CN108314024A - A kind of plasma preparation method of transparent graphene conductive film - Google Patents
A kind of plasma preparation method of transparent graphene conductive film Download PDFInfo
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- CN108314024A CN108314024A CN201810411860.2A CN201810411860A CN108314024A CN 108314024 A CN108314024 A CN 108314024A CN 201810411860 A CN201810411860 A CN 201810411860A CN 108314024 A CN108314024 A CN 108314024A
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Abstract
The present invention provides a kind of plasma preparation method of transparent graphene conductive film.Oxidative modification is carried out to the outer layer of the graphene of diatomic layer or three atomic layer level thickness by plasma oxidation technology, obtain being dispersed in the outer modification grapheme material in common solvents, it is restored after preparing film with bar coating method and spin-coating method etc., obtains high conductivity transparent conductive film.The method of the present invention carries out oxidative modification with the two outside layers of three atom layer graphene of plasma technique pair or the outside of diatomic layer, lamella among three atomic layer grapheme materials is not oxidized, still maintain good electric conductivity, diatomic layer graphene only has side to be aoxidized, degree of oxidation also can decrease compared to single layer, simultaneously, oxygen-containing group overcomes diatomic layer or the problem of three atomic layer high-quality graphene materials are difficult to handle and are easy accumulation in modification, realize the holding of the better performances of graphene, it can be applicable to the fields such as photoelectric device and energy storage.
Description
Technical field
The present invention relates to graphene-based transparent conductive film preparation fields, by plasma oxidation technology to double-deck or three
The outer layer of layer high-quality graphene carries out oxidative modification, obtains being dispersed in the outer modification grapheme material in common solvents to make
Standby transparent conductive film.
Background technology
Graphene is one kind completely by sp2The thickness that the carbon atom of hydridization is constituted is only monoatomic layer or several monoatomic layers
Quasi- two dimensional crystal material, no matter chemically stability, flexibility, electric conductivity, the transparency, thermal conductivity or from cost of material side
Face considers one of the material for being considered as most promising transparent conductive film.The graphene of structural integrity is any by being free of
The two dimensional crystal that the carbon hexatomic ring of labile bond is composed, the inert state in surface, chemical stability is high, the phase with solvent
Interaction is weaker, there is stronger Van der Waals force between piece and piece, easy tos produce aggregation, it is made to be insoluble in water and common organic molten
Agent, this has caused great difficulties to the further research and application of graphene.In order to give full play to its advantageous property, and improve
Its molding processibility, such as improve dissolubility and dispersibility in the base, it is necessary to the effective functionalization of graphene progress.It is logical
It crosses and introduces specific functional group, can also impart to the new property of graphene, further expand its application field.Functionalization is to realize
Graphene dispersion, the most important means of dissolving and processing and forming.
Plasma be deprived of by part electronics after atom and atom be ionized after the positron-electron that generates form
Vaporous substance is ionized, this ionized gas is made of atom, molecule, atomic group, ion and electronics, frequently as a kind of to stone
The means that black alkene is modified.Atomic group (free radical) is mainly realized to energy transmission in body surface chemical reaction process
" activation " acts on;Electronics includes mainly two aspects to body surface effect:On the one hand it is the effect of impact to body surface, it is another
Aspect is to cause to chemically react by a large amount of electronic impact.Nourbakhsh etc. has found that oxygen plasma treatment can be shelled to machinery
Decrystallized structure is introduced in the single-layer graphene prepared from method, to open the energy band of graphene, it is made to show semiconductor spy
Property, while the optical property of graphene can also be made to change, show apparent photoluminescence property;The utilizations such as Surwade
Oxygen plasma processes nano pore in single-layer graphene film prepared by CVD method, it is found that the film after processing almost can be with
100% prevention salinity passes through, to obtain the desalination film of high quality.Low-temperature oxygen plasma processing can draw on graphene
Enter more hydroxyl (C-OH) and carbonyl (C=O), so that its defect concentration is increased, crystal grain refinement.Using plasma oxidation technology
Oxidative modification is carried out to the outside of the high-quality graphene material of diatomic layer or three atomic layer level thickness, obtains being dispersed in common
Outer modification grapheme material in solvent overcomes the problem of grapheme material is difficult to handle and is easy to accumulate, realizes graphite
The holding of the better performances of alkene can be applicable to the fields such as photoelectric device and energy storage.
