CN104313549A - Making method of graphene-based film with automatic cleaning function - Google Patents
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- CN104313549A CN104313549A CN201410472524.0A CN201410472524A CN104313549A CN 104313549 A CN104313549 A CN 104313549A CN 201410472524 A CN201410472524 A CN 201410472524A CN 104313549 A CN104313549 A CN 104313549A
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- graphene
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
Abstract
The invention relates to a making method of a graphene-based film with an automatic cleaning function. The method comprises the following steps: respectively preparing a graphene oxide dispersion and a titanium dioxide dispersion, blending the graphene oxide dispersion with the titanium dioxide dispersion to obtain a graphene oxide/titanium dioxide dispersion, and injecting the graphene oxide/titanium dioxide dispersion to a target substrate in order to obtain a graphene oxide-based film; and irradiating the graphene oxide-based film by ultraviolet light to reduce the graphene oxide-based film in order to obtain the graphene-based film with an automatic cleaning function. Compared with graphene-based films in the prior art, the graphene-based film prepared through making the graphene oxide-based film by injecting and utilizing ultraviolet irradiation has the advantages of certain conductivity and certain automatic cleaning function. The graphene-based film can be further applied in the fields of graphene-based conductive coatings and graphene-based surface strain sensors.
Description
Technical field
The present invention relates to a kind of preparation method of graphene-based film, especially relate to a kind of preparation method with the graphene-based film of self-cleaning function, belong to film material with function technical field.
Background technology
Graphene has good transmitance, and theoretical and experimental result shows, single-layer graphene absorbs the visible ray of 2.3%, and namely transmittance is 97.7%.Each carbon atom in Graphene is with sp
2mode (σ key) and other 3 carbon atoms of hybridized orbital are connected, and extremely strong C-C key causes graphene sheet layer to have excellent mechanical property.A remaining p electronic orbit, perpendicular to graphene planes, forms the π key of delocalization with the carbon atom of surrounding, causes electronics can move freely in crystal, imparts the electrical property that Graphene is good.Because interatomic reactive force is very strong, at normal temperatures, even if around carbon atom telescopes, the interference that the electronics in Graphene is subject to is also very little.Not easily scattering occurs when electronics transmits in Graphene, mobility can reach 2 × 10
5cm
2/ (Vs).Its surface resistance is about 31 Ω/sq, and specific conductivity can reach 10
6s/m is the material of room temperature conductivity the best.
The preparation method of Graphene is mainly divided into CVD, liquid phase physics stripping method, epitaxial growth method and oxidation reduction process.And oxidation reduction process is mainly manifested in following method compared to the advantage of other several method: (1) production cost is lower, (2) preparation technology is comparatively simple, and (3) preparation efficiency is higher.Therefore, oxidation reduction process prepares the important directions studied after Graphene will be.The method at present preparing graphene-based film based on oxidation reduction process mainly contains vacuum filtration method, spin-coating method, self-assembly, LangmuirBlodgett (LB) method, spraying method etc.By some reduction means in the process preparing film, as hydrazine hydrate reduction, HI acid reduction or thermal reduction etc. process graphene oxide film, the graphene-based film of final preparation.Graphene film is had, and following one or more are functional: (1) conducts electricity, and (2) are transparent, (3) sensing etc.
At present domestic and international based on oxidation reduction process in the process preparing graphene film, do not find that graphene film has certain self-cleaning function.
Summary of the invention
Object of the present invention be exactly provide to overcome defect that above-mentioned prior art exists a kind of simple, efficient, can the preparation method with the graphene-based film of self-cleaning function of engineering expanding production.
Object of the present invention can be achieved through the following technical solutions:
There is a preparation method for the graphene-based film of self-cleaning function, comprise the following steps:
(1) in water/ethanol or ethanolic soln, prepare graphene oxide dispersion, the concentration of graphene oxide is 0.1 ~ 2mg/ml, has prepared dispersed and the good graphene oxide dispersion of stability after sonic oscillation.
