CN104402242A - Preparation method for superhydrophobic rigid carbon film - Google Patents
Preparation method for superhydrophobic rigid carbon film Download PDFInfo
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- CN104402242A CN104402242A CN201410654545.4A CN201410654545A CN104402242A CN 104402242 A CN104402242 A CN 104402242A CN 201410654545 A CN201410654545 A CN 201410654545A CN 104402242 A CN104402242 A CN 104402242A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/28—Other inorganic materials
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Abstract
The invention discloses a preparation method for a superhydrophobic rigid carbon film. The preparation method comprises the following steps: preparing a graphene/ polyimide precursor film; preparing a graphene/ glass carbon composite film adopting a special micro-nano structure; performing surface treatment on the graphene/ glass carbon composite film to obtain the rigid carbon film with superhydrophobicity. The superhydrophobic rigid carbon film has the advantages of being uniform and smooth, controllable in thickness and shape, simple and feasible in preparation method, good in mechanical properties, good in superhydrophobicity and the like, and has a wide application prospect in the self-cleaning field, the microfluidic system field, the biocompatibility field and the like.
Description
Technical field
What the present invention relates to is the preparation of a kind of functional carbon film in carbon material field, is specifically related to a kind of preparation method of super-hydrophobic rigidity C film.
Background technology
Super-hydrophobic research starts from natural animals and plants, and such as the leg of lotus leaf surface, water skipper, the wing etc. of dragonfly all show super-hydrophobic phenomenon, and therefore, it receives pays close attention to widely.Super-hydrophobic definition is that the water contact angle of material surface is greater than 150 °, and Structure deformation angle is less than 10 °.Utilize the surface property of its uniqueness, super hydrophobic material in automatically cleaning field, microfluid system direction, all respects such as biocompatibility field are with a wide range of applications.Realize super-hydrophobic mode and be mainly divided into two kinds, one constructs micro-nano structure at material surface; Another kind is the surface energy being reduced material surface by chemical process.
Through finding the retrieval of prior art, the material such as fluorinated polymkeric substance, metal or metal oxide, carbon nano-tube material, Graphene all achieves ultra-hydrophobicity.In carbon material field, the people such as Lau K.K.S. write articles proposition Nano Letters the 3rd volume 1701 ~ 1705 pages, successfully prepare the carbon nanotube forest array with ultra-hydrophobicity; Proposition is write articles Small the 9th volume 75 ~ 80 pages by Shenyang seminar of Cheng Huiming research institute of metal institute, is obtained the grapheme foam material with super-hydrophobicity by template chemical vapour deposition.Carbon material like this has the advantages such as good anti-adhesive, automatically cleaning, anticorrosive, low friction.But the starting material of preparing of carbon nanotube and grapheme material have the shortcomings such as expensive, preparation process is complicated, cost rate is low.
Therefore, except with carbon nanotube and Graphene for except starting material, be badly in need of exploitation and construct more simple, more extensively, more cheap carbon material and micro-nano structure thereof, and realize its surface super hydrophobic performance.
Summary of the invention
The present invention is directed to prior art above shortcomings, a kind of preparation method of super-hydrophobic rigidity C film is provided, through Graphene/polyimide precursor preparation, there is the step such as the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure, the surface treatment of Graphene/vitreous carbon laminated film, realize the preparation of super-hydrophobic rigidity C film.
The present invention is achieved by the following technical solutions, and a kind of preparation method of super-hydrophobic rigidity C film, comprises the following steps:
The first step, the preparation of Graphene/polyimide precursor film: at room temperature, by a certain amount of graphene dispersion in organic solvent, ultrasonic disperse for some time, after adding a certain amount of 4,4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stirring polyreaction is spent the night, and obtains Graphene/polyamic acid solution.By Graphene/polyamic acid solution casting film-forming on the glass sheet, remove after solvent at 50 ~ 180 DEG C of heating 1 ~ 24h, then heating 1 ~ 24h under the condition being placed in 180 ~ 350 DEG C of vacuum or protection of inert gas, obtain Graphene/polyimide precursor film.
Preferably, the concentration of Graphene dispersion in organic solvent is 0.01 ~ 5mg/mL.
Preferably, organic solvent can be the mixed solution of N,N-dimethylacetamide, DMF, N-Methyl pyrrolidone, methyl alcohol and tetrahydrofuran (THF).
Preferably, the solid content of Graphene/polyamic acid solution is 0.1 ~ 10wt%.
Preferably, rare gas element is nitrogen, argon gas or helium etc.
