for reducing graphene oxide |
| CN105347340A (en) * | 2015-12-14 | 2016-02-24 | 太原理工大学 | Preparation method of graphene oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102659096A (en) * | 2012-04-27 | 2012-09-12 | 湖南大学 | Preparation methods of graphene dispersion solution and thin film of graphene |
| CN103496696A (en) * | 2013-10-16 | 2014-01-08 | 盐城工学院 | Method for preparing reduction-state graphene |
| CN103738952A (en) * | 2013-12-16 | 2014-04-23 | 湖南大学 | Method for reducing graphene oxide |
| CN105347340A (en) * | 2015-12-14 | 2016-02-24 | 太原理工大学 | Preparation method of graphene oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112028061A (en) * | 2019-06-04 | 2020-12-04 | 成都中医药大学 | Graphene oxide prepared by illumination method |
| CN111892044A (en) * | 2020-08-28 | 2020-11-06 | 中南大学 | Method for large-scale preparation of graphene powder |
| CN111892044B (en) * | 2020-08-28 | 2023-01-06 | 中南大学 | Method for large-scale preparation of graphene powder |
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