CN106587028A - Method of preparing graphene by oxidation and reduction process - Google Patents
Method of preparing graphene by oxidation and reduction process Download PDFInfo
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- CN106587028A CN106587028A CN201710071320.XA CN201710071320A CN106587028A CN 106587028 A CN106587028 A CN 106587028A CN 201710071320 A CN201710071320 A CN 201710071320A CN 106587028 A CN106587028 A CN 106587028A
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- C01B2204/00—Structure or properties of graphene
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention belongs to the field of graphene preparation, and particularly relates to a method of preparing graphene by an oxidation and reduction process. The method comprises the following effective steps: firstly, mixing sodium selenate with nickelate to obtain an acidic mixture; then putting graphite powder and potassium permanganate in a reaction kettle and uniformly stirring and mixing the mixture; then adding the acidic mixture into the reaction kettle, mixing and stirring the mixture with graphene and potassium permanganate to obtain a reaction product; uniformly mixing ice and hydrogen peroxide to obtain an ice water mixture; then fully stirring the reaction product and the ice water mixture till gas is not generated, then performing centrifugal separation to take out a lower precipitate, and washing the precipitate with hydrochloric acid thoroughly to obtain a pre-product; then performing dialysis on the pre-product two days, then freezing and drying the product to obtain graphene oxide powder; and preparing a graphene oxide solution by the graphene oxide powder, adding an excessive amount of ascorbic acid, performing a reaction 30 minutes at 80 DEG C, and performing centrifugal separation on the product, and washing and drying the product to obtain the graphene oxide powder.
Description
Technical field
The invention belongs to field of preparation of graphene, more particularly to a kind of method that oxidation-reduction method prepares Graphene.
Background technology
Graphene (Graphene) is the two-dimensional atomic crystal that carbon atom is constituted with the monoatomic layer that SP2 hydridization connects, its
Basic structural unit is most stable of benzene hexatomic ring in organic material.Single-layer graphene thickness is only 0.35nm, is in the world most
Thin two-dimensional material, this special construction makes Graphene show many excellent properties.
From 2004, Novoselvo research groups were obtained for the first time with mechanical stripping method (Mechanical cleavage)
Since single-layer graphene lamella, Graphene and its composite with its peculiar performance, in electronic device, gas sensor, energy
The broad prospect of application in the field such as amount storage and composite, causes the extensive concern and great research interest of scientist.
The preparation of material is premise and the basis studied its performance and explore its application.The time of a few years, researcher
Just achieved in terms of the preparation of Graphene actively progress, it was found that mechanical stripping, crystal epitaxy, oxidoreduction,
Various preparation methoies such as chemical vapor deposition.By different preparation methoies, the yield and quality of Graphene has largely
Raising, be greatly facilitated the research to the intrinsic physical property of Graphene and application.
In order to update the preparation method of Graphene, there has been proposed various methods, for example, State Intellectual is produced
A kind of preparation method { 201410269250.5 } of Graphene that power office provides, its methods described step is as follows：Preparation has
Machine acid procyanidin solution, by graphene oxide by certain mass fraction ultrasonic disperse in procyanidin solution, ultrasound
After 40～60min, homogeneous graphene oxide mixed solution, in the mixed solution, the concentration of graphene oxide are filtrated to get
For 0.5～2mg/ml, the concentration of procyanidin is 0.1～1mg/ml, and solution ph exists above-mentioned mixed solution between 4～5
1～2h is reacted at 70～100 DEG C, the cleaning of product deionized water is dried to obtain Graphene.
Or be a kind of Graphene of State Intellectual Property Office's offer or the preparation method of graphene oxide
{ 201210202629.5 }, preparation method includes that wet method is prepared and dry process, and prepared by wet method is by carbon materials, magnetic draw point
Abrasive body and solvent, it is closed in being put into grinding container；Container is inserted in the space with conversion magnetic field, is peeled off, peeled off
The mixture of graphite nano micro-flake-Graphene is obtained afterwards；Graphite nanosheets-Graphene and draw point are separated, through sedimentation, centrifugation
After separation, the transperent suspension liquid of Graphene is obtained.Dry process is, by carbon materials and magnetic draw point abrasive body, to be put into grinding and hold
It is closed in device；Container is inserted in the space with conversion magnetic field, is peeled off, graphite nano micro-flake-graphite is obtained after stripping
The mixture dry powder of alkene.