Invention content
To overcome the deficiencies of existing technologies, it is proposed that a kind of new graphene-based method for preparing transparent conductive film solves
Grapheme material is difficult to handle, poorly conductive, high oxygen content, structure destroy big problem.It is saturating that the present invention provides a kind of graphene
The plasma preparation method of bright conductive film, it is small to the laminated structure destruction of graphene, it overcomes graphene and is difficult to handle simultaneously
And the problem of being easy accumulation, the holding of the better performances of graphene is realized, the graphene electrically conducting transparent of high conductivity can be obtained
Film.
The present invention adopts the following technical scheme that:
A kind of plasma preparation method of transparent graphene conductive film, includes the following steps:
(1) lodine chloride, Iodide Bromide or anhydrous ferric trichloride etc. and graphite Hybrid Heating are prepared into second order or three rank graphite
Intercalation compound makes graphite intercalation compound be chemically reacted in turbulent flow, high temperature or Asia/supercritical fluid, to high
Effect prepares two atomic layers or three atomic layer high-quality graphenes;
(2) using plasma oxidation technology is to the outer of the high-quality graphene material of diatomic layer or three atomic layer level thickness
Side carries out oxidative modification, obtains being dispersed in the outer modification grapheme material in common solvents, with bar coating method and spin coating
Method etc. restores after preparing film, obtains high conductivity transparent conductive film.
The intercalator of second order or three rank graphite intercalation compounds is lodine chloride, Iodide Bromide or anhydrous trichlorine in step (1)
Change iron etc..
The residing environment of chemical reaction is the turbulent flow of high speed rotation generation, has the high temperature ring of protective atmosphere in step (1)
Border or Asia/supercritical fluid environment.
Chemical reaction type is Iodide Bromide and the reacting of water, the pyrolytic or ferric trichloride of lodine chloride in step (1)
With reacting for hydrogen peroxide.
Oxygen is excited into plasma by step (2) plasma oxidation technology, then etches diatomic layer or three atoms
Layer graphene outer surface is modified processing.
In step (2) outside carry out diatomic layer that oxidative modification be preparation or three atom layer graphene outer surfaces wait from
Oxygen-containing group is attached under daughter oxidation processes.
The present invention has following advantage:
(1) it is proposed by the present invention using plasma oxidation technology to the outside of diatomic layer or three atom layer graphenes into
Row oxidative modification prepares the strategy of high conductivity transparent conductive film.Oxygen-containing group on the outside of graphene makes graphene be dispersed among
In common solvents, overcome the problems, such as that grapheme material is difficult to handle and is easy accumulation.Three atom layer graphene middle sheets are protected
Low oxygen content ensure that graphene electrically conducting transparent caused by holding outside oxidation of the graphene eigen state with diatomic layer graphene
The high conductivity of film.
(2) it is relatively low to prepare requirement of the method for grapheme material and transparent conductive film to equipment by the present invention, is suitable for industry
Or laboratory operation.
Description of the drawings
Fig. 1 is the method for the present invention diatomic layer and three atomic layer graphene film schematic diagrames.
Fig. 2 is the TEM figures that the method for the present invention plasma oxidation handles graphene.
Fig. 3 is the infrared figure that the method for the present invention plasma oxidation handles graphene.
Specific implementation mode
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1
(1) 60g Iodide Bromide is uniformly mixed with 100mg expanded graphites, is packed into protection gas Ar gas, is enclosed within 100mL glass
In glass bottle.
(2) vial is placed in 100 DEG C of oil bath environment, is heated 48h, is prepared three rank graphite intercalation compounds.