As optimal way, be added with enhancing electro-conductive material in described graphene oxide dispersion, graphene oxide is 1: 1 ~ 10: 1 with the weight ratio of enhancing electro-conductive material.Described enhancing electro-conductive material is carbon nanotube or metal nanometer line.
(2) Nano titanium dioxide is joined in ethanolic soln, after ultrasonic 1h, prepared the titanium oxide dispersion that concentration is 0.1 ~ 1mg/ml.
(3) by graphene oxide dispersion and titanium oxide dispersion blended after, suitably ultrasonic, obtain graphene oxide/titanium oxide dispersion, in described graphene oxide/titanium oxide dispersion, the weight ratio of graphene oxide and titanium dioxide is 1: 1 ~ 20: 1, is preferably 1: 1.
(4) get a certain amount of graphene oxide/titania solution dispersion liquid to join and be associated with in the spray gun of air pump, target base plate is sprayed, evenly prepares graphene oxide base film.
(5) irradiated under ultraviolet light by prepared film, fluorescent tube is 175W, and the distance of fluorescent tube and sample is 15cm, and irradiation time is 10h, reduces to film, obtains having the graphene-based film of self-cleaning function.
In the present invention, the Catalysis Principles of titanium dioxide is as follows: when a photon with hv energy size or have the photon being greater than semi-conductor energy gap Eg inject semi-conductor time, an electronics is energized into conduction band (CB) by valence band (VB), thus on conduction band, produces a high reactivity electronics (e
-), valence band leaves a hole (h+), forms redox system.Dissolved oxygen and power and water and hole interaction, final produce highly active hydroxyl.OH
-, O
2 -, OOH
-free radical has strong oxidizing property, great majority can be adsorbed on TiO
2the organic pollutant degradation on surface is CO
2, H
2o, is oxidized inorganic pollutant or is reduced to harmless object.Wherein the reduction principle of titanium dioxide to graphene oxide can be expressed as:
TiO2+hv→TiO2(h+e)→C2H5OH→TiO2(e)+·C2H4OH+H
+ (1)
TiO2(e)+graphene oxide(GO)→TiO2+graphene reduced(GR) (2)
Compared with prior art, the present invention has the following advantages:
(1) the present invention has prepared graphene oxide/titanium dioxide mixed solution, graphene oxide base film is prepared by spraying, utilizing UV-irradiation, while prepared graphene-based film has certain electroconductibility, also there is certain self-cleaning function.
(2) effect of titanium dioxide, show the reduction to graphene oxide on the one hand, showing on the other hand makes film self have certain self-cleaning function, and has the germ in surrounding environment and certain murder effect, and formaldehyde etc. have certain Degradation.
(3) the method is in the reduction process realizing film, and do not use as HI acid, the toxic substances such as hydrazine hydrate, but the titanium dioxide that have employed environmental protection, whole reduction process is safe and harmless.
(4) the method prepares graphene-based film based on spraying method, and reduction adopts UV-irradiation, suitably can amplify and carry out through engineering approaches application.
(5) the present invention efficiently, has simply prepared the graphene-based function film had from cleaning function, can be applied to graphene-based conductive coating and graphene-based surface strains sensor field further.