Second step; there is the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure: by Graphene/Kapton obtained above under the condition of vacuum or protection of inert gas; thermal treatment for some time under high temperature, obtain the Graphene/vitreous carbon laminated film of rigidity.
Preferably, rare gas element is nitrogen, argon gas or helium etc.
Preferably, high-temperature heat treatment temperature is 600 ~ 1800 DEG C; The high-temperature heat treatment time is 5 ~ 180min.
3rd step, the surface treatment of Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma for some time, carry out film surface process by certain density fluorine containing silane toluene solution subsequently thus realize its super-hydrophobicity, namely obtaining super-hydrophobic rigidity C film.
Preferably, plasma treatment time is 5 ~ 60s.
Preferably, fluorine containing silane is 1H, in 1H, 2H, 2H-perfluoro decyl trichlorosilane, ten difluoro heptyl propyl trimethoxy silicanes, ten trifluoro octyl group Trimethoxy silanes, 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane any one or its combination;
Preferably, the concentration of fluorine containing silane toluene solution is 1 ~ 20vol%.
Compared with prior art, the invention has the beneficial effects as follows: preparation method has abundant raw materials, method is simple, the advantage that can prepare on a large scale; The as easy as rolling off a log surface super hydrophobic process realizing C film, and this film has good mechanical property; Can design as required prepare there is ultra-hydrophobicity different thickness, size and dimension rigidity C film.
Accompanying drawing explanation
Fig. 1 is the overall flow schematic diagram of preparation method of the present invention;
Fig. 2 is the photo of Graphene/polyimide precursor film prepared by the embodiment of the present invention 1;
Fig. 3 is photo and the surface scan Electronic Speculum figure of Graphene/vitreous carbon laminated film prepared by the embodiment of the present invention 1;
Fig. 4 is the mechanical experimental results figure of Graphene/vitreous carbon laminated film prepared by the embodiment of the present invention 1;
Fig. 5 is the ultra-hydrophobicity schematic diagram after the Graphene/vitreous carbon laminated film surface treatment of the embodiment of the present invention 1 preparation.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
As shown in Figure 1, a kind of preparation method of super-hydrophobic rigidity C film comprises the following steps:
The preparation of 1, Graphene/polyimide precursor film: at room temperature, by graphene dispersion at 10mL N, in N-N,N-DIMETHYLACETAMIDE, concentration is 0.2mg/mL, ultrasonic disperse 1h, add a certain amount of 4, after 4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stir polyreaction and spend the night, obtain Graphene/polyamic acid solution, solid content is 0.5wt%.By Graphene/polyamic acid solution casting film-forming on the glass sheet, heat 1h respectively at 60 DEG C, 90 DEG C, 120 DEG C, 150 DEG C successively and remove after solvent, then heat 1h under the condition being placed in 350 DEG C of vacuum, obtain Graphene/polyimide precursor film.
2, there is the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure: by Graphene/Kapton obtained above under the condition of vacuum, thermal treatment 1h at 900 DEG C, obtain rigidity Graphene/vitreous carbon laminated film.The carbon nano rod array that film surface homoepitaxial is a large amount of.
The surface treatment of 3, Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma 15s, pass through 5vol%1H subsequently, 1H, 2H, 2H-perfluoro decyl trichlorosilane toluene solution carries out film surface process thus realizes its super-hydrophobicity, and contact angle is 155 degree.
Fig. 1 is the overall preparation flow figure of super-hydrophobic rigidity C film, and preparation method is simple; Fig. 2 is the digital photograph of the Graphene/polyimide precursor film obtained; Fig. 3 is digital photograph and the surface scan Electronic Speculum figure thereof of Graphene/vitreous carbon laminated film; Fig. 4 is the Mechanics Performance Testing of this Graphene/vitreous carbon laminated film, and three-point bending Modulus Strength is 203MPa, and modulus is 33.8GPa, illustrates that Graphene of the present invention/vitreous carbon laminated film has good mechanical property; Fig. 5 is the ultra-hydrophobicity after Graphene/vitreous carbon laminated film surface treatment, and contact angle test result.
Embodiment 2
The preparation of 1, Graphene/polyimide precursor film: at room temperature, by graphene dispersion at 10mL N, in dinethylformamide, concentration is 0.5mg/mL, ultrasonic disperse 1h, add a certain amount of 4, after 4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stir polyreaction and spend the night, obtain Graphene/polyamic acid solution, solid content is 1.3wt%.By Graphene/polyamic acid solution casting film-forming on the glass sheet, heat 1h respectively at 60 DEG C, 90 DEG C, 120 DEG C, 150 DEG C successively and remove after solvent, then heat 1h under the condition being placed in 300 DEG C of argon shields, obtain Graphene/polyimide precursor film.