(3) graphite intercalation compound is taken out and is filtered from vial rapidly.
(4) intercalation compound is put into rapidly in the water heating kettle that volume is 50mL, 10mL aqueous solutions is added into water heating kettle,
Fix water heating kettle equipment rapidly.
(5) water heating kettle is heated to 180 DEG C, 1h, reaction is kept to finish, take out sample, cleaning sample obtains three atomic layers
High-quality graphene powder aggregation.
(6) three atomic layer high-quality graphenes are put into small size vacuum oxygen plasma cleaning machine cavity, utilize vacuum pump
Operating room is carried out to vacuumize the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, three atomic layer graphene solutions are modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Fig. 2 is the TEM figures that the present embodiment plasma oxidation handles graphene.
Fig. 3 is the infrared figure that the present embodiment plasma oxidation handles graphene.
Embodiment 2
(1) 30g Iodide Bromide is uniformly mixed with 50mg expanded graphites, is packed into protection gas Ar gas, is enclosed within 50mL glass
It in bottle, is placed in 100 DEG C of oil bath environment, heats 12h, prepare three rank graphite intercalation compounds.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly.
(3) intercalation compound is put into rapidly in the supercritical water device that volume is 50mL.
(4) 2mL aqueous solutions are added into supercritical water device, fix equipment rapidly.
(5) high supercritical water installations are heated to 180 DEG C, boost in pressure to 22.1Mpa keeps 1h, reaction to finish, and takes out
Sample, cleaning sample obtain graphene powder aggregation.
(6) three atomic layer high-quality graphenes are put into small size vacuum oxygen plasma cleaning machine cavity, utilize vacuum pump
Operating room is carried out to vacuumize the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, three atomic layer graphene solutions are modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Embodiment 3
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare three rank graphite intercalation compounds.
(2) graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(3) graphite intercalation compound is put into rapidly to the supercritical CO that volume is 50mL2In device.
(4) to supercritical CO2The hydrogen peroxide solution that 5mL mass fractions are 30% is added in device, fixes equipment rapidly.
(5) by high supercritical CO2Device is heated to 38 DEG C, and boost in pressure to 75atm keeps 1h, reaction to finish, and takes out sample
Product, cleaning sample obtain graphene powder aggregation.
(6) three atomic layer high-quality graphenes are put into small size vacuum oxygen plasma cleaning machine cavity, utilize vacuum pump
Operating room is carried out to vacuumize the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, three atomic layer graphene solutions are modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Embodiment 4
(1) by the anhydrous FeCl of 0.3g3It being mixed with 0.05g expanded graphites, vacuum tightness, 1h is warming up to 380 DEG C, maintains 12h,
Prepare three rank graphite intercalation compounds.
(2) graphite intercalation compound is dissolved in dilute hydrochloric acid solution, filters drying, for use.
(3) intercalation compound is distributed in organic solvent N-Methyl pyrrolidone, prepares the suspension of 5mg/mL.
(4) hydrogen peroxide solution that the mass fraction of 10mL is 30% is added, runs supercentrifuge, rotating speed 7000 at once
Rpm, the time is 0.5 hour.
(5) reaction finishes, and cleaning sample obtains three atomic layer graphene powder aggregations.
(6) three atomic layer high-quality graphenes are put into small size vacuum oxygen plasma cleaning machine cavity, utilize vacuum pump
Operating room is carried out to vacuumize the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, three atomic layer graphene solutions are modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Embodiment 5
(1) 30g Iodide Bromide is uniformly mixed with 50mg expanded graphites, is packed into protection gas Ar gas, is enclosed within 50mL glass
It in bottle, is placed in 100 DEG C of oil bath environment, heats 12h, prepare three rank graphite intercalation compounds.
(2) graphite intercalation compound is taken out and is filtered from vial rapidly.
(3) all graphite intercalation compounds are put into quartz boat rapidly, quartz boat is put into argon gas protection atmosphere.
