CN107253716A - A kind of preparation method of graphene paper - Google Patents
A kind of preparation method of graphene paper Download PDFInfo
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- CN107253716A CN107253716A CN201710445862.9A CN201710445862A CN107253716A CN 107253716 A CN107253716 A CN 107253716A CN 201710445862 A CN201710445862 A CN 201710445862A CN 107253716 A CN107253716 A CN 107253716A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention discloses a kind of preparation method of graphene paper, comprise the following steps：(1) electro spinning nanometer fiber membrane substrate；(2) EFI combined oxidation graphene film；(3) substrate is removed；(4) redox graphene.Compared to existing method, the preparation method operates simpler, cost low, the graphene paper thickness of gained is uniform, with preferable chemical property, and be easy to separate with backing material, the graphene paper of large area can be prepared, the patterning of graphene paper can be directly realized by preparation process simultaneously, the application field of material is expanded.
Description
Technical field
The invention belongs to grapheme material preparing technical field, and in particular to a kind of preparation method of graphene paper.
Background technology
Graphene is a kind of individual layer Two-dimensional Carbon atomic crystal found in 2004, its unique two-dimensional layered structure and excellent
The performances such as different electricity, calorifics, mechanics, make it be shown in various fields such as flexible electronic, photodetection, energy stores non-
Chang Youyi application prospect.The preparation method of graphene is limited to, the measured single-layer graphene sample of large scale matter is prepared at present
Difficulty is also there is, micro-meter scale is limited in mostly, in order to realize application, the grapheme material with macro-scale how is assembled
One of focus of recent researcher research is become.Graphene paper is macroscopical as a kind of graphene of typical two-dimensional structure
Assembled material, because it is easy to blend with the material manufacturing process of modern popular, is particularly received extensively in energy storage field
Concern.Preparing the method for graphene paper at present mainly has the side such as vacuum filtration, liquid phase electrophoretic deposition and the self assembly of gas-liquid face
Method, but some limitations are all there are in different aspect, such as most widely used vacuum filtration method in preparation process there is also
The shortcomings of high and material that consumes energy separates difficulty with filter membrane.In addition, with the wearable device based on flexible electronic
Progressively develop, it is to increase the conventional strategy of material tensile property to construct special construction or patterning, but is preparing pattern at present
Preferable achievement in research is there is no in terms of the graphene paper of change.
The content of the invention
The technical problem to be solved in the present invention is：Overcoming prior art defect, there is provided a kind of grapheme material technology of preparing
Field, compared to existing method, the preparation method operates simpler, cost low, and the graphene paper thickness of gained is uniform, have
Preferable chemical property, and be easy to separate with backing material, the graphene paper of large area can be prepared, while can prepare
During be directly realized by the patterning of graphene paper, expand the application field of material.
In order to solve the above problems, the invention provides a kind of preparation method of graphene paper, comprise the following steps：
(1) electro spinning nanometer fiber membrane substrate：High molecular polymer spinning precursor liquid is prepared, gained spinning precursor liquid is added
In the liquid storage mechanism of electrostatic spinning apparatus, high molecular polymer nano fibrous membrane is prepared using method of electrostatic spinning, that is, is collecting bottom
Nano fibrous membrane substrate is obtained on plate；
(2) EFI combined oxidation graphene film：Graphene oxide dispersion is placed in the liquid storage machine of electrostatic atomizer
In structure, step (1) nano fibrous membrane substrate is placed on the collecting mechanism of electrostatic atomizer, using electrostatic spraying processes in nanometer
Direct spraying combined oxidation graphene film on tunica fibrosa substrate；
(3) substrate is removed：The nano fibrous membrane substrate of composite film material obtained by step (2) is removed, graphite oxide is obtained
Alkene film；
(4) redox graphene：Graphene oxide film reduction obtained by step (3) is produced into graphene paper.