Above-mentioned technical proposal all has significant improvement by different preparation methoies, the yield and quality of Graphene,
It has been greatly facilitated the research to the intrinsic physical property of Graphene and application.But how different applications is directed to, realizes the grand of Graphene
Prepared by amount control, its quality, structure are regulated and controled, and is still the significant challenge of current Graphene research field.、
The content of the invention
The present invention is directed to above-mentioned technical problem, proposes the stone that a kind of reasonable in design, method is simple, with low cost and produces
The method that black alkene quality better, quality height and the high oxidation-reduction method of yield prepare Graphene.
In order to achieve the above object, the technical solution used in the present invention is that the present invention provides a kind of oxidation-reduction method and prepares
The method of Graphene, it is characterised in that including following effective procedure：
A, it is first according to mass ratio 10:1～8:1 ratio mixing sodium selenate and nickelate mixing, mix homogeneously obtains acid
Property mixture；
B then by graphite powder and potassium permanganate according to mass ratio 1:3～1:8 ratio is put in reactor, and stirring is mixed
Close uniform；
C and then the acidic mixture that a steps are obtained is added in reactor, according to mass ratio 20:1 ratio and stone
Black alkene and potassium permanganate are mixed, while noticing that control system temperature is less than 40 degree, after being sufficiently mixed, are warming up to 50-
65 degree, be incubated 12 hours, after naturally cool to room temperature, period keeps mechanical agitation uninterrupted, obtains product；
D, step c stir during, by ice and hydrogen peroxide according to mass ratio 140:1～100:1 ratio mix homogeneously, obtains
To mixture of ice and water；
E then by product and mixture of ice and water according to volume ratio 1:1 ratio, is stirred well to and no longer produce gas
Body, then, centrifugation takes lower sediment thing, and clean with hydrochloric acid and water washing, obtains pre-product；
F and then by pre-product dialysis treatment 2 days, lyophilization afterwards, you can obtain graphene oxide powder；
G, the graphene oxide powder for obtaining is configured to graphene oxide solution, adds excess of ascorbate, 80 degree instead
Answer 30 minutes.Centrifugation product, washing and drying obtains graphene powder.
Preferably, in a steps, the mass ratio of the sodium selenate and nickelate is 8:1.
Preferably, in the b step, the mass ratio of the graphite powder and potassium permanganate is 1:6.
Preferably, in the step e, the mass ratio of hydrochloric acid and water is 1:10.
Preferably, in the f steps, the specification of pre-product dialysis treatment is 100KD.
Preferably, in the g steps, the concentration of the graphene oxide is less than 0.5mg/L.
Preferably, in the g steps, the concentration of the graphene oxide is higher than 2mg/L.
Compared with prior art, advantages of the present invention and good effect be,
1st, the present invention provides a kind of method that oxidation-reduction method prepares Graphene, by improving conventional oxidation reducing process,
By the use of sodium selenate and nickelate as inorganic proton acid by tight graphite layer open, by the use of potassium permanganate as strong oxidizer pair
Graphite powder carries out oxidation processes, and then obtains graphene oxide, then, then by carrying out to the graphene oxide under variable concentrations
Process, and then obtain Graphene powder, method provided by the present invention is simple, Graphene yield with low cost and obtaining is high, matter
Measure, suitable large-scale promotion is used.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are some embodiments of the present invention, for ability
For the those of ordinary skill of domain, without having to pay creative labor, can be with other according to these accompanying drawings acquisitions
Accompanying drawing.
Fig. 1 is the SEM figures of Graphene prepared by embodiment 1；
Fig. 2 is the XRD curve charts of Graphene prepared by embodiment 1；
Fig. 3 is the infared spectrum of Graphene prepared by embodiment 1；
Fig. 4 is the Raman curve of Graphene prepared by embodiment 1.
Specific embodiment
In order to be more clearly understood that the above objects, features and advantages of the present invention, with reference to the accompanying drawings and examples
The present invention will be further described.It should be noted that in the case where not conflicting, in embodiments herein and embodiment
Feature can be mutually combined.
Many details are elaborated in the following description in order to fully understand the present invention, but, the present invention may be used also
To be implemented using other modes described here are different from, therefore, the present invention is not limited to the concrete of description described below
The restriction of embodiment.
