CN106927457A - A kind of Graphene and preparation method thereof - Google Patents
A kind of Graphene and preparation method thereof Download PDFInfo
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- CN106927457A CN106927457A CN201710300748.7A CN201710300748A CN106927457A CN 106927457 A CN106927457 A CN 106927457A CN 201710300748 A CN201710300748 A CN 201710300748A CN 106927457 A CN106927457 A CN 106927457A
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Abstract
The invention provides a kind of preparation method of Graphene, it is comprised the following steps：A) graphite powder is mixed with the highly crystalline silk-fibroin nanofiber aqueous solution, then is carried out ultrasonically treated；The crystallinity of highly crystalline silk-fibroin nanofiber is more than 40% in the highly crystalline silk-fibroin nanofiber aqueous solution, and a diameter of 10~30nm, length is 100nm~3 μm；B) by step A) mixed liquor that obtains is centrifuged, and obtains graphene solution.Present invention also provides Graphene prepared by above-mentioned preparation method, within 5 layers, planar dimension is 500nm~5 μm to its number of plies.In preparation process, the application is finally obtained the high concentration graphene aqueous solution of stabilization using highly crystalline silk-fibroin nanofiber as dispersant and stabilizer.This kind of preparation method avoids the problem of conformational change in the silk-fibroin ultrasonic procedure that other oroteins stabilizer and other conformations are constituted, and realizes the stabilization preparation of the Graphene with application value.
Description
Technical field
The present invention relates to the preparing technical field of grapheme material, more particularly to one kind is with highly crystalline silk-fibroin nanofiber
The method and Graphene of Graphene are prepared as dispersant and stabilizer.
Background technology
Graphene due to excellent mechanical property, optical property, electrical and thermal conductivity performance and excellent biocompatibility,
The every field such as battery, electronic device, optical device and bio-medical are respectively provided with great potential application foreground.How to use
It is to determine that Graphene really realizes the core and key of application that gentle method realizes prepared by the scale of high-quality graphene.
Current researcher has been developed diversified graphene preparation technology, particularly in terms of prepare with scale,
It is main to have the various ways such as the stripping of graphite oxide alkylene, electrochemical stripping, ultrasound stripping, stabilizer grinding up-stripping.Change
The Graphene peeled off is learned due to the change of functional group, causes its combination property to be remarkably decreased, strongly limit its practical application, and
Although the methods such as grinding stripping have advantage at aspects such as prepare with scale, the prepared graphene film number of plies is too high, and quality is received
To greatly limitation.Ultrasonic wave added is peeled off, and mild condition prepares that the graphene film number of plies is low, and defect is few, and can directly prepare to enter
The solvent dispersion system of one step application, therefore it is constantly subjected to the common concern of people.Although the ultrasonically treated Graphene for preparing is being produced
Rate aspect has certain limitation, but by condition optimizing, answering for related application, particularly bio-medical field is disclosure satisfy that substantially
With with great market prospects.
The method that ultrasound is peeled off is varied, from terms of solvent angle, including two kinds of systems of organic solvent and the aqueous solution, from point
In powder selection, then various species such as including surfactant, macromolecule and polysaccharide, protein, polypeptide.In view of specific
Using the particularly application of biomedical sector makees solvent using water, and simultaneous selection has the natural material of good biocompatibility
Material such as albumen, polysaccharide have more significant advantage as stabilizer and dispersant, therefore are rapidly developed in recent years.However,
The natural polymer structural instability such as polysaccharide, albumen, sensitive to ultrasonically treated reaction, often recurring structure turns in ultrasonic procedure
Become, so as to reduce the quality and yield of Graphene stripping.Research has more preferable stability and has more preferably dispersion to Graphene
Performance, the new material with biocompatibility is still the key issue of field of preparation of graphene.