Accompanying drawing explanation
Fig. 1 is the TEM figure that graphene oxide/titanium deoxid film is prepared in spraying;
Fig. 2 is the TEM figure that graphene oxide/titanium deoxid film is prepared in spraying;
Fig. 3 is the TEM figure that graphene oxide/carbon nano-tube/titanic oxide film is prepared in spraying;
Fig. 4 is the TEM figure that graphene oxide/carbon nano-tube/titanic oxide film is prepared in spraying;
Fig. 5 is the SEM figure that graphene oxide/carbon nano-tube/titanic oxide film is prepared in spraying;
Fig. 6 is the SEM figure that graphene oxide/carbon nano-tube/titanic oxide film is prepared in spraying.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Take ethanol as solvent, the graphene oxide solution of preparation 0.2mg/ml, the titania solution of 0.5mg/ml.The two is carried out blended, makes the mass ratio of graphene oxide and titanium dioxide be 1: 1, ultrasonic 30min.Namely graphene oxide and titanium oxide dispersion is obtained.Get 6ml homogeneous solution to join in spray gun.PC substrate is cleaned, with post-drying, puts on warm table and be warmed up to 100 DEG C.Now utilize the spray gun being associated with air pump to be injected in by above-mentioned solution on the PC substrate that area is 5 × 5cm, jet length is about 5cm.Prepare graphene oxide film/titanium deoxid film (as shown in Figure 1 and Figure 2).Stood on by film and 200ml is housed, concentration is carry out degradation experiment in the methyl orange solution of 2mg/L.Wherein the power of ultraviolet lamp is 175W, and fluorescent tube is 15cm apart from the distance of sample, and irradiation time is 10h.Characterize the sample after irradiating 10h, experimental result shows that methyl orange solution has been degraded 12%.
Embodiment 2
Take ethanol as solvent, the graphene oxide solution of preparation 0.2mg/ml, adds carbon nanotube and makes the mass ratio of graphene oxide and carbon nanotube be 5: 1.Carry out ultrasonic 30min subsequently, prepare graphene oxide/carbon nanotube composite solution.Same is that the titania solution of 0.5mg/ml prepared by solvent with ethanolic soln.Undertaken blended by three, make graphene oxide, the mass ratio of carbon nanotube and titanium dioxide is 5: 1: 5, ultrasonic 10min.Namely graphene oxide/carbon nano-tube/titanic oxide dispersion liquid is obtained.Get 6ml homogeneous solution to join in spray gun.PC substrate is cleaned, with post-drying, puts on warm table and be warmed up to 100 DEG C.Now utilize the spray gun being associated with air pump to be injected in by above-mentioned solution on the PC substrate that area is 5 × 5cm, jet length is about 5cm.Prepare graphene oxide/carbon nano-tube/titanic oxide film (as shown in Fig. 3 ~ Fig. 6).Stood on by film and 200ml is housed, concentration is carry out degradation experiment in the methyl orange solution of 2mg/L.Wherein the power of ultraviolet lamp is 175W, and fluorescent tube is 15cm apart from the distance of sample, and irradiation time is 10h.Characterize the sample after irradiating 10h, experimental result shows that methyl orange solution has been degraded 18%.Degraded and carried out electrical performance testing to film afterwards, its square resistance is 100k Ω/sq.
Embodiment 3
There is the preparation method of the graphene-based film of self-cleaning function, comprise the following steps:
(1) in water/ethanol or ethanolic soln, prepare graphene oxide dispersion, the concentration of graphene oxide is 0.1mg/ml, has prepared dispersed and the good graphene oxide dispersion of stability after sonic oscillation.
As optimal way, be added with enhancing electro-conductive material in graphene oxide dispersion, graphene oxide is 1: 1 with the weight ratio of enhancing electro-conductive material.Strengthening electro-conductive material is carbon nanotube or metal nanometer line.
(2) Nano titanium dioxide is joined in ethanolic soln, after ultrasonic 1h, prepared the titanium oxide dispersion that concentration is 0.1mg/ml.
(3) by graphene oxide dispersion and titanium oxide dispersion blended after, suitably ultrasonic, obtain graphene oxide/titanium oxide dispersion, in graphene oxide/titanium oxide dispersion, the weight ratio of graphene oxide and titanium dioxide is 1: 1.
(4) get a certain amount of graphene oxide/titania solution dispersion liquid to join and be associated with in the spray gun of air pump, target base plate is sprayed, and jet length is about 5cm, evenly prepares graphene oxide base film.
(5) irradiated under ultraviolet light by prepared film, fluorescent tube is 175W, and the distance of fluorescent tube and sample is 15cm, and irradiation time is 10h, reduces to film, obtains having the graphene-based film of self-cleaning function.
