CN102173597A - Preparation method of light-induced hydrophobic film - Google Patents
Preparation method of light-induced hydrophobic film Download PDFInfo
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- CN102173597A CN102173597A CN 201110048053 CN201110048053A CN102173597A CN 102173597 A CN102173597 A CN 102173597A CN 201110048053 CN201110048053 CN 201110048053 CN 201110048053 A CN201110048053 A CN 201110048053A CN 102173597 A CN102173597 A CN 102173597A
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Abstract
The invention belongs to the technical field of thin-film materials, in particular relates to a preparation method of a light-induced hydrophobic film. The method comprises the following steps of: preparing graphite oxide from graphite powders which are used as raw materials by the Hummers oxidation method; then preparing a colloidal solution of graphene oxide (GO) by ultrasonic dispersion and controlling the concentration of the GO colloidal solution within the range from 1 mg/mL to 10 mg/mL; subsequently preparing a GO film on the surface of a solid matter by film coating by using a drawing machine or homogenizing machine; and finally exposing to ultraviolet irradiation for 0.5 to 5 hours to obtain the hydrophobic film. The reduction of GO by ultraviolet irradiation can eliminate oxygen-containing groups of GO, so as to control the number of oxygen-containing groups on the surface of GO and further to control the surface hydrophilicity of the GO-modified solid matter.
Description
Technical field
The invention belongs to the thin-film material technical field, be specifically related to a kind of preparation method of the photic hydrophobic film relevant with graphene oxide.
Background technology
The wetting property of solid surface is relevant with many scientific domains, along with people to the improving constantly of material performance requirement, make investigation of materials become new in recent years focus with hydrophobic performance.Super hydrophobic material in many fields such as national defence, industrial and agricultural production and daily life such as snow defence, anti-oxidant, from clean, microfluid injection, prevent that conduction of current, aspect such as anti-pollution, anticorrosion from having wide practical use and receive much concern [].
Studies show that, wettability of the surface is relevant with the chemical property and the surface tissue of surface mass, the wetting property of material surface is the hydrophilic and hydrophobic prerequisite of decision, and improving surface microstructure and control surface composition is key and the Basic Ways [] that improves its hydrophobic performance.In general, the super-hydrophobicity interface can be constructed by following two kinds of methods, a kind of is to make up coarse structure at solid surface, and method therefor has sol-gel method, hydrothermal method, plasma etching, anonizing, phase separation method, template, electrochemical deposition method, crystallization control method etc.Another kind method is to modify low surface energy substance change surface composition on solid surface, and low surface energy material commonly used has fluorinated alkyl silane, fluoropolymer, wax etc.
(Graphene Oxide is the presoma of preparation Graphene GO) to graphene oxide, is the stratified material that obtains by graphite oxide.Body phase graphite is after the concentrated acid solution-treated of being fuming, graphene layer is oxidized to hydrophilic graphene oxide, graphite layers is apart from being increased to 7 ~ 10 by 3.35 before the oxidation, through heating or in water ultrasonic stripping process be easy to form isolating graphene oxide laminated structure [].Characterization results such as XPS, infrared spectra, solid-state nuclear magnetic resonance spectrum show that graphene oxide contains a large amount of oxygen-containing functional groups, comprise [3] such as hydroxyl, epoxy-functional, carbonyl, carboxyls.Hydroxyl and epoxy-functional mainly are positioned on the basal plane of graphite, and carbonyl and carboxyl then are in the edge of Graphene, because there is a large amount of oxygen-containing functional groups in the graphene oxide surface, thus the wetting ability of showing as, Graphene then is a hydrophobicity [].
The present invention utilizes UV-light can eliminate the effect of the oxy radical of GO to the reduction of GO dexterously, thereby controls the quantity of GO surface oxy radical, and then control is modified with the wetting ability of the solid surface of GO.
Summary of the invention
The objective of the invention is to propose the method for simple, the easy to operate photic hydrophobic film of preparation of a kind of technology.
The method of the photic hydrophobic film of preparation that the present invention proposes, used main raw material is a Graphite Powder 99, equipment has the conventional equipment that utilizes the colloidal sol thin films, as pulling machine or sol evenning machine.Utilize Graphite Powder 99 to adopt the Hummers oxidation style to prepare graphite oxide [] earlier, ultra-sonic dispersion obtains the colloidal solution of graphene oxide, the concentration 1-10mg/ml of GO colloidal solution; The method of utilizing pulling machine or sol evenning machine to get rid of film then prepares the GO film at glass or other solid surface, and by ultraviolet (UV) photo-irradiation treatment, light application time is 0.5-5 hour, promptly obtains hydrophobic film.