The special block structure of silk-fibroin makes it have certain hydrophobicity such that it is able to Graphene stable bond, from
It is expected to be applied to prepare grapheme material theoretically.But common silk protein solution is equally unstable, it is easy in ultrasonic mistake
It is transformed into gel in journey, causes to peel off failure.And the highly crystalline silk-fibroin of stabilization is then insoluble in water, it is impossible to make in aqueous
With, therefore stripping prepares Graphene and has no report always in water solution system using silk-fibroin.Therefore, based on above-mentioned progress,
It is necessary to provide that a kind of suitable silk-fibroin nanofiber, as stabilizer and dispersant, stone is peeled off in water solution system ultrasound
Ink, prepares high-quality grapheme material, and by condition optimizing, obtains and prepares high concentration, high yield graphene aqueous solution
Method.
The content of the invention
Present invention solves the technical problem that be that a kind of preparation method of Graphene is provided, the preparation method that the application is provided
A kind of high concentration, high yield can be prepared with high-quality Graphene.
In view of this, this application provides a kind of preparation method of Graphene, comprise the following steps：
A), graphite powder is mixed with the highly crystalline silk-fibroin nanofiber aqueous solution, then is carried out ultrasonically treated；It is described highly crystalline
The crystallinity of highly crystalline silk-fibroin nanofiber is more than 40%, a diameter of 10~30nm in the silk-fibroin nanofiber aqueous solution, long
It is 100nm~3 μm to spend；
B), by step A) mixed liquor that obtains is centrifuged, and obtains graphene solution.
Preferably, the highly crystalline silk-fibroin nanofiber aqueous solution is prepared by the following method：
Silk protein aqueous solution is concentrated into the first silk protein solution that concentration is 8~12wt%；
First silk protein solution is concentrated into the second silk protein solution that concentration is 18~22wt%；
Second silk protein solution is diluted with water to concentration for 0.5~2wt%, sealing is cultivated, and obtains highly crystalline silk
Protein nano fiber solution.
Preferably, it is described obtain in the first silk protein solution be concentrated in 40~60 DEG C and carry out；It is described to obtain second egg
Being concentrated in 25~35 DEG C and carry out in white solution, the temperature that the sealing is cultivated is 50~70 DEG C.
Preferably, the concentration of the highly crystalline silk-fibroin nanofiber aqueous solution is 0.1~3wt%；The highly crystalline silk
Highly crystalline silk-fibroin nanofiber and the mass ratio of the graphite powder in the protein nano fiber aqueous solution are 1：(1~100).
Preferably, step A) in, the ultrasonically treated power is 50~200W, and the ultrasonically treated time is
10min~24h.
Preferably, step B) in, the speed of the centrifugation is 500~5000rpm, time of the centrifugation for 5min~
2h。
Preferably, step B) also include afterwards：
C), the graphene solution is centrifuged again, separate Graphene.
Preferably, step C) in, the speed of the centrifugation is 8000~20000rpm, time of the centrifugation for 5min~
2h。
Present invention also provides the Graphene prepared by the preparation method described in such scheme, the lamella of the Graphene is small
In 5 layers, planar dimension is 500nm~5 μm.
This application provides a kind of preparation method of Graphene, it is first by graphite powder and highly crystalline silk-fibroin nanofiber
The aqueous solution mixes, then carries out ultrasonically treated, makes graphite peel off to form graphene sheet layer；Then by the ultrasonically treated mixed liquor for obtaining
It is centrifuged, to remove unstripped graphite, is obtained graphene solution.The application is high during stripping prepares Graphene
The crystallization silk-fibroin nanofiber aqueous solution both has hydrophobicity, while can disperse in water, therefore it is as dispersant and surely
Determine agent, when ultrasound peels off Graphene, highly crystalline silk-fibroin nanofiber is attached on the Graphene of stripping, is suppressed it and is gathered again
Collection and precipitation, the final high concentration graphene aqueous solution for obtaining stabilization, the yield of Graphene are higher.Graphene prepared by the present invention
Lamella be less than 5 layers, planar dimension be 500nm~5 μm.Test result indicate that, the yield of the present embodiment Graphene 30% with
On, the concentration in water is in more than 20mg/ml.