Preparation method of the invention is simple to operate, cost is low, and the high molecular nanometer that this method is prepared with method of electrostatic spinning is fine
Dimension film is substrate, and utilizes electric field force in the compound one layer of dense uniform of substrate fiber surface direct spraying using electrostatic spraying processes
Graphene oxide film, because the nano-fiber film as substrate can be removed easily by methods such as dissolving, burnings, most
Graphene paper in uniform thickness is can be prepared by oxidation graphene film afterwards, the removal substrate approach is not only simple, and should
During graphene oxide film performance and pattern without influence so that this method can easily realize graphene paper and substrate
Separation, effectively solve and be attached in graphene paper preparation process on substrate, be not readily separated the problem of applying, meanwhile, warp
Testing the graphene paper has the chemical property for being better than common graphite alkene paper, and applicant guesses that this is come from two during EFI
The introducing of moveable platform is tieed up, causes graphene oxide microplate scattered more uniform in an assembling process, simultaneously because electric field
The presence of power effect causes the gap between graphene oxide layer to reduce, and can all cause the raising of chemical property；Additionally, due to
Nano fibrous membrane substrate has fibre structure so that the graphene substrate surface also has the micro- knot complementary with substrate tunica fibrosa
Difference in structure, this structure may also cause the lifting of the graphene paper performance.
It is preferred that, the high polymer material described in step (1) is nylon, polyethylene pyrrole network alkanone, polyethylene glycol oxide, poly- inclined fluorine
One or more in ethene, polycaprolactone, polystyrene, polymethyl methacrylate.
It is preferred that, the bottom plate of collecting of described step (1) is the metallic plate with pierced pattern.
It is preferred that, described step (2) is that graphene oxide dispersion is placed in the liquid storage mechanism of electrostatic atomizer,
The collecting mechanism of described electrostatic atomizer is the two-dimensional movement platform that computer is controlled, by step (1) nano fibrous membrane substrate
Be placed in together with the collection bottom plate of its bottom on two-dimensional movement platform, using electrostatic spraying processes on nano fibrous membrane substrate it is straight
Connect spraying combined oxidation graphene film.
As collector there is obtained nano fibrous membrane substrate using the metallic plate with pierced pattern in step (1)
The structure of patterning, collecting plate connection electrostatic spray dress is used as in step (2) using the metallic plate with pierced pattern again
The high voltage power supply put, in the nano fibrous membrane surface EFI graphene oxide film of patterning, between shower nozzle and collecting plate not
Under the double action of the nano fibrous membrane of uniform electric field and patterning so that the graphene oxide film of substrate surface formation
With pattern structure, the graphene paper easily can much with pattern structure is handled by following process, meanwhile, two dimension
Mobile platform can be driven collecting plate by computer control, computer by pre-set programme-control two-dimensional movement platform
Shuttling movement is done on X, Y-direction, so that the even application graphene oxide on nano fibrous membrane substrate, can be according to actual need
Will, the graphene paper of large area is prepared, cycle-index can be also set on computers, to control the thickness of film forming, is expanded
The application field of material.
It is preferred that, during the electrostatic spray of described step (2), the vertical distance of shower nozzle and nano fibrous membrane substrate is
1.5~4cm, 7~10KV of spray voltage, the μ L/min of propulsion pump fltting speed 20~40 of liquid storage mechanism.
It is preferred that, the solvent of the graphene oxide dispersion described in step (2) is DMF (DMF), institute
The graphene oxide concentration contained is 11.7mg/g.
It is preferred that, described step (3) is the height that the composite film material obtained by step (2) is dipped in dissolvable step (1)
In the solvent of Molecularly Imprinted Polymer, immersion is until nano fibrous membrane substrate takes out sample after being completely dissolved, after being cleaned with deionized water
Obtain graphene oxide film.
It is preferred that, described step (3) is that the composite film material obtained by step (2) is carried out at high warm under oxygen atmosphere
Sample is taken out after reason, burn-up nano fibrous membrane substrate, graphene oxide film is produced.
It is preferred that, described step (4) is gone back for the graphene oxide film obtained by step (3) is placed in reducing agent
Original reaction, graphene oxide is reduced to after graphene, and cleaning, dry gained sample produce graphene paper.
It is preferred that, described step (4) is 88wt%'s for the graphene oxide film obtained by step (3) is dipped in into concentration
In hydroiodic acid, heat 100 DEG C and reduce 1 hour, graphene oxide is to be reduced, and is rinsed 3-4 times repeatedly with deionized water, by gained
Sample, which is put into vacuum shelf dryer, produces graphene paper after air drying.
It is preferred that, described step (4) is that the graphene oxide film obtained by step (3) is carried out into height under reducing atmosphere
Warm processing, is reduced to graphene oxide, produces graphene paper.
