CN101474897A - Grapheme-organic material layered assembling film and preparation method thereof - Google Patents
Grapheme-organic material layered assembling film and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a graphene-organic material layered assembly film and a preparation method thereof. The preparation method comprises: using a graphene material and an organic material as raw materials, utilizing interaction of static electricity, hydrogen bonds, coordinate bonds or charge transfer and the like between the graphene and the organic material, and superposing films layer by layer through the film preparation methods such as spin coating, spraying, dipping, lifting and pulling and the like to prepare the film, wherein the thickness of each layer of the film can be controlled between 10 nanometers and 2 millimeters according to requirement. The layered assembly film and the preparation method have the characteristics that multilayer film materials with different functions are prepared by utilizing unique electric, magnetic, mechanical and chemical properties of the grapheme, and can be used as biomaterials, conductive materials, electromagnetic shielding and wave absorbing materials, photovoltaic materials, electrode materials, film filtering and separating materials, and the like to be applied to chemistry and chemical industry, biology and precision instruments, and manufacture of micro electrons, machinery and aviation and aerospace devices according to the selected different organic materials.
Description
Technical field
The present invention relates to the preparation of thin-film material, particularly a kind of Graphene-organic material layered assembling film and preparation method thereof.Utilize electricity, magnetic, mechanics and the chemical property of Graphene uniqueness, difference according to selected organic material, prepare multilayered film material, can be used as the manufacturing that biomaterial, conductive material, electromagnetic shielding and absorbing material, photovoltaic material, electrode material, membrane filtration and parting material etc. are applied to chemical, biology, precision instrument and microelectronics, machinery and Aero-Space device with difference in functionality.
Background technology
The stratiform component film is the multilayered film material that utilizes interactions such as static between the different material, hydrogen bond, coordinate bond, molecular recognition, electric charge transfer to prepare.1966, reported first such as Iler be the film preparing technology of motive force based on the electrostatic interaction between the material of oppositely charged, but do not cause the concern that people are enough at that time.Up to 1991, Decher etc. proposed this technology of static alternating deposit again, and were applied to the preparation of the ultrathin membrane of functional polyalkylene electrolyte and organic molecule, and this stratiform package technique just really attracts much attention.In the last few years, the stratiform package technique has obtained developing swift and violently, destatic outside the interaction, based on hydrogen bond, coordinate bond, molecular recognition, interactional motive forces such as electric charge transfer also are applied to the preparation of stratiform component film, greatly enrich the kind and the quantity that can be used for the material that layered assembling film constructs, comprised polyelectrolyte, organic and inorganic particles, large biological molecule such as protein, enzyme, virus and the organic dyestuff and the oligomer that contain few electric charge, dendrimers etc. all can be used as the preparation of constructing primitive and carrying out layered assembling film at interior numerous materials.This technology also has the restriction that film forming is not subjected to substrate kind, shape, size etc., the chemical composition of film and thickness, surface topography are controlled, preparation process is simple, make things convenient for advantages such as large-scale production, make the stratiform component film be subjected to people's attention day by day, and become one of the most promising film technique of constructing functional membrane material.
Graphene (Graphene, or title mono-layer graphite) is meant the monolayer carbon atom of tightly packed one-tenth bi-dimensional cellular shape lattice structure, and it is the elementary cell that makes up other dimension graphite materials (as zero dimension fullerene, one dimension CNT, three-dimensional graphite).Scientific research finds that Graphene has excellent electric property, and its room temperature electron mobility can reach 10,000cm
2V
-1s
-1Have excellent mechanical property, its hot strength and Young's modulus can reach 130GPa and 1TPa respectively, are the highest materials of finding at present of intensity; Its thermal conductivity can reach 5000W/m.K, is three times of pure diamond under the room temperature, is higher than the highest CNT of thermal conductivity of generally acknowledging at present.In addition, the researcher finds that also Graphene has light transmission and gas impenetrability.The excellent properties of grapheme material makes it have good application prospects in a lot of fields such as fields such as nanometer electronic device, chemistry and biology sensor, film separation and filtration, nesa coating, battery and capacitor, an emission.
Summary of the invention
The purpose of this invention is to provide a kind of Graphene-organic material layered assembling film and preparation method thereof, it is based on the layered assembling film and the preparation method of Graphene and organic material.Utilize the interactions such as static, hydrogen bond, coordinate bond or electric charge transfer between Graphene and the organic material to prepare multilayered film material, this material can not only make full use of Graphene and organic material self property, and exist interfacial interaction between every layer material, thereby demonstrate unique function, in the thin-film material science, light, electricity, magnetic information conversion and processing apparatus, bioengineering, aspects such as Surface Engineering and molecular configuration have uses potential widely.