Brief description of the drawings
Fig. 1 is the photomacrograph of highly crystalline silk-fibroin nanofiber prepared by the embodiment of the present invention 1；
Fig. 2 is the micrograph of highly crystalline silk-fibroin nanofiber prepared by the embodiment of the present invention 1；
Fig. 3 is the infrared spectrogram of highly crystalline silk-fibroin nanofiber prepared by the embodiment of the present invention 1；
Fig. 4 is the photomacrograph of Graphene prepared by the embodiment of the present invention 2；
Fig. 5 is the transmission electron microscope photo of Graphene prepared by the embodiment of the present invention 2；
Fig. 6 is the Raman spectrogram of Graphene prepared by the embodiment of the present invention 2；
Fig. 7 is the photomacrograph of the Graphene that comparative example of the present invention is prepared with embodiment.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but
It should be appreciated that these descriptions are simply to further illustrate the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
In the research of applicant, by regulating and controlling the assembling of silk-fibroin, a kind of highly crystalline silk-fibroin nanometer has been prepared
Fiber, its surface carries more negative electrical charges, so as to can disperse in water, this silk-fibroin nanofiber avoids tradition
The defect of silk-fibroin, is expected to be realized as stabilizer and dispersant the stripping and preparation of Graphene.Thus, this application discloses one
The preparation method of Graphene is planted, is comprised the following steps：
A), graphite powder is mixed with the highly crystalline silk-fibroin nanofiber aqueous solution, then is carried out ultrasonically treated；It is described highly crystalline
The crystallinity of highly crystalline silk-fibroin nanofiber is more than 40%, a diameter of 10~30nm in the silk-fibroin nanofiber aqueous solution, long
It is 100nm~3 μm to spend；
B), by step A) mixed liquor that obtains is centrifuged, and obtains graphene solution.
The application in Graphene preparation process, using highly crystalline silk-fibroin nanofiber as dispersant and stabilizer, most
The graphene aqueous solution of the high concentration of stabilization is obtained eventually, and the quality of Graphene is higher.
According to the present invention, during Graphene is prepared, first by Graphene powder and highly crystalline silk-fibroin nanofiber
The aqueous solution mixes, and obtains original mixture, and the mixing of this process is a simple mixed process, and any change does not occur.
Graphite powder is material well known to those skilled in the art, and this application is had no particular limits.The highly crystalline silk-fibroin is received
The rice fiber aqueous solution is a kind of silk-fibroin of special construction, could have preferable effect during Graphene is peeled off；Tool
Body, the crystallinity of the highly crystalline silk-fibroin nanofiber in the highly crystalline silk-fibroin nanofiber aqueous solution is more than 40%,
A diameter of 10~30nm, length is 100nm~3 μm.The preparation method of the highly crystalline silk-fibroin nanofiber aqueous solution is specific
For：
Silk protein aqueous solution is concentrated into the first silk protein solution that concentration is 8~12wt%；
First silk protein solution is concentrated into the second silk protein solution that concentration is 18~22wt%；
Second silk protein solution is diluted with water to concentration for 0.5~2wt%, sealing is cultivated, and obtains highly crystalline silk
Protein nano fiber solution.
It is above-mentioned prepare the highly crystalline silk-fibroin nanofiber aqueous solution during, silk protein solution is concentrated into first dense
It is 8~12wt% to spend, and obtains the first silk protein solution, and this process is concentrated at 40~60 DEG C；Then by above-mentioned first
Protein solution continues to be concentrated into 18wt%~22wt% to normal temperature, and this process intermediate filment is transformed to metastable nanometer
Grain；The second silk protein solution is finally diluted with water to concentration for 0.5~2wt%, sealing is cultivated, and is obtained highly crystalline silk-fibroin and is received
Rice fiber solution, the temperature that the sealing is cultivated is 50~70 DEG C.