The beneficial effects of the invention are as follows：The invention provides a kind of grapheme material preparing technical field, compared to existing
Method, the preparation method operates simpler, cost low, and the graphene paper thickness of gained is uniform, with preferable electrochemistry
Can, and be easy to separate with backing material, the graphene paper of large area can be prepared, while can be directly realized by preparation process
The patterning of graphene paper, expands the application field of material.Specifically：
(1) preparation method of the invention is simple to operate, cost is low, the high molecular nanometer that this method is prepared with method of electrostatic spinning
Tunica fibrosa is substrate, and is combined one layer of dense uniform in substrate fiber surface direct spraying using electric field force using electrostatic spraying processes
Graphene oxide film, due to the nano-fiber film as substrate can easily by dissolving, burning etc. method remove,
Graphene paper in uniform thickness finally is can be prepared by oxidation graphene film, the removal substrate approach is not only simple, and
The performance of graphene oxide film and the influence of pattern thing during this so that this method can easily realize graphene paper and lining
The separation at bottom, effectively solves and is attached in graphene paper preparation process on substrate, be not readily separated the problem of applying, meanwhile,
The graphene paper has the chemical property better than common graphite alkene paper after tested, and applicant guesses that this is come from during EFI
The introducing of two-dimentional moveable platform, causes graphene oxide microplate scattered more uniform in an assembling process, simultaneously because electric
The presence of field force effect causes the gap between graphene oxide layer to reduce, and can all cause the raising of chemical property；In addition, by
There is fibre structure in nano fibrous membrane substrate so that the graphene substrate surface also has the micro- knot complementary with substrate tunica fibrosa
The reason for difference in structure, this structure is probably the graphene paper excellent performance.
(2) obtained nano fibrous membrane substrate is made as collector using the metallic plate with pierced pattern in step (1)
Structure with patterning, electrostatic is connected in step (2) using the metallic plate with pierced pattern as collecting plate again
The high voltage power supply of mist device, in the nano fibrous membrane surface EFI graphene oxide film of patterning, in shower nozzle and collecting plate
Between uneven electric field and patterning nano fibrous membrane double action under so that the graphene oxide of substrate surface formation is thin
Film also has pattern structure, and the graphene paper easily can much with pattern structure is handled by following process, meanwhile,
Two-dimensional movement platform can be driven by pre-set programme-control two-dimensional movement platform and be collected by computer control, computer
Pole plate does shuttling movement on X, Y-direction, so that the even application graphene oxide on nano fibrous membrane substrate, can be according to reality
Border needs, and prepares the graphene paper of large area, cycle-index can be also set on computers, to control the thickness of film forming,
Expand the application field of material.
Brief description of the drawings
Fig. 1：The structural representation of electrostatic atomizer used in embodiment；
Fig. 2：The flow chart of the preparation method of embodiment 1；
Fig. 3：The electron scanning micrograph of graphene paper made from embodiment 1；
Fig. 4：The electron scanning micrograph in the section of the graphene paper of embodiment 1；
Fig. 5：Graphene paper electrode constant current charge-discharge curve map made from embodiment 1；
Fig. 6：The optical microscope photograph of graphene paper made from embodiment 2；
In figure, 1- promotes pump；2- liquid storage mechanisms；3- shower nozzles；4- high voltage power supplies；5- two-dimensional movement platforms；6- computers；7-
Collecting plate；8- woven hoses.
Embodiment
For the technical characterstic for illustrating this programme can be understood, this programme is illustrated below by embodiment.
Embodiments of the invention thus electrostatic atomizer structure as shown in figure 1, the electrostatic atomizer include storage
There is the liquid storage mechanism 2 of graphene oxide dispersion, described liquid storage mechanism 2, which is arranged on, to be promoted on pump 1, described liquid storage mechanism
2 connect shower nozzle 3 by woven hose 8, and shower nozzle connects the positive pole of high voltage power supply 4, and the collecting mechanism of the electrostatic atomizer includes two
Tie up the collecting plate 7 that connection high voltage power supply (4) is placed with mobile platform 5, described two-dimensional movement platform 5, the two-dimensional movement
Platform 5 is controlled by computer 6, and computer 6 can drive collecting plate by pre-set programme-control two-dimensional movement platform 5
7 do shuttling movement on X, Y-direction, and cycle-index can be set on computers, to control the thickness of film forming.