(4) quartz boat is heated to 800 DEG C.
(5) reaction finishes, and takes out sample, and cleaning sample obtains graphene powder aggregation.
(6) three atomic layer high-quality graphenes are put into small size vacuum oxygen plasma cleaning machine cavity, utilize vacuum pump
Operating room is carried out to vacuumize the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, three atomic layer graphene solutions are modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Embodiment 6
(1) 30g lodine chlorides are uniformly mixed with 50mg high temperature directional thermal decomposition graphite, are packed into protection gas Ar gas, are enclosed within
In 50mL vials.
(2) it is placed in 160 DEG C of oil bath environment, heats 48h, prepare second order graphite intercalation compound.
(3) graphite intercalation compound is taken out and is filtered from vial rapidly.
(4) all graphite intercalation compounds are put into quartz boat rapidly, quartz boat is put into argon gas protection atmosphere.
(5) quartz boat is heated to 800 DEG C, 5min, reaction is maintained to finish, take out sample, cleaning sample obtains the double-deck stone
Black alkene powder aggregates.
(6) bilayer graphene is put into small size vacuum oxygen plasma cleaning machine cavity, using vacuum pump by operating room into
It goes and vacuumizes the vacuum degree for reaching 0.02-0.03mbar maintenance 0.5 hour.
(7) working gas is oxygen, and power about 300W maintains 0.5h.
(8) by product, bilayer graphene solution is modified in ultrasonic disperse, acquisition outside in ethanol.
(9) transparent conductive film is prepared using bar coating method.
(10) transparent conductive film immerses hydroiodic acid solution and is restored, and is taken out after half an hour.
(11) transparent conductive film is cleaned repeatedly with ethyl alcohol, dry.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (6)
1. a kind of plasma preparation method of transparent graphene conductive film, includes the following steps:
(1) lodine chloride, Iodide Bromide or anhydrous ferric trichloride etc. and graphite Hybrid Heating are prepared into second order or three rank graphite intercalations
Compound makes graphite intercalation compound be chemically reacted in turbulent flow, high temperature or Asia/supercritical fluid, to efficiently make
Standby two atomic layers or three atomic layer high-quality graphenes;
(2) using plasma oxidation technology to the outside of the high-quality graphene material of diatomic layer or three atomic layer level thickness into
Row oxidative modification obtains being dispersed in the outer modification grapheme material in common solvents, with bar coating method and spin-coating method etc.
It is restored after preparing film, obtains high conductivity transparent conductive film.
2. preparation method according to claim 1, which is characterized in that second order described in step (1) or three rank graphite intercalations
The intercalator of compound is lodine chloride, Iodide Bromide or anhydrous ferric trichloride etc..
3. preparation method according to claim 1, which is characterized in that chemically react residing environment described in step (1)
The turbulent flow that is generated for high speed rotation has the hot environment or Asia/supercritical fluid environment of protective atmosphere.
4. preparation method according to claim 1, which is characterized in that it is bromination to chemically react type described in step (1)
The reacting of iodine and water, the pyrolytic of lodine chloride or ferric trichloride are reacted with hydrogen peroxide.
5. preparation method according to claim 1, which is characterized in that plasma oxidation technology described in step (2) will
Oxygen is excited into plasma, then etches diatomic layer or three atom layer graphene outer surfaces are modified processing.
6. preparation method according to claim 1, which is characterized in that outside described in step (2) carries out oxidative modification and is
The diatomic layer of preparation or three atom layer graphene outer surfaces attached oxygen-containing group under plasma oxidation processing.
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Effective date of registration: 20211101 Address after: No. 108 and 109, Lizhi building, No. 625, geguan Road, Jiangbei new area, Nanjing, Jiangsu 211500 Patentee after: Zhang Zheng Address before: 224000 No.2, hope Avenue South Road, Yancheng City, Jiangsu Province Patentee before: YANCHENG TEACHERS University |