2, there is the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure: by Graphene/Kapton obtained above under the condition of argon shield; thermal treatment 30min at 1200 DEG C, obtains rigidity Graphene/vitreous carbon laminated film that surface growth has a large amount of uniform carbon nanometer stick array.
The surface treatment of 3, Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma 5s, carried out film surface process by 10vol% ten difluoro heptyl propyl trimethoxy silicane toluene solution thus realized its super-hydrophobicity subsequently, contact angle is 158 degree.
Embodiment 3
The preparation of 1, Graphene/polyimide precursor film: at room temperature, by graphene dispersion in the mixed solution of 10mL methyl alcohol and tetrahydrofuran (THF), concentration is 3.3mg/mL, ultrasonic disperse 1h, after adding a certain amount of 4,4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stirring polyreaction is spent the night, and obtains Graphene/polyamic acid solution, and solid content is 7.5wt%.By Graphene/polyamic acid solution casting film-forming on the glass sheet, heat 1h respectively at 60 DEG C, 90 DEG C, 120 DEG C, 150 DEG C successively and remove after solvent, then heat 3h under the condition being placed in 350 DEG C of vacuum, obtain Graphene/polyimide precursor film.
2, there is the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure: by Graphene/Kapton obtained above under the condition of nitrogen protection; thermal treatment 1h at 1500 DEG C, obtains rigidity Graphene/vitreous carbon laminated film that surface growth has a large amount of uniform carbon nanometer stick array.
The surface treatment of 3, Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma 20s, carried out film surface process by 2vol% ten trifluoro octyl group Trimethoxy silane toluene solution thus realized its super-hydrophobicity subsequently, contact angle is 145 degree.
Embodiment 4
The preparation of 1, Graphene/polyimide precursor film: at room temperature, by graphene dispersion at 10mL N, in N-N,N-DIMETHYLACETAMIDE, concentration is 1mg/mL, ultrasonic disperse 1h, add a certain amount of 4, after 4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stir polyreaction and spend the night, obtain Graphene/polyamic acid solution, solid content is 1.5wt%.By Graphene/polyamic acid solution casting film-forming on the glass sheet, heat 1h respectively at 60 DEG C, 90 DEG C, 120 DEG C, 150 DEG C successively and remove after solvent, then heat 1h under the condition being placed in 350 DEG C of vacuum, obtain Graphene/polyimide precursor film.
2, there is the preparation of the Graphene/vitreous carbon laminated film of special micro-nano structure: under the condition protected at helium by Graphene/Kapton obtained above; thermal treatment 30min at 1800 DEG C, obtains Graphene/vitreous carbon laminated film that surface growth has the rigidity of a large amount of uniform carbon nanometer stick array.
The surface treatment of 3, Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma 45s, pass through 20vol%1H subsequently, 1H, 2H, 2H-perfluoro decyl trichlorosilane toluene solution carries out film surface process thus realizes its super-hydrophobicity, and contact angle is 152 degree.
Embodiment 5
The preparation of 1, Graphene/polyimide precursor film: at room temperature, by graphene dispersion in 10mL N-Methyl pyrrolidone, concentration is 5mg/mL, ultrasonic disperse 1h, after adding a certain amount of 4,4'-diphenyldiamine, add pyromellitic acid anhydride in batches, stirring polyreaction is spent the night, and solid content is 10.0wt%.By Graphene/polyamic acid solution casting film-forming on the glass sheet; after heating 1h removal solvent respectively at 60 DEG C, 90 DEG C, 120 DEG C, 150 DEG C successively; heat 2h under being placed in the condition of 300 DEG C of argon gas protections again, obtain Graphene/polyimide precursor film.
The preparation of 2, Graphene/vitreous carbon laminated film: by Graphene/Kapton obtained above under the condition of vacuum, thermal treatment 3h at 600 DEG C, obtains rigidity Graphene/vitreous carbon laminated film that surface growth has a large amount of uniform carbon nanometer stick array.