Experiment shows, can control preparation method simple (Fig. 1) by light application time by the hydrophobicity of the film of the inventive method preparation.The photoelectric current test result shows that considerable change takes place the GO film that is prepared by the present invention behind ultraviolet lighting, the GO film can be applied aspect the infiltrating control of solid.
1. under UV-irradiation, the GO film for preparing with the present invention shows tangible photic hydrophobicity.Is 28 ° at the GO of slide surface film to the contact angle of water.At 254nm, 0.2 mW.cm
-2UV-light under the irradiation 1 hour after, the GO film that obtains rises to 42 ° to the contact angle of water, as shown in Figure 2.
2. be 24 ° with spin coating method at the contact angle to water of the GO film of conductive glass surface preparation.At 254nm, 0.2 mW.cm
-2UV-light under the irradiation 3 hours after, the GO film that obtains becomes 57 ° to the contact angle of water, as shown in Figure 3.The GO film can be applied aspect the light guide of solid hydrophilic.
3. through after the UV-irradiation, GO film generation obvious variation, the transparency descends, and transmittance reduces, and as shown in Figure 4, the photoelectric current of corresponding membrane electrode reduces, as shown in Figure 5.Show that illumination produces material impact to the GO film.
4. the infrared spectra (Fig. 6) of the GO before and after the mensuration treatment with ultraviolet light, through after the treatment with ultraviolet light, the oh group of GO reduces.
The present invention utilizes UV-light can eliminate the effect of the oxy radical of GO to the reduction of GO, thereby controls the quantity of GO surface oxy radical, and then control is modified with the wetting ability of the solid surface of GO.
Description of drawings
Fig. 1 is the preparation flow synoptic diagram of photic hydrophobic film, at first prepares hydrophilic GO film, and optical processing then obtains hydrophobic reductive graphene oxide (r-GO) film.
Fig. 2 is that GO film light on glass is according to the hydrophilic variation in front and back.Wherein, (a) be the wetting ability microgram before the illumination, contact angle is 28o; (b) be wetting ability microgram behind the 254 nm UV illumination 1h, contact angle is 42o.
Fig. 3 is that the GO film light shines the hydrophilic variation in front and back on the conductive glass.Wherein, (a) be the wetting ability microgram before the illumination, contact angle is 24o; (b) be wetting ability microgram behind the 254 nm UV illumination 3h, contact angle is 57o.
Fig. 4 is film UV-VIS transmitted spectrum of (r-GO) after (GO) and the illumination before illumination.
Fig. 5 is the variation of the photoelectric current of GO film with light application time.Wherein, (a) light application time: 0 h, (b) light application time: 0.5 h, (c) light application time: 5 h.
Fig. 6 is film infrared spectra of (r-GO) after (GO) and the illumination before illumination.
Embodiment
Embodiment 1: with commercially available Graphite Powder 99 is starting material, by the Hummers oxidation style
[](graphene oxide GO), takes by weighing the prepared GO of 0.1 g then, is dissolved in the 20 mL deionized waters, and ultrasonic to obtain brown colloidal solution standby to make graphene oxide.
Adopt sol evenning machine to get rid of membrane prepare and prepare the GO film in slide surface in glass sheet surface, dry under the room temperature.UV-vis test shows, GO film are transparent.Test its wetting property to water and show, the GO film is 28 ° to the contact angle of water, and film is placed on (253.7nm, 0.2 mW.cm under the ultraviolet lamp
-2) illumination is after 1 hour, test finds that the GO film is 42 ° to the contact angle of water, demonstrates photic hydrophobicity (Fig. 2).
Embodiment 2: with commercially available Graphite Powder 99 is starting material, by the Hummers oxidation style
[6](graphene oxide GO), takes by weighing the prepared GO of 0.2 g then, is dissolved in the 20mL deionized water, and ultrasonic to obtain brown colloidal solution standby to make graphene oxide.
Adopt sol evenning machine to get rid of membrane prepare GO film at conductive glass surface, dry under the room temperature.UV-VIS test shows, GO