Embodiment 1
As shown in the flowchart of figure 2, a kind of preparation method of graphene paper, comprises the following steps：
(1) electro spinning nanometer fiber membrane substrate：Nylon and formic acid in mass ratio 3:22 ratio mixing, is entered with magnetic stirring apparatus
Row stirring obtains uniform spinning precursor liquid in 4 hours, in the liquid storage mechanism that gained spinning precursor liquid is added to electrostatic spinning apparatus, with
Aluminium foil prepares nylon nano fiber film as collector using method of electrostatic spinning, spinning power supply 20kV, spinning apart from 12-15cm,
Spinning solution 3ml, i.e., obtain nano fibrous membrane substrate on aluminium foil；
(2) EFI combined oxidation graphene film：Graphene oxide dispersion is placed in the electrostatic atomizer shown in Fig. 1
Liquid storage mechanism 2 in, by the aluminium foil for being attached with step (1) nano fibrous membrane substrate be placed in electrostatic atomizer two-dimensional movement put down
On platform 5, the collecting plate 7 using the aluminium foil as electrostatic atomizer, using electrostatic spraying processes on nano fibrous membrane substrate it is straight
Spraying combined oxidation graphene film is connect, collecting plate 7 does circulating under the drive of two-dimensional movement platform on X, Y-direction
It is dynamic, in nano fibrous membrane substrate surface uniform deposition formation graphene oxide film, the output voltage of high voltage power supply 4 during this
The vertical distance of 8KV, the propulsion fltting speed 30ul/min of pump 1, shower nozzle and nano fibrous membrane substrate is 2.5cm, described oxidation
The solvent of graphene dispersing solution is DMF, and contained graphene oxide concentration is 11.7mg/g；
(3) substrate is removed：The aluminium foil (collecting plate) for being attached with composite film material obtained by step (2) is dipped in formic acid molten
In liquid, until dissolving after nylon nano fiber film, graphene oxide film is separated with aluminium foil, and sample is cleaned with deionized water
Product, obtain graphene oxide film；
(4) redox graphene：Graphene oxide film obtained by step (3) is dipped in the hydrogen iodine that concentration is 88wt%
In acid, heat 100 DEG C and reduce 1 hour, graphene oxide is to be reduced, and is rinsed repeatedly with deionized water 3 times, and gained sample is put
Enter and produce graphene paper in vacuum shelf dryer after air drying, the thickness of gained graphene paper is about 1-5 μm, depending on EFI circulation time
Depending on number, the graphene paper surface of gained and the electron scanning micrograph in section as shown in Figure 3 and Figure 4, by Fig. 3 and Fig. 4
It can be seen that the graphene paper surface has the micro-structural complementary with substrate fiber, while from sectional view it is also seen that by the party
Material prepared by method is added by finely dispersed graphene film layer stackup to be formed, graphene film interlayer part folded array, piece
Interlayer is combined closely, and gap is small and uniform.
Performance test：The graphene paper of a piece of above-mentioned preparation is taken, the circular electric of about 1 square centimeter of size is cut into
Graphene electrodes are placed on the survey of barrier film two by pole piece, are instilled the appropriate KOH aqueous solution (KOH concentration 6mol/L) and are made as electrolyte
Double layer capacitor, and 8 hours are stood, electro-chemical test is carried out in two-electrode system, test graphene paper electrode is in difference
Constant current charge-discharge characteristic under current density, as shown in figure 5, in different discharge current density 1A/g, 2A/g, 5A/g, under 10A/g
Utilize formula：
The specific capacity respectively 185F/g of electrode can be calculated, 172F/g, 147F/g, 117F/, high rate performance are preferable.
Fig. 5 is that graphene paper makees the constant current charge-discharge curve map that electrode of super capacitor carries out electro-chemical test, it can be seen that
Well, voltage drop very little is calculated the chemical property of the graphene paper prepared using this method under 1A/g current densities
Specific capacity be 185F/g.Electrode capacity is an important indicator of capacitor quality, the pure graphite prepared compared to other method
The volumetric properties of alkene paper are preferable.