The highly crystalline silk-fibroin nanofiber that the application is used has crystallinity high, specific diameter and length model
Enclose, its crystallinity high and electric charge are arranged, make it that both there is hydrophobicity, while it can disperse in water, this special property
The key of Graphene stripping can be their ability to carry out.If the crystal structure and diameter and length of nanofiber change, right
Peeling effect can make a difference.
In this application, the concentration of the highly crystalline silk-fibroin nanofiber aqueous solution is 0.1~3wt%, specific real
Apply in example, the concentration of the highly crystalline silk-fibroin nanofiber aqueous solution is 0.3~2wt%.The graphite powder and the knot high
The mass ratio of highly crystalline silk-fibroin nanofiber is (1~100) in the brilliant silk-fibroin nanofiber aqueous solution：1.The highly crystalline silk
Protein nano fiber concentration of aqueous solution is too high to cause that solution viscosity is excessive, and energy transmission is obstructed, and Graphene is difficult to peel off；Concentration
Too low, highly crystalline silk-fibroin nanofiber peels off the decline of Graphene stability with the interaction reduction of Graphene.Dry state is high
Crystallization silk-fibroin nanofiber is excessive with the mass ratio of graphite powder, and prepared Graphene amount is too low, lacks actually used value；
Ratio is too low, and the ratio of the high-quality graphene prepared in solution declines, and a large amount of low quality Multi-layer graphites are present, yield drop
It is low, therefore only could obtain high-quality grapheme material in suitable ratio.
Then the application carries out above-mentioned initial mixing liquid ultrasonically treated, makes graphite peel off to form graphene sheet layer.It is described
The ultrasonically treated time is 10min~24h, and power is 50~300W, and in a particular embodiment, the ultrasonically treated time is
1~18h, power is 80~250W.
According to the present invention, then will be ultrasonically treated after mixed liquor centrifugation, to remove unstripped graphite, obtain silk-fibroin
The graphene solution of nanofiber stabilization.The rotating speed of the centrifugation is 500~5000rpm, and the time is 5min~2h, specific real
Apply in example, the rotating speed of the centrifugation is 800~3000rpm, and the time is 20min~1.5h.In this step, have been able to obtain
Graphene, the graphene solution for simply obtaining is at the middle and upper levels highly crystalline silk-fibroin nanofiber, and lower floor is Graphene.
For practical application, graphene solution obtained above is centrifuged the application again, Graphene is tied with high
Brilliant silk-fibroin nanofiber is completely separated, and obtains the grapheme material of lower floor's high-purity.In above process, the centrifugation
Rotating speed be 8000~20000rpm, the time be 5min~2h；In a particular embodiment, the rotating speed of the centrifugation be 10000~
15000rpm, the time is 10~100min.
Present invention also provides the Graphene that the above method is prepared, the lamella of the Graphene is less than 5 layers, plane meter
Very little is 500nm~5 μm.
The invention provides a kind of grapheme material of highly crystalline silk-fibroin nanofiber up-stripping and preparation method thereof,
Below 5, between 500nm~5 μm, concentration can be in more than 20mg/ml, and yield is 30% for size for the number of plies of prepared Graphene
More than, it is significantly better than graphene aqueous solution prepared by the ultrasonically treated stripping reported at present.Preparing the process of Graphene
In, a diameter of 10~200nm of the highly crystalline silk-fibroin nanofiber for utilizing, length is 100nm~3 μm, and crystallinity is 40%
More than, this kind of silk-fibroin nanofibrous structures stabilization, with good hydrophobicity, while can disperse in water, therefore, it is possible to
Conformational stability is kept in ultrasonic procedure, and is combined with Graphene, suppress reassociating for Graphene, finally realize concentration and yield
Be greatly improved.In addition, silk-fibroin and Graphene are combined into physical bond, can also be by high speed centrifugation, by the same stone of silk-fibroin
Black alkene is completely separated, and obtains the grapheme material of high-purity.Meanwhile, this kind of preparation method, process is simple, and the product for obtaining without
Organic solvent, good biocompatibility.