The surface treatment of 3, Graphene/vitreous carbon laminated film: first Graphene obtained above/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma 60s, carried out film surface process by 8vol%4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane toluene solution thus realized its super-hydrophobicity subsequently, contact angle is 148 degree.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. a preparation method for super-hydrophobic rigidity C film, is characterized in that, comprise the following steps:
The first step, the preparation of Graphene/polyimide precursor film: at room temperature, by graphene dispersion in organic solvent, ultrasonic disperse obtains Graphene dispersion in organic solvent; In described Graphene dispersion in organic solvent, add 4,4'-diphenyldiamine, then add pyromellitic acid anhydride in batches, stir polyreaction, obtain Graphene/polyamic acid solution; By described Graphene/polyamic acid solution casting film-forming on the glass sheet; after 50 ~ 180 DEG C of heating 1 ~ 24h remove described organic solvent; heat 1 ~ 24h under being placed in the condition of 180 ~ 350 DEG C of vacuum or protection of inert gas again, obtain described Graphene/polyimide precursor film.
Second step; the preparation of Graphene/vitreous carbon laminated film: by the thermal treatment under the condition of vacuum or protection of inert gas of described Graphene/polyimide precursor film, obtain described Graphene/vitreous carbon laminated film that surface growth has uniform carbon nanometer stick array.
3rd step, the surface treatment of Graphene/vitreous carbon laminated film: first described Graphene/vitreous carbon laminated film is carried out Cement Composite Treated by Plasma, carries out film surface process by fluorine containing silane toluene solution subsequently, thus obtain described super-hydrophobic rigidity C film.
2. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, is characterized in that, the concentration of the dispersion in organic solvent of Graphene described in the first step is 0.01 ~ 5mg/mL.
3. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, organic solvent described in the first step is the one among the mixed solution of N,N-dimethylacetamide, DMF, N-Methyl pyrrolidone, methyl alcohol and tetrahydrofuran (THF).
4. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, is characterized in that, the solid content of Graphene/polyamic acid solution described in the first step is 0.1 ~ 10wt%.
5. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, rare gas element described in the first step is nitrogen, argon gas or helium.
6. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, thermal treatment temp described in second step is 600 ~ 1800 DEG C.
7. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, heat treatment time described in second step is 5 ~ 180min.
8. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, described in the 3rd step, plasma treatment time is 5 ~ 60s.
9. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, described in 3rd step, fluorine containing silane is 1H, 1H, a kind of or multiple arbitrarily combination in 2H, 2H-perfluoro decyl trichlorosilane, ten difluoro heptyl propyl trimethoxy silicanes, ten trifluoro octyl group Trimethoxy silanes, 4-methyl-(perfluoro hexyl ethyl) propyl trimethoxy silicane.
10. the preparation method of a kind of super-hydrophobic rigidity C film according to claim 1, it is characterized in that, described in the 3rd step, the concentration of fluorine containing silane toluene solution is 1 ~ 20vol%.
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| CN106497056A (en) * | 2016-11-23 | 2017-03-15 | 常州碳润新材料科技有限公司 | A kind of easy to process, high temperature resistant and wear-resisting polyimides Graphene bearing and preparation method thereof |
| CN107237141A (en) * | 2017-05-08 | 2017-10-10 | 上海大学 | The preparation method that the hydrophobic polyimides that a kind of surface is modified is weaved cotton cloth |
| CN107501586A (en) * | 2017-08-22 | 2017-12-22 | 江苏大学 | A kind of preparation method and its usage of super-hydrophobic composite film material |
| CN108314033A (en) * | 2017-01-18 | 2018-07-24 | 北京化工大学 | A kind of graphitization film and its preparation method and application |
| CN108314032A (en) * | 2018-04-18 | 2018-07-24 | 哈尔滨工业大学 | It is a kind of that there is anti-icing and deicing function the graphene-based material of 3 D stereo reticular structure and preparation method thereof |
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| CN106497056A (en) * | 2016-11-23 | 2017-03-15 | 常州碳润新材料科技有限公司 | A kind of easy to process, high temperature resistant and wear-resisting polyimides Graphene bearing and preparation method thereof |
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| CN108314032A (en) * | 2018-04-18 | 2018-07-24 | 哈尔滨工业大学 | It is a kind of that there is anti-icing and deicing function the graphene-based material of 3 D stereo reticular structure and preparation method thereof |
| CN108996915A (en) * | 2018-08-27 | 2018-12-14 | 深圳南科新材科技有限公司 | A kind of hydrophobic composite, preparation method, purposes and the glass containing it |
| CN111673285A (en) * | 2020-06-30 | 2020-09-18 | 吉林大学 | Method for forming micro-nano multilayer structure on amorphous carbon surface through nanosecond laser irradiation induction |
| CN117126586A (en) * | 2023-10-26 | 2023-11-28 | 成都石大力盾科技有限公司 | Thread seizure preventing coating and preparation method thereof |
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Application publication date: 20150311 |