Embodiment 1, the present embodiment provides a kind of method that oxidation-reduction method prepares Graphene, and concrete grammar is as follows, first
Mix according to mass ratio 360ml sodium selenate and 40ml nickelates (lithium nickelate), mix homogeneously obtains acidic mixture, in this reality
In applying example, substituting traditional sulphuric acid using sodium selenate and nickelate can quickly open close graphite as inorganic proton acid
Layer, while, it is also possible to carry out more close cooperation with following raw material, so as to get Graphene yield and quality more preferably；
Then the potassium permanganate of the graphite powder of 3g and 18g is put in reactor according to the ratio of mass ratio, stirring is mixed
Close uniform, it is to be mixed it is uniform after, then the acidic mixture for obtaining is added in reactor, it is mixed with Graphene and potassium permanganate
Stirring is closed, while noticing that control system temperature is less than 40 degree, after being sufficiently mixed, 50-65 degree is warming up to, 12 hours are incubated,
After naturally cool to room temperature, period keeps mechanical agitation uninterrupted, product is obtained, now, by sodium selenate and nickelate group
Into inorganic proton acid will open close graphite linings, strong acid molecule is inserted between graphite linings, then, potassium permanganate make
Oxidation processes are carried out to graphite for strong oxidizer, product is obtained, in step, disposably processes different from traditional
It is, the strategy that this method is walked using two steps to be stirred mixing below 40 degree first, then carries out between 50-65 degree anti-
Should, less than 40 degree of stirring can be considered as pre-oxidation, and reaction is carried out between 50-65 degree can be considered as formal oxidation reaction,
Pre-oxidation gives the graphite enough intercalation time and improves intercalation probability, has loosened closely coupled graphite linings, carries
High interlayer distance, increases the probability that group penetrates into from graphite edge toward internal layer, is follow-up so as to improve intercalation probability
Peroxidating process provides enough oxidation spaces.
Ensuing process is to process product, and the ice of 400ml and the hydrogen peroxide mix homogeneously of 3ml are obtained
Mixture of ice and water, then by product and mixture of ice and water according to volume ratio 1:1 ratio, is stirred well to and no longer produce gas
Body, then, centrifugation takes lower sediment thing, and clean with hydrochloric acid and water washing, obtains pre-product, needs what is illustrated here
It is that the mass ratio of hydrochloric acid and water is 1:10, the main purpose washing of hydrochloric acid and water is added, wash away residual acid and metal ion.
Cleaning in view of metal ion totally may not need for pre-product to do dialysis treatment, dialysis treatment it is main
If purpose removes deionization, by ion-transfer out, after the water in bag filter is in neutrality, lyophilization afterwards, you can
Graphene oxide powder is obtained, in the present embodiment, the specification of dialysis treatment is 100KD.
Then, the graphene oxide powder for obtaining is configured to into graphene oxide solution, adds excess of ascorbate, 80 degree
Reaction 30 minutes.Centrifugation product, washed several times with water is dried, that is, obtain graphene powder, ascorbic acid (vitamin C) molecule knot
There is dienol structure, with extremely strong reproducibility, in vivo vitamin may participate in redox reaction and hydroxyl in structure
Change reaction, have particularly significant effect the normal biochemical metabolism of organism and physiological function is maintained.Using ascorbic acid for also
Former agent, nontoxic reaction condition is gentle and oxidation product environmental friendliness.At this it should be noted that when graphene oxide concentration is less than
0.5mg/L can be only formed the graphene powder of black, and the initial concentration for forming Graphene gel is 2mg/L.The Graphene of synthesis
Hydrogel has stronger electric conductivity (1s/m) and good mechanical strength, shows excellent chemical property.
Graphene quality is very soft, and a large amount of folds can be formed in substrate, and these folds can clearly be divided in the secure execution mode (sem
Distinguish, can just see its profile substantially, result of study shows that the surface of Graphene is not inherently substantially flat, in order to maintain
Its heat stability, can reduce the free energy of system, so as to surface occurs the lumpy fold of certain altitude, fold degree
Can be less and less with the increase of the Graphene number of plies, as shown in figure 1, the surface topography degree of folding of Graphene is larger, explanation is obtained
The Graphene number of plies it is few, the Graphene quality for also just obtaining is more next.