A kind of Graphene provided by the invention-organic material layered plural layers that are assembled into, every tunic is thick in 10nm-2mm, it is to be raw material with Graphene and organic material, according to mass ratio 1～100:1～100 of Graphene and organic material, on substrate or directly, apply the stack film forming at device surface by the method that applies.Or, after finishing, preparation removes the layered assembling film that sacrifice layer (for example, using solvent that sacrifice layer is dissolved) obtains self-supporting by precoating layer polymer sacrifice layer between substrate and self-assembled film.
Described Graphene is meant that the mono-layer graphite atom that molecular skeleton is arranged by hexagonal lattice forms, and pass through functionalization and obtain contain the two dimensional surface material that enriches organo-functional group.Thickness distribution is between 0.34 to 2nm, and diameter is distributed in 10nm between the 20 μ m.
Described grapheme material can contain carboxyl, hydroxyl, epoxy bond, sulfonic group, phenyl isocyanate, thiophene, pyrroles, aniline through functionalization and/or contain the chain alkyl functional group of 6 to 18 carbon at least a.The molar percentage of contained organo-functional group is 10%～30%.And according to the difference of contained functional group, grapheme material can dissolve in water or other organic solvents, therefore can be made into certain density solution.When containing organo-functional group such as carboxyl, hydroxyl, epoxy bond, sulfonic group, Graphene has good dissolubility in water; Can well be dissolved in the organic solvent when containing functional groups such as sulfonic group, phenyl isocyanate, thiophene, pyrroles, aniline, chain alkyl.
Described organic material can be at least a in organic molecule and/or the macromolecular material.
Described organic molecule can be at least a in metal organic complex, aromatics, heterocyclic compound, luxuriant class, porphyrin class and/or the phthalocyanine-like compound.
Described macromolecular material can be at least a in polyaminoacid and derivative, polyamine, polymethylacrylic acid, polyurethane, polyacrylate, polyamide, polyester, ABS, polyethylene, polypropylene, Merlon, polyvinyl chloride, epoxy resin, polyimides, shitosan, gelatin, phenolic resins and/or the rubber.Polymer molecular weight is between 2000-200000.
The preparation method of Graphene-organic material layered assembling film provided by the invention may further comprise the steps:
1) Graphene is added in entry or the organic solvent, handled 0.5-2 hour, Graphene is dispersed or dissolved through ultrasonic wave;
2) be coated on the substrate by painting method Graphene solution or the device surface film forming, washing, drying;
3) organic material or its precursor fully be dissolved in make homogeneous solution or colloidal sol in corresponding water and/or the organic solvent, by painting method at above-mentioned graphene film surface filming, washing, drying, heat treatment;
Repeat 2)-3) step, the coating that circulates is layering, and up to reaching the required number of plies, can obtain multilayered film material based on grapheme material through Overheating Treatment again.
Described painting method comprises spin coating, spraying, dipping-lift.
Described organic solvent is a methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, acetone, ethyl acetate, chloroform, carbon tetrachloride, oxolane, N, dinethylformamide, dimethyl sulfoxide (DMSO), benzene, toluene, dimethylbenzene, chlorobenzene, dichloro-benzenes, trichloro-benzenes.
Described heat treatment is 60-300 ℃ of roasting 1-12 hour.Described cycle-index at least once.
Outstanding characteristics of the present invention are electricity, magnetic, mechanics and chemical property of utilizing Graphene good, difference according to selected organic material, prepare multilayered film material, can be used as the manufacturing that biomaterial, conductive material, electromagnetic shielding and absorbing material, photovoltaic material, electrode material, membrane filtration and parting material etc. are applied to chemical, biology, precision instrument and microelectronics, machinery and Aero-Space device with difference in functionality.
Owing to the low price of Graphene, light weight has the solution handlability among the present invention, and processing and forming is good.As carrier, can realize load and the controlled release of guest molecule in multilayer film with Graphene-cationic polymer layered assembling film, be particularly suitable for coating as genophore or medicament slow release.Simultaneously, because Graphene has electricity best in the known nano material and mechanical property and good heat conductivility, make multilayered film material of the present invention have higher intensity and modulus and be easy to heat radiation again, be expected under particular surroundings such as precision instrument and microelectronics, building, machinery and Aero-Space, to obtain extensive use.