Compared with prior art, the selection that the application passes through specific conformation and the silk-fibroin of nanostructured so that silk-fibroin
Can disperse in water, while avoiding negative effect of the ultrasound to silk-fibroin conformation, it is stabilization finally to realize with silk-fibroin
Agent and dispersant, under the conditions of ultrasonically treated prepare can in water scattered high-quality graphene；By silk-fibroin with addition
Graphite ratio, ultrasonic power and time, and centrifugation rate adjustment, realize Graphene high concentration in aqueous and height
Yield, maximum concentration can reach more than 20mg/ml, and maximum output is higher than 30%, is all remarkably higher than under existing water solution system
Ultrasound peels off prepared Graphene；By the optimization of centrifugation rate, silk-fibroin is further capable of achieving with the separation of Graphene, obtain
High purity graphite alkene, it is to avoid influence of the certain applications intermediate filment to Graphene performance, is the effect high of grapheme material
With offer more more options and advantage；The Graphene number of plies prepared by the final present invention is low, and defect is few, concentration and yield in water
Height, the prospect with prepare with scale and application；Therefore, the preparation method of the Graphene that the application is provided, with water as solvent, work
Skill is simple, the product good biocompatibility for obtaining.
For a further understanding of the present invention, the Graphene provided the present invention with reference to embodiment and preparation method thereof enters
Row is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
(1) common silk protein solution is obtained into the silk protein solution that concentration is 10wt% in 40~60 DEG C of slow concentrations；
(2) silk protein solution that step (1) is obtained is transferred into normal temperature to continue to be concentrated into 20wt%, in the process silk egg
It is transformed into metastable nano particle in vain；
(3) the silk-fibroin nanoparticles solution that step (2) is obtained is diluted with water to 0.5wt%~2wt%, is placed into 60
DEG C sealing cultivate, obtain highly crystalline silk-fibroin nanofiber.
Fig. 1 is the photomacrograph of highly crystalline silk-fibroin nanofiber manufactured in the present embodiment；Fig. 2 is manufactured in the present embodiment
The micrograph of highly crystalline silk-fibroin nanofiber；From Fig. 1 and Fig. 2, highly crystalline silk-fibroin nanometer manufactured in the present embodiment
Fiber can keep solution state, and fibre diameter is 10~20nm, length be 100nm~μm between；Fig. 3 is prepared for the present embodiment
Highly crystalline silk-fibroin nanofiber infrared spectrogram, from the figure 3, it may be seen that highly crystalline silk-fibroin Nanowire manufactured in the present embodiment
The conformation of dimension is mainly beta-sheet crystalline textures.
Embodiment 2
(1) with 10ml concentration it is that the highly crystalline silk-fibroin nanofiber aqueous solution of 1wt% mixes by 100mg graphite powders；
(2) mixture for obtaining step (1) makes graphite peel off to form graphite by the ultrasonically treated 18h of ultrasonic instrument 80W
Alkene lamella；
(3) mixed liquor after treatment is centrifuged 40min at 800 rpm, removes unstripped graphite, obtain upper strata silk egg
The graphene solution of white nanofiber stabilization.The yield of Graphene is 20%, the concentration 2mg/ml of graphene solution.
Fig. 4 is the photomacrograph of Graphene manufactured in the present embodiment, and Fig. 5 is the transmission electricity of Graphene manufactured in the present embodiment
Mirror photo；From Fig. 4 and Fig. 5, below 5 layers, planar dimension is 500nm~5 μm to the Graphene number of plies manufactured in the present embodiment；
Fig. 6 is the Raman spectrogram of Graphene manufactured in the present embodiment, it will be appreciated from fig. 6 that Graphene defect manufactured in the present embodiment is less,
Quality is high.