Embodiment 2
A kind of preparation method of graphene paper, comprises the following steps：
(1) electro spinning nanometer fiber membrane substrate：Nylon and formic acid in mass ratio 3:22 ratio mixing, is entered with magnetic stirring apparatus
Row stirring obtains uniform spinning precursor liquid in 4 hours, in the liquid storage mechanism that gained spinning precursor liquid is added to electrostatic spinning apparatus, with
Metallic plate with hollow out circular pattern prepares nylon nano fiber film, spinning power supply as collector using method of electrostatic spinning
20kV, spinning obtains nano fibrous membrane apart from 15cm, spinning solution 3ml on the metal sheet surface with hollow out circular pattern
Substrate；
(2) EFI combined oxidation graphene film：Graphene oxide dispersion is placed in the electrostatic atomizer shown in Fig. 1
Liquid storage mechanism 2 in, the metallic plate with hollow out circular pattern for being attached with step (1) nano fibrous membrane substrate is placed in electrostatic
On the two-dimensional movement platform 5 of mist device, the collecting plate 7 using the metallic plate with hollow out circular pattern as electrostatic atomizer,
Using electrostatic spraying processes on nano fibrous membrane substrate direct spraying combined oxidation graphene film, collecting plate 7 two dimension move
Shuttling movement is done on X, Y-direction under the drive of moving platform, in nano fibrous membrane substrate surface uniform deposition formation graphite oxide
Alkene film, the output voltage 10KV of high voltage power supply 4 during this promotes the fltting speed 40ul/min of pump 1, shower nozzle and nano fibrous membrane
The vertical distance of substrate is 4cm, and the solvent of described graphene oxide dispersion is DMF, contained oxidation
Graphene concentration is 11.7mg/g；
(3) substrate is removed：By the composite film material being attached with the collecting plate 7 of composite film material obtained by step (2)
Removed from collecting plate 7, composite film material is dipped in formic acid solution, until dissolving after nylon nano fiber film, spent
Ionized water cleaning sample, obtains graphene oxide film；
(4) redox graphene：Graphene oxide film obtained by step (3) is dipped in the hydrogen iodine that concentration is 88wt%
In acid, heat 100 DEG C and reduce 1 hour, graphene oxide is to be reduced, and is rinsed repeatedly with deionized water 3 times, and gained sample is put
Enter and produce graphene paper in vacuum shelf dryer after air drying, the thickness of gained graphene paper is about 1-5um, depending on EFI circulation time
Depending on number, gained thickness is as shown in Figure 6 for the optical microscope photograph of 3 μm of graphene paper.
Embodiment 3
A kind of preparation method of graphene paper, comprises the following steps：
(1) electro spinning nanometer fiber membrane substrate：Polyethylene pyrrole network alkanone (PVP) is dissolved in deionized water, with before solution-polymerized SBR
The mass fraction for driving PVP in liquid, spinning precursor liquid is 12%, and gained spinning precursor liquid is added to the liquid storage machine of electrostatic spinning apparatus
In structure, using the metallic plate with hollow out circular pattern as collector, nylon nano fiber film, spinning are prepared using method of electrostatic spinning
Power supply 20kV, spinning obtains nanometer apart from 15cm, spinning time 20min on the metal sheet surface with hollow out circular pattern
Tunica fibrosa substrate；
(2) EFI combined oxidation graphene film：Graphene oxide dispersion is placed in the electrostatic atomizer shown in Fig. 1
Liquid storage mechanism 2 in, the metallic plate with hollow out circular pattern for being attached with step (1) nano fibrous membrane substrate is placed in electrostatic
On the two-dimensional movement platform 5 of mist device, the collecting plate 7 using the metallic plate with hollow out circular pattern as electrostatic atomizer,
Using electrostatic spraying processes on nano fibrous membrane substrate direct spraying combined oxidation graphene film, collecting plate 7 two dimension move
Shuttling movement is done on X, Y-direction under the drive of moving platform, in nano fibrous membrane substrate surface uniform deposition formation graphite oxide
Alkene film, the output voltage 10KV of high voltage power supply 4 during this promotes the fltting speed 40ul/min of pump 1, shower nozzle and nano fibrous membrane
The vertical distance of substrate is 4cm, and the solvent of described graphene oxide dispersion is DMF, contained oxidation
Graphene concentration is 11.7mg/g；
(3) substrate is removed：The collecting plate 7 for being attached with composite film material obtained by step (2) is transferred in Muffle furnace,
Logical oxygen, 500-600 DEG C of temperature control is heat-treated 1 hour, and nano fibrous membrane substrate is burned off, and is taken out sample, is produced pure oxygen graphite
Alkene film；
(4) redox graphene：Graphene oxide film obtained by step (3) is placed in Muffle furnace, argon gas is passed through,
800 DEG C of temperature control is heat-treated 1 hour, and graphene oxide is reduced, and obtains pure graphene paper.
Illustrative embodiments listed above are only not to technical scheme described in the invention for understanding that the present invention is used
Restriction, about the those of ordinary skill in field, on the basis of technical scheme described in claim, a variety of changes can also be made
Change or deform, all equivalent changes or deformation should all be covered within the claims of the present invention.The present invention is not
Part is described in detail, is the known technology of those skilled in the art of the present technique.