Description of drawings
The stereoscan photograph on Fig. 1 Graphene/polymine layered assembling film (embodiment 2) surface.
The stereoscan photograph of Fig. 2 Graphene/polymine layered assembling film (embodiment 2) section.
The specific embodiment
Below by embodiment the present invention is specifically described; present embodiment only is used for the present invention is further detailed; can not be interpreted as limiting the scope of the invention; those skilled in the art makes some nonessential improvement and adjustment according to the content of the invention described above, all belongs to protection domain of the present invention.
Embodiment 1: the preparation of Graphene
5g graphite and 3.75g sodium nitrate (analyzing pure) are added in the flask, add the 375mL concentrated sulfuric acid (analyzing pure) then.In ice-water bath, slowly add 22.5g potassium permanganate while stirring afterwards, the joining day is controlled at 1h, keeps 2h to make it to be cooled to room temperature afterwards.Stirring at room five days.In these five days, reaction solution fades to green earlier, and then becomes dark-brown, and it is brown to become brick at last, and it is thick to become sticky.Reaction solution is slowly joined in the dilute sulfuric acid of 700mL5wt%, the joining day is controlled at 1h, keeps stirring, and temperature is controlled at 98 ℃.Reactant liquor continues to stir 2h under this temperature again, is cooled to 60 ℃ then.Add 15mL hydrogen peroxide (30% aqueous solution), keep 2h, reduce to room temperature afterwards, stir 2h again at 60 ℃.For removing the ion that oxidizing substance brings, especially manganese ion, use centrifugation method to carry out removal of impurities reaction solution, centrifugal number of times is 15 times: centrifugal 10min under 4000rpm, remove supernatant, the mixed liquor that adds the 2L3wt% concentrated sulfuric acid/0.5wt% hydrogen peroxide, strong agitation and under 140W the ultrasonic 30min of water-bath, repeat 15 times.Use the hydrochloric acid of 3wt% to repeat above-mentioned steps 3 times afterwards, use distilled water to repeat 1 time.Afterwards reactant liquor is transferred in the acetone, removed remaining acid.Drying obtains Graphene then.This grapheme material contains carboxyl, hydroxyl, the epoxide group of 10-20mol.%.
Embodiment 2:
The preparation of material liquid: 50mg Graphene (press the method preparation among the embodiment 1, average diameter 1-2 μ m, thickness is about 0.7-1.4nm) is added in the 250ml water, handled 30 minutes, it is dissolved fully through ultrasonic wave (500W); Get 2g polymine (PEI, mean molecule quantity 10000) and be dissolved in the 200ml deionized water, stir the back set aside for use.
The following step of preparation process of Graphene/polymine layered self-packaging film:
1. on teflon substrate, be coated with one deck cellulose polyacetate (1wt.%, acetone soln) sacrifice layer with spin-coating method, dry naturally;
2. the polymine drips of solution is added on the substrate with 3000 rev/mins of rotations, spin coating is after 15 seconds, and the 60-80 ℃ of oven dry in back dried in washing;
3. the Graphene drips of solution that configures is added on the substrate with 3000 rev/mins of rotations, spin coating is after 15 seconds, washing, after drying under the room temperature again through 80 ℃ of oven dry;
Repeat the 2-3 step, circulate 50 times.The following 120 ℃ of heat treatments of nitrogen protection 3 hours.With molten substrate and the middle sacrifice layer of membrane material of going of acetone, obtain the Graphene/polymine layered assembling film of self-supporting.The about 1 μ m of thickness.
Embodiment 3:
The preparation of material liquid: 200mg Graphene (press the method preparation among the embodiment 1, average diameter 5-10 μ m, thickness is about 1-2nm) is added in the 200ml ethanol, handled 40 minutes, make it dissolve the back set aside for use fully through ultrasonic wave (500W); Epoxy resin (bisphenol A-type, 618), low molecular polyamides and ferrocene dissolve in the acetone soln by mass ratio 55/30/1, stir, and obtain concentration and be 50% solution.