Then X-ray diffraction analysis are carried out, obvious graphite is occurred in that at 25.5 ° or so as can see from Figure 2
Change diffraction maximum, this explanation sample has graphited structure.This diffraction maximum is the diffraction maximum of crystal face (002).(002) of graphite
The diffraction maximum of crystal face illustrates the thorough of reduction at 26 ° or so.At the same time, it can be observed that this diffraction maximum is wider, intensity compared with
Weak, this obtained Graphene of explanation reduction has very thin laminate structure.This is consistent with the observation result of SEM.
Followed by infrared spectrum analysiss, as seen from Figure 3, the hydroxyl absorption peak in 3420cm-1 vicinity does not almost have
Have, illustrate that hydroxyl is all reduced substantially.Also there is an absworption peak in 1627cm-1 vicinity, this absworption peak is corresponding to be
The vibration of C=C skeletons.There is a very weak absworption peak to correspond to C-O in epoxy radicals in 1110cm-1 and 1234cm-1 vicinity
Stretching vibration peak, this explanation reduction after Graphene oxygen-containing functional group content it is few, reduction it is thorough.This result with XRD analysis
It is consistent.
Raman spectrum analyses are finally carried out, the instrument that experiment test is used is confocal Raman microscopy, from Fig. 4
It will be clear that two of surveyed graphene product obviously characteristic peaks, i.e. D peaks and G peaks.What G peaks were characterized is carbon
The architectural characteristic of sp2, this represents the symmetry and crystallization degree of this material with carbon element；D peaks are defect peaks, and it represents each layer of graphite
The randomness of piece.The quality quality of obtained Graphene, this intensity rate are differentiated by the intensity rate at D peaks and G peaks
It is commonly used to represent the carbon number purpose ratio of the carbon atom number with sp3 of sp2, is the important finger of the order for weighing material
Mark, defect, the randomness of the bright Graphene of this ratio more novel etc. are better, crystallize more perfect.Graphene as seen in Figure 4
Reduction better off, it is thorough that oxygen-containing functional group is removed, and Graphene obtained in embodiment 1 does very well in terms of defect, randomness.
This is consistent with the analysis result of XRD and the analysis result of infrared absorption spectroscopy.
Embodiment 2, the present embodiment provides a kind of method that oxidation-reduction method prepares Graphene, and concrete grammar is as follows, first
Mix according to mass ratio 500ml sodium selenate and 50ml nickelates (lithium nickelate), mix homogeneously obtains acidic mixture, in this reality
In applying example, substituting traditional sulphuric acid using sodium selenate and nickelate can quickly open close graphite as inorganic proton acid
Layer, while, it is also possible to carry out more close cooperation with following raw material, so as to get Graphene yield and quality more preferably；
Then the potassium permanganate of 5 graphite powder and 15g is put in reactor according to the ratio of mass ratio, stirring mixing
Uniformly, it is to be mixed it is uniform after, then the acidic mixture for obtaining is added in reactor, mix with Graphene and potassium permanganate
Stirring, while noticing that control system temperature is less than 40 degree, after being sufficiently mixed, is warming up to 50-65 degree, is incubated 12 hours, after
Room temperature is naturally cooled to, period keeps mechanical agitation uninterrupted, obtains product, now, is made up of sodium selenate and nickelate
Inorganic proton acid will open close graphite linings, strong acid molecule is inserted between graphite linings, then, potassium permanganate conduct
Strong oxidizer carries out oxidation processes to graphite, obtains product, in step, and unlike traditional disposable process,
The strategy that this method is walked using two steps, is stirred first mixing below 40 degree, is then reacted between 50-65 degree,
Less than 40 degree of stirring can be considered as pre-oxidation, and reaction is carried out between 50-65 degree can be considered as formal oxidation reaction, pre- oxygen
Change gives the graphite enough intercalation time and improves intercalation probability, has loosened closely coupled graphite linings, improves
Interlayer distance, increases the probability that group penetrates into from graphite edge toward internal layer, is follow-up peroxide so as to improve intercalation probability
Change process provides enough oxidation spaces.