Embodiment 4
There is the preparation method of the graphene-based film of self-cleaning function, comprise the following steps:
(1) in water/ethanol or ethanolic soln, prepare graphene oxide dispersion, the concentration of graphene oxide is 2mg/ml, has prepared dispersed and the good graphene oxide dispersion of stability after sonic oscillation.
As optimal way, be added with enhancing electro-conductive material in graphene oxide dispersion, graphene oxide is 5: 1 with the weight ratio of enhancing electro-conductive material.Strengthening electro-conductive material is carbon nanotube or metal nanometer line.
(2) Nano titanium dioxide is joined in ethanolic soln, after ultrasonic 1h, prepared the titanium oxide dispersion that concentration is 1mg/ml.
(3) by graphene oxide dispersion and titanium oxide dispersion blended after, suitably ultrasonic, obtain graphene oxide/titanium oxide dispersion, in graphene oxide/titanium oxide dispersion, the weight ratio of graphene oxide and titanium dioxide is 10: 1.
(4) get a certain amount of graphene oxide/titania solution dispersion liquid to join and be associated with in the spray gun of air pump, target base plate is sprayed, evenly prepares graphene oxide base film.
(5) irradiated under ultraviolet light by prepared film, fluorescent tube is 175W, and the distance of fluorescent tube and sample is 15cm, and irradiation time is 10h, reduces to film, obtains having the graphene-based film of self-cleaning function.
Embodiment 5
There is the preparation method of the graphene-based film of self-cleaning function, comprise the following steps:
(1) in water/ethanol or ethanolic soln, prepare graphene oxide dispersion, the concentration of graphene oxide is 1mg/ml, has prepared dispersed and the good graphene oxide dispersion of stability after sonic oscillation.
As optimal way, be added with enhancing electro-conductive material in graphene oxide dispersion, graphene oxide is 10: 1 with the weight ratio of enhancing electro-conductive material.Strengthening electro-conductive material is carbon nanotube or metal nanometer line.
(2) Nano titanium dioxide is joined in ethanolic soln, after ultrasonic 1h, prepared the titanium oxide dispersion that concentration is 0.5mg/ml.
(3) by graphene oxide dispersion and titanium oxide dispersion blended after, suitably ultrasonic, obtain graphene oxide/titanium oxide dispersion, in graphene oxide/titanium oxide dispersion, the weight ratio of graphene oxide and titanium dioxide is 20: 1.
(4) get a certain amount of graphene oxide/titania solution dispersion liquid to join and be associated with in the spray gun of air pump, target base plate is sprayed, evenly prepares graphene oxide base film.
(5) irradiated under ultraviolet light by prepared film, fluorescent tube is 175W, and the distance of fluorescent tube and sample is 15cm, and irradiation time is 10h, reduces to film, obtains having the graphene-based film of self-cleaning function.
Above-mentioned is can understand and use invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to above-described embodiment, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (8)
1. one kind has the preparation method of the graphene-based film of self-cleaning function, it is characterized in that, prepare graphene oxide dispersion and titanium oxide dispersion respectively, and by graphene oxide dispersion and titanium oxide dispersion blended after obtain graphene oxide/titanium oxide dispersion, graphene oxide/titanium oxide dispersion is ejected in target base plate, obtains graphene oxide base film; UV-irradiation graphene oxide base film, to its reduction, obtains having the graphene-based film of self-cleaning function.
2. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 1, is characterized in that, be added with enhancing electro-conductive material in described graphene oxide dispersion.
3. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 2, is characterized in that, in described graphene oxide dispersion, graphene oxide is 1: 1 ~ 10: 1 with the weight ratio of enhancing electro-conductive material.
4. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 2, is characterized in that, described enhancing electro-conductive material is carbon nanotube or metal nanometer line.
5. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 1, is characterized in that, in described graphene oxide dispersion, the concentration of graphene oxide is 0.1 ~ 2mg/ml.
6. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 1, is characterized in that, in described titanium oxide dispersion, the concentration of titanium dioxide is 0.1 ~ 1mg/ml.
7. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 1, is characterized in that, in described graphene oxide/titanium oxide dispersion, the weight ratio of graphene oxide and titanium dioxide is 1: 1 ~ 20: 1.
8. a kind of preparation method with the graphene-based film of self-cleaning function according to claim 1, is characterized in that, preparing titanium dioxide dispersion liquid titanium dioxide used is Nano titanium dioxide.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877572A (en) * | 2015-04-20 | 2015-09-02 | 青岛瑞利特新材料科技有限公司 | Graphene additive and application thereof in shoe cream |
| CN106153621A (en) * | 2015-03-16 | 2016-11-23 | 北京中清国研环境技术研究院 | A kind of water quality monitoring automatically cleaning film sensors |
| CN107293765A (en) * | 2017-07-28 | 2017-10-24 | 韦德永 | A kind of fuel battery gas diffusion layer structure |
| CN107537320A (en) * | 2017-08-25 | 2018-01-05 | 杭州高瓴环境科技有限公司 | A kind of composite membrane and preparation method thereof |
| CN108043379A (en) * | 2017-12-11 | 2018-05-18 | 河南师范大学 | Graphene/TiO2Composite and flexible photocatalysis membrana and preparation method thereof |
| CN108722206A (en) * | 2018-07-04 | 2018-11-02 | 同济大学 | A kind of antipollution self-cleaning type GO/ZnO-PVDF films and preparation method thereof |
| CN108754460A (en) * | 2018-05-18 | 2018-11-06 | 蚌埠心里程电子科技有限公司 | A kind of Metal surface anti-corrosion automatically cleaning processing method |
| CN109423068A (en) * | 2017-06-23 | 2019-03-05 | 北京国信优控***技术有限公司 | Super-hydrophobic wear-resisting graphene composite coating and the solar energy heat collection pipe for applying it |
| CN113694915A (en) * | 2021-08-25 | 2021-11-26 | 特灵空调***(中国)有限公司 | Preparation method of titanium dioxide/graphene composite material |
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| CN106153621A (en) * | 2015-03-16 | 2016-11-23 | 北京中清国研环境技术研究院 | A kind of water quality monitoring automatically cleaning film sensors |
| CN104877572A (en) * | 2015-04-20 | 2015-09-02 | 青岛瑞利特新材料科技有限公司 | Graphene additive and application thereof in shoe cream |
| CN109423068A (en) * | 2017-06-23 | 2019-03-05 | 北京国信优控***技术有限公司 | Super-hydrophobic wear-resisting graphene composite coating and the solar energy heat collection pipe for applying it |
| CN107293765A (en) * | 2017-07-28 | 2017-10-24 | 韦德永 | A kind of fuel battery gas diffusion layer structure |
| CN107537320A (en) * | 2017-08-25 | 2018-01-05 | 杭州高瓴环境科技有限公司 | A kind of composite membrane and preparation method thereof |
| CN108043379A (en) * | 2017-12-11 | 2018-05-18 | 河南师范大学 | Graphene/TiO2Composite and flexible photocatalysis membrana and preparation method thereof |
| CN108754460A (en) * | 2018-05-18 | 2018-11-06 | 蚌埠心里程电子科技有限公司 | A kind of Metal surface anti-corrosion automatically cleaning processing method |
| CN108722206A (en) * | 2018-07-04 | 2018-11-02 | 同济大学 | A kind of antipollution self-cleaning type GO/ZnO-PVDF films and preparation method thereof |
| CN108722206B (en) * | 2018-07-04 | 2020-10-30 | 同济大学 | Anti-pollution self-cleaning GO/ZnO-PVDF film and preparation method thereof |
| CN113694915A (en) * | 2021-08-25 | 2021-11-26 | 特灵空调***(中国)有限公司 | Preparation method of titanium dioxide/graphene composite material |
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