The preparation of Graphene/epoxy resin-ferrocene plural layers:
1. on teflon substrate, be coated with one deck cellulose polyacetate (1wt.%, acetone soln) sacrifice layer with spin-coating method, dry;
2. aforesaid substrate is impregnated in epoxy resin-ferrocene solution, pulls out after 2 seconds, dry under the room temperature;
3. the Graphene drips of solution that configures is added on the substrate with 3000 rev/mins of rotations, spin coating was dried under the room temperature after 30 seconds, again through 40-80 ℃ of low temperature drying;
4. above-mentioned substrate is impregnated in epoxy resin-ferrocene solution, pulls out after 2 seconds, dry under the room temperature;
Repeat the 3-4 step, circulate after 5 times, sample 120 ℃ of following heat treatments 12 hours, with the molten sacrifice layer that goes to substrate and membrane material centre of acetone, can be obtained Graphene/epoxy resin-ferrocene multilayered film material.The about 2mm of thickness.
Embodiment 4:
The preparation of dodecyl Graphene: the 200mg Graphene (is pressed the method preparation among the embodiment 1, average diameter 10-100nm, thickness is about 0.34-0.7nm) add 80ml thionyl chloride and 2ml N, in the mixed solution of dinethylformamide, 70 ℃ were reacted 24 hours down.After reaction is finished, the thionyl chloride that pressure reducing and steaming is excessive, and with dry toluene washing three times.Add 100mg lauryl amine, 2ml triethylamine and 80ml anhydrous chloroform then in above-mentioned solid, the lucifuge reaction is three days under the protection of inert gas.After reaction is finished, above-mentioned drips of solution is added in the acetone soln to be settled out product, filters, with chloroform washing five times, each washing of water and acetone once, vacuum drying 24h under the room temperature obtains connecting with amido link the Graphene black solid powder-product of dodecane.Get 200mg the said goods and join 300ml N, in the dinethylformamide (DMF), ultrasonic dispersion makes it dissolve the back set aside for use fully;
Get 100mg 5-(4) aminocarbonyl phenyl)-10,15,20-triphenyl porphyrin (TTP-NH
2) be dissolved among the 100ml DMF.
Graphene/TTP-NH
2The preparation of plural layers
1. the Graphene drips of solution that configures is added on the glass substrate with 3000 rev/mins of rotations, spin coating 15 seconds washes twice with DMF, after drying under the room temperature again through 40-60 ℃ of low temperature;
2. with TTP-NH
2Drips of solution is added on the substrate with 3000 rev/mins of rotations, and spin coating 15 seconds cleans twice with DMF, dries 40-60 ℃ of low temperature drying under the room temperature;
Repeat above-mentioned steps, circulate 40 times, 80 ℃ of heat treatment 2 hours obtains Graphene/TTP-NH
2Plural layers.The about 2 μ m of thickness.
Embodiment 5:
The preparation of sulfonated graphene solution: the 225mg Graphene (is pressed the method preparation among the embodiment 1, average diameter 1-2 μ m, thickness is about 0.4-1.1nm) add in the 225ml water, ultrasonic dispersion forms even clear solutions, and it is 9-10 that the sodium carbonate liquor of Dropwise 5 % is transferred the pH value of solution.The aqueous solution (containing the 2.7g sodium borohydride) of 67.5ml sodium borohydride is added dropwise in the above-mentioned solution, reacted 90 minutes down at 80 ℃.The black solid that obtains is washed-centrifugal repeatable operation five times.Be dispersed in the 225ml water solid is ultrasonic again, add 2g (4-sulfonic benzo diazonium villaumite), 200ml water and hydrochloric acid (0.2g, mixed solution 1N).Ice bath reacted 2 hours down, rose to room temperature reaction 12 hours then gradually.Solid is washed-centrifugal repeatable operation five times.Be dispersed in the 225ml water solid is ultrasonic again, add the 6ml hydrazine hydrate, 100 ℃ of reactions 24 hours down.Solid is washed-centrifugal repeatable operation five times.Obtain the Graphene of sulfonation after the drying.The 100mg sulfonated graphene is added 200ml water, handled 30 minutes, make it dissolve the back set aside for use fully through ultrasonic wave (500W).
The preparation of Kynoar-ethyl orthosilicate mixed solution: (PVDF) is dissolved in N with the 2g Kynoar, be configured to the solution of 20wt.% in N-dimethylacetylamide (DMAC) solvent, add 0.4g polyvinylpyrrolidone (PVP, molecular weight 30000, pore former) and 0.1g sodium dodecyl benzenylsulfonate (anion surfactant, dispersant), stir; The 2ml ethyl orthosilicate is added in the mixed solution of 40ml ethanol and water, drip the hydrochloric acid solution of a certain amount of pH=2, after stirring, be added drop-wise in the DMAC solution of PVDF, stir.