Ensuing process is to process product, and the ice of 420ml and the hydrogen peroxide mix homogeneously of 1ml are obtained
Mixture of ice and water, then by product and mixture of ice and water according to volume ratio 1:1 ratio, is stirred well to and no longer produce gas
Body, then, centrifugation takes lower sediment thing, and clean with hydrochloric acid and water washing, obtains pre-product, needs what is illustrated here
It is that the mass ratio of hydrochloric acid and water is 1:10, the main purpose washing of hydrochloric acid and water is added, wash away residual acid and metal ion.
Cleaning in view of metal ion totally may not need for pre-product to do dialysis treatment, dialysis treatment it is main
If purpose removes deionization, by ion-transfer out, after the water in bag filter is in neutrality, lyophilization afterwards, you can
Graphene oxide powder is obtained, in the present embodiment, the specification of dialysis treatment is 100KD.
Then, the graphene oxide powder for obtaining is configured to into graphene oxide solution, adds excess of ascorbate, 80 degree
Reaction 30 minutes.Centrifugation product, washed several times with water is dried, that is, obtain graphene powder, ascorbic acid (vitamin C) molecule knot
There is dienol structure, with extremely strong reproducibility, in vivo vitamin may participate in redox reaction and hydroxyl in structure
Change reaction, have particularly significant effect the normal biochemical metabolism of organism and physiological function is maintained.Using ascorbic acid for also
Former agent, nontoxic reaction condition is gentle and oxidation product environmental friendliness.At this it should be noted that when graphene oxide concentration is less than
0.5mg/L can be only formed the graphene powder of black, and the initial concentration for forming Graphene gel is 2mg/L.The Graphene of synthesis
Hydrogel has stronger electric conductivity (1s/m) and good mechanical strength, shows excellent chemical property.
Embodiment 3, the present embodiment provides a kind of method that oxidation-reduction method prepares Graphene, and concrete grammar is as follows, first
Mix according to mass ratio 200ml sodium selenate and 25ml nickelates (lithium nickelate), mix homogeneously obtains acidic mixture, in this reality
In applying example, substituting traditional sulphuric acid using sodium selenate and nickelate can quickly open close graphite as inorganic proton acid
Layer, while, it is also possible to carry out more close cooperation with following raw material, so as to get Graphene yield and quality more preferably；
Then the potassium permanganate of 2 graphite powder and 16g is put in reactor according to the ratio of mass ratio, stirring mixing
Uniformly, it is to be mixed it is uniform after, then the acidic mixture for obtaining is added in reactor, mix with Graphene and potassium permanganate
Stirring, while noticing that control system temperature is less than 40 degree, after being sufficiently mixed, is warming up to 50-65 degree, is incubated 12 hours, after
Room temperature is naturally cooled to, period keeps mechanical agitation uninterrupted, obtains product, now, is made up of sodium selenate and nickelate
Inorganic proton acid will open close graphite linings, strong acid molecule is inserted between graphite linings, then, potassium permanganate conduct
Strong oxidizer carries out oxidation processes to graphite, obtains product, in step, and unlike traditional disposable process,
The strategy that this method is walked using two steps, is stirred first mixing below 40 degree, is then reacted between 50-65 degree,
Less than 40 degree of stirring can be considered as pre-oxidation, and reaction is carried out between 50-65 degree can be considered as formal oxidation reaction, pre- oxygen
Change gives the graphite enough intercalation time and improves intercalation probability, has loosened closely coupled graphite linings, improves
Interlayer distance, increases the probability that group penetrates into from graphite edge toward internal layer, is follow-up peroxide so as to improve intercalation probability
Change process provides enough oxidation spaces.
Ensuing process is to process product, and the ice of 300ml and the hydrogen peroxide mix homogeneously of 1ml are obtained
Mixture of ice and water, then by product and mixture of ice and water according to volume ratio 1:1 ratio, is stirred well to and no longer produce gas
Body, then, centrifugation takes lower sediment thing, and clean with hydrochloric acid and water washing, obtains pre-product, needs what is illustrated here
It is that the mass ratio of hydrochloric acid and water is 1:10, the main purpose washing of hydrochloric acid and water is added, wash away residual acid and metal ion.
Cleaning in view of metal ion totally may not need for pre-product to do dialysis treatment, dialysis treatment it is main
If purpose removes deionization, by ion-transfer out, after the water in bag filter is in neutrality, lyophilization afterwards, you can
Graphene oxide powder is obtained, in the present embodiment, the specification of dialysis treatment is 100KD.