Claims (10)
1. a kind of preparation method of graphene paper, it is characterised in that comprise the following steps：
(1) electro spinning nanometer fiber membrane substrate：High molecular polymer spinning precursor liquid is prepared, gained spinning precursor liquid is added into electrostatic
In the liquid storage mechanism of device for spinning, high molecular polymer nano fibrous membrane is prepared using method of electrostatic spinning, i.e., on bottom plate is collected
Obtain nano fibrous membrane substrate；
(2) EFI combined oxidation graphene film：Graphene oxide dispersion is placed in the liquid storage mechanism of electrostatic atomizer,
Step (1) nano fibrous membrane substrate is placed on the collecting mechanism of electrostatic atomizer, using electrostatic spraying processes in nanofiber
Direct spraying combined oxidation graphene film on film substrate；
(3) substrate is removed：The nano fibrous membrane substrate of composite film material obtained by step (2) is removed, graphene oxide is obtained thin
Film；
(4) redox graphene：Graphene oxide film reduction obtained by step (3) is produced into graphene paper.
2. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that the macromolecule described in step (1)
Material is nylon, polyethylene pyrrole network alkanone, polyethylene glycol oxide, Kynoar, polycaprolactone, polystyrene, polymethyl
One or more in sour methyl esters.
3. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that the collection of described step (1)
Bottom plate is the metallic plate with pierced pattern.
4. a kind of preparation method of graphene paper as claimed in claim 3, it is characterised in that described step (2) is by oxygen
Graphite alkene dispersion liquid is placed in the liquid storage mechanism of electrostatic atomizer, and the collecting mechanism of described electrostatic atomizer is computer
The two-dimensional movement platform of control, the collection bottom plate by step (1) nano fibrous membrane substrate together with its bottom is placed in two-dimentional shifting
On moving platform, using electrostatic spraying processes on nano fibrous membrane substrate direct spraying combined oxidation graphene film, described step
Suddenly during the electrostatic spray of (2), the vertical distance of shower nozzle and nano fibrous membrane substrate is 1.5~4cm, spray voltage 7~
10KV, the μ L/min of propulsion pump fltting speed 20~40 of liquid storage mechanism.
5. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that the oxidation stone described in step (2)
The solvent of black alkene dispersion liquid is DMF, and contained graphene oxide concentration is 11.7mg/g.
6. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that described step (3) is will step
Suddenly the composite film material obtained by (2) is dipped in the solvent of the high molecular polymer of dissolvable step (1), and immersion is until nanofiber
Film substrate takes out sample after being completely dissolved, and graphene oxide film is obtained after being cleaned with deionized water.
7. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that described step (3) is step
(2) composite film material obtained by takes out sample after high-temperature heat treatment, burn-up nano fibrous membrane substrate are carried out under oxygen atmosphere, produces
Graphene oxide film.
8. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that described step (4) is will step
Suddenly the graphene oxide film obtained by (3), which is placed in reducing agent, carries out reduction reaction, and graphene oxide is reduced to after graphene,
Cleaning, dry gained sample produce graphene paper.
9. a kind of preparation method of graphene paper as claimed in claim 8, it is characterised in that described step (4) is will step
Suddenly the graphene oxide film obtained by (3) is dipped in the hydroiodic acid that concentration is 88wt%, is heated 100 DEG C and is reduced 1 hour, aoxidizes stone
Black alkene is to be reduced, and is rinsed 3-4 times repeatedly with deionized water, gained sample is put into vacuum shelf dryer after air drying and produced
Graphene paper.
10. a kind of preparation method of graphene paper as claimed in claim 1, it is characterised in that described step (4) is will step
Suddenly the graphene oxide film obtained by (3) carries out high-temperature heat treatment under reducing atmosphere, is reduced to graphene oxide, produces stone
Black alkene paper.
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| CN106698405A (en) * | 2017-01-12 | 2017-05-24 | 东南大学 | Method for preparing large-area graphene paper by utilizing hydroiodic acid |
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| CN104409222A (en) * | 2014-11-21 | 2015-03-11 | 华东理工大学 | Preparation method for ternary composites of graphene/manganese dioxide nanosheet /polyaniline nanorod |
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