The preparation of Graphene/Kynoar-silica stratiform self-assembled film:
1. Kynoar-ethyl orthosilicate mixed solution is added drop-wise on the quartz plate with 3000 rev/mins of rotations, spin coating 15 seconds cleans twice with DMAC, dries 40-60 ℃ of low temperature drying under the room temperature;
2. the Graphene drips of solution that configures is added on the quartz plate with 3000 rev/mins of rotations, spin coating 30 seconds, the washing twice, after drying under the room temperature again through 40-60 ℃ of low temperature drying;
3. Kynoar-ethyl orthosilicate mixed solution is added drop-wise on the quartz plate with 3000 rev/mins of rotations, spin coating 15 seconds cleans twice with DMAC, dries 40-60 ℃ of low temperature drying under the room temperature;
Repeat the 2-3 step, circulate 50 times, 60-80 ℃ of heat treatment 2 hours obtains Graphene/Kynoar-silica stratiform self-assembled film.The about 20 μ m of thickness.
Claims (10)
1, a kind of Graphene-organic material layered assembling film, it is characterized in that it is is raw material with Graphene and organic material, mass ratio 1～100:1～100 according to Graphene and organic material, method by film forming applies the multilayer stack film that forms at device surface on substrate or directly, every tunic is thick in 10nm-2mm.
2,, it is characterized in that described organic material is at least a in organic molecule, the macromolecular material according to the described layered assembling film of claim 1.
3,, it is characterized in that described organic molecule is at least a in metal organic complex, aromatics, heterocyclic compound, luxuriant class, porphyrin class and/or the phthalocyanine-like compound according to the described layered assembling film of claim 2.
4,, it is characterized in that described macromolecular material can be at least a in polyaminoacid and derivative, polyamine, polymethylacrylic acid, polyurethane, polyacrylate, polyamide, polyester, ABS, polyethylene, polypropylene, Merlon, polyvinyl chloride, epoxy resin, polyimides, shitosan, gelatin, phenolic resins and/or the rubber according to the described layered assembling film of claim 2; Polymer molecular weight is between 2000-200000.
5, according to the described layered assembling film of claim 1, it is characterized in that the mono-layer graphite atom that described grapheme material is meant that molecular skeleton is arranged by hexagonal lattice forms, and what obtain through functionalization contains the two dimensional surface material that enriches organo-functional group, its thickness distribution between 0.34 to 3nm, average diameter at 10nm between the 20 μ m; Described organo-functional group is that carboxyl, hydroxyl, epoxy bond, sulfonic group, phenyl isocyanate, thiophene, pyrroles, aniline and/or the chain alkyl functional group that contains 6 to 18 carbon are at least a; The molar percentage of contained organo-functional group is 10%～30%.
6, according to the described layered assembling film of claim 1, it is characterized in that described layered assembling film is: Graphene/polymine layered assembling film, Graphene/epoxy resin-ferrocene plural layers, Graphene/TTP-NH
2Plural layers or Graphene/Kynoar-silica stratiform self-assembled film.
7, the preparation method of the described layered assembling film of claim 1 is characterized in that may further comprise the steps:
1) Graphene is added in entry or the organic solvent, handled 0.5-2 hour, Graphene is dispersed or dissolved through ultrasonic wave;
2) organic material or its precursor fully be dissolved in make homogeneous solution or colloidal sol in corresponding water or the organic solvent, by painting method in the substrate surface film forming, washing, drying;
3) with Graphene solution by painting method at the organic layer surface filming, the washing, drying;
Repeat 2)-3) step, up to reaching the required number of plies; Can obtain layered self-packaging film through Overheating Treatment based on Graphene and organic material.
8,, it is characterized in that described painting method comprises spin coating, spraying, dipping-pulling method according to the described preparation method of claim 7.
9,, it is characterized in that described organic solvent is a methyl alcohol, ethanol, ethylene glycol according to the described preparation method of claim 7, isopropyl alcohol, acetone, ethyl acetate, chloroform, carbon tetrachloride, oxolane, N, dinethylformamide, N, N-dimethylacetylamide, dimethyl sulfoxide (DMSO), benzene, toluene, dimethylbenzene, chlorobenzene, dichloro-benzenes, trichloro-benzenes.
10,, it is characterized in that described heat treatment is 60-200 ℃ of roasting 1-12 hour according to the described preparation method of claim 7.
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