Embodiment 3
(1) with 10ml concentration it is that the highly crystalline silk-fibroin nanofiber aqueous solution of 1wt% mixes by 100mg graphite powders；
(2) mixture for obtaining step (1) makes graphite peel off to form graphite by the ultrasonically treated 18h of ultrasonic instrument 80W
Alkene lamella；
(3) mixed liquor after treatment is centrifuged 40min at 800 rpm, removes unstripped graphite, obtain upper strata silk egg
The graphene solution of white nanofiber stabilization；
(4) graphene solution is continued in 10000rpm that 10min is centrifuged, Graphene is separated with silk-fibroin nanofiber,
Obtain the grapheme material of lower floor's high-purity.The yield of Graphene is about 16%, and the concentration of graphene solution is about 1.6mg/ml.
Embodiment 4
(1) with 10ml concentration it is that the highly crystalline silk-fibroin nanofiber aqueous solution of 0.5wt% mixes by 1000mg graphite powders；
(2) mixture for obtaining step (1) peels off graphite to form graphite by the ultrasonically treated 1h of ultrasonic instrument 200W
Alkene lamella；
(3) mixed liquor after treatment is centrifuged 20min at 1500 rpm, removes unstripped graphite, obtain upper strata silk egg
The graphene solution of white nanofiber stabilization；
(4) graphene solution is continued in 18000rpm that 20min is centrifuged, Graphene is separated with silk-fibroin nanofiber,
Obtain the grapheme material of lower floor's high-purity.The yield of Graphene is about 20%, the concentration 20mg/ml of graphene solution.
Embodiment 5
(1) with 20ml concentration it is that the highly crystalline silk-fibroin nanofiber aqueous solution of 2wt% mixes by 400mg graphite powders；
(2) mixture for obtaining step (1) makes graphite peel off to form graphite by the ultrasonically treated 4h of ultrasonic instrument 150W
Alkene lamella；
(3) mixed liquor after treatment is centrifuged 1.5h under 1200rpm, removes unstripped graphite, obtain upper strata silk egg
The graphene solution of white nanofiber stabilization；
(4) graphene solution is continued in 10000rpm that 100min is centrifuged, Graphene is separated with silk-fibroin nanofiber,
Obtain the grapheme material of lower floor's high-purity.The yield of Graphene is about 22%, the concentration 4.4mg/ml of graphene solution.
Embodiment 6
(1) with 30ml concentration it is that the highly crystalline silk-fibroin nanofiber aqueous solution of 0.3wt% mixes by 200mg graphite powders；
(2) mixture for obtaining step (1) makes graphite peel off to form graphite by the ultrasonically treated 8h of ultrasonic instrument 250W
Alkene lamella；
(3) mixed liquor after treatment is centrifuged 20min at 800 rpm, removes unstripped graphite, obtain upper strata silk egg
The graphene solution of white nanofiber stabilization；
(4) graphene solution is continued in 12000rpm that 10min is centrifuged, Graphene is separated with silk-fibroin nanofiber,
Obtain the grapheme material of lower floor's high-purity.The yield 28% of Graphene, the concentration 1.87mg/ml of graphene solution.
Comparative example 1
(1) with 10ml concentration it is that 1wt% tradition amorphous silk protein aqueous solutions mix by 100mg graphite powders；
(2) mixture for obtaining step (1) makes graphite peel off to form graphite by the ultrasonically treated 18h of ultrasonic instrument 80W
Alkene lamella, but ultrasonic procedure intermediate filment result changes, and solution forms gel Graphene and cannot collect separation, causes graphite
Alkene solution prepares failure, as shown in fig. 7, Fig. 7 is macroscopical picture of Graphene prepared by comparative example 1 and embodiment 3, in Fig. 7 A and
Picture on the left of B is macroscopical picture of the Graphene of the preparation of comparative example 1, and the picture on right side is the graphite of the preparation of embodiment 3
Macroscopical picture of alkene, as seen from the figure, Graphene prepared by this comparative example is gel state, it is difficult to separate Graphene.