Then, the graphene oxide powder for obtaining is configured to into graphene oxide solution, adds excess of ascorbate, 80 degree
Reaction 30 minutes.Centrifugation product, washed several times with water is dried, that is, obtain graphene powder, ascorbic acid (vitamin C) molecule knot
There is dienol structure, with extremely strong reproducibility, in vivo vitamin may participate in redox reaction and hydroxyl in structure
Change reaction, have particularly significant effect the normal biochemical metabolism of organism and physiological function is maintained.Using ascorbic acid for also
Former agent, nontoxic reaction condition is gentle and oxidation product environmental friendliness.At this it should be noted that when graphene oxide concentration is less than
0.5mg/L can be only formed the graphene powder of black, and the initial concentration for forming Graphene gel is 2mg/L.The Graphene of synthesis
Hydrogel has stronger electric conductivity (1s/m) and good mechanical strength, shows excellent chemical property.
The above, is only presently preferred embodiments of the present invention, is not the restriction for making other forms to the present invention, is appointed
What those skilled in the art changed possibly also with the technology contents of the disclosure above or be modified as equivalent variations etc.
Effect embodiment is applied to other fields, but every without departing from technical solution of the present invention content, according to the technical spirit of the present invention
Any simple modification, equivalent variations and the remodeling made to above example, still falls within the protection domain of technical solution of the present invention.
Claims (7)
1. a kind of method that oxidation-reduction method prepares Graphene, it is characterised in that including following effective procedure：
A, it is first according to mass ratio 10:1～8:1 ratio mixing sodium selenate and nickelate mixing, mix homogeneously, obtain acid mixed
Compound；
B then by graphite powder and potassium permanganate according to mass ratio 1:3～1:8 ratio is put in reactor, and stirring mixing is equal
It is even；
C and then the acidic mixture that a steps are obtained is added in reactor, according to mass ratio 20:1 ratio and Graphene
Mix with potassium permanganate, while noticing that control system temperature is less than 40 degree, after being sufficiently mixed, be warming up to 50-65 degree,
Insulation 12 hours, after naturally cool to room temperature, period keeps mechanical agitation uninterrupted, obtains product；
D, step c stir during, by ice and hydrogen peroxide according to mass ratio 140:1～100:1 ratio mix homogeneously, obtains ice
Aqueous mixtures；
E then by product and mixture of ice and water according to volume ratio 1:1 ratio, is stirred well to and no longer produce gas, so
Afterwards, centrifugation takes lower sediment thing, and clean with hydrochloric acid and water washing, obtains pre-product；
F and then by pre-product dialysis treatment 2 days, lyophilization afterwards, you can obtain graphene oxide powder；
G, the graphene oxide powder for obtaining is configured to graphene oxide solution, adds excess of ascorbate, 80 degree are reacted 30
Minute.Centrifugation product, washing and drying obtains graphene powder.
2. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in a steps, institute
The mass ratio for stating sodium selenate and nickelate is 8:1.
3. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in the b step, institute
The mass ratio for stating graphite powder and potassium permanganate is 1:6.
4. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in the step e, salt
The mass ratio of acid and water is 1:10.
5. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in the f steps, in advance
The specification of product dialysis treatment is 100KD.
6. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in the g steps, institute
The concentration for stating graphene oxide is less than 0.5mg/L.
7. the method that oxidation-reduction method according to claim 1 prepares Graphene, it is characterised in that in the g steps, institute
The concentration for stating graphene oxide is higher than 2mg/L.
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| CN109037616A (en) * | 2018-07-10 | 2018-12-18 | 桂林理工大学 | Change the method for preparing high performance LiFePO4/three-dimensional graphene composite material by the morphology and size of ferric phosphate |
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| CN105752977A (en) * | 2016-04-29 | 2016-07-13 | 江苏超电新能源科技发展有限公司 | Preparation method of high-conductivity graphene powder |
| CN106044750A (en) * | 2016-05-25 | 2016-10-26 | 南京凤源新材料科技有限公司 | Method for preparing graphene oxide with controllable defects |
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| CN109037616A (en) * | 2018-07-10 | 2018-12-18 | 桂林理工大学 | Change the method for preparing high performance LiFePO4/three-dimensional graphene composite material by the morphology and size of ferric phosphate |
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