The explanation of above example is only intended to help and understands the method for the present invention and its core concept.It should be pointed out that right
For those skilled in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or uses the present invention.
Various modifications to these embodiments will be apparent for those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention
The embodiments shown herein is not intended to be limited to, and is to fit to and principles disclosed herein and features of novelty phase one
The scope most wide for causing.
Claims (9)
1. a kind of preparation method of Graphene, comprises the following steps：
A), graphite powder is mixed with the highly crystalline silk-fibroin nanofiber aqueous solution, then is carried out ultrasonically treated；The highly crystalline silk egg
The crystallinity of highly crystalline silk-fibroin nanofiber is more than 40% in the white nanofiber aqueous solution, a diameter of 10~30nm, and length is
100nm~3 μm；
B), by step A) mixed liquor that obtains is centrifuged, and obtains graphene solution.
2. preparation method according to claim 1, it is characterised in that the highly crystalline silk-fibroin nanofiber aqueous solution is pressed
Prepared according to following methods：
Silk protein aqueous solution is concentrated into the first silk protein solution that concentration is 8~12wt%；
First silk protein solution is concentrated into the second silk protein solution that concentration is 18~22wt%；
Second silk protein solution is diluted with water to concentration for 0.5~2wt%, sealing is cultivated, and obtains highly crystalline silk-fibroin
Nanofiber solution.
3. preparation method according to claim 2, it is characterised in that it is described obtain in the first silk protein solution be concentrated in
40~60 DEG C are carried out；It is described obtain in the second silk protein solution be concentrated in 25~35 DEG C and carry out, the temperature that the sealing is cultivated
It is 50~70 DEG C.
4. preparation method according to claim 1, it is characterised in that the highly crystalline silk-fibroin nanofiber aqueous solution
Concentration is 0.1~3wt%；Highly crystalline silk-fibroin nanofiber in the highly crystalline silk-fibroin nanofiber aqueous solution with it is described
The mass ratio of graphite powder is 1：(1~100).
5. preparation method according to claim 1, it is characterised in that step A) in, the ultrasonically treated power is 50
~200W, the ultrasonically treated time is 10min~24h.
6. preparation method according to claim 1, it is characterised in that step B) in, the speed of the centrifugation for 500~
5000rpm, the time of the centrifugation is 5min~2h.
7. the preparation method according to any one of claim 1~6, it is characterised in that step B) after also include：
C), the graphene solution is centrifuged again, separate Graphene.
8. preparation method according to claim 7, it is characterised in that step C) in, the speed of the centrifugation for 8000~
20000rpm, the time of the centrifugation is 5min~2h.
9. the Graphene prepared by the preparation method described in claim 1, it is characterised in that the lamella of the Graphene is less than 5
Layer, planar dimension is 500nm~5 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108298531A (en) * | 2018-03-28 | 2018-07-20 | 苏州大学 | A kind of preparation method of graphene |
| CN109569347A (en) * | 2018-12-14 | 2019-04-05 | 苏州大学 | A kind of method of hydrophobic material water phase transfer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103407998A (en) * | 2013-07-19 | 2013-11-27 | 华侨大学 | Preparation method of high concentration and small flake diameter graphene dispersion |
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| US11261092B2 (en) | 2018-03-28 | 2022-03-01 | Soochow University | Method of producing graphene |
| CN109569347A (en) * | 2018-12-14 | 2019-04-05 | 苏州大学 | A kind of method of hydrophobic material water phase transfer |
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| CN106927457B (en) | 2019-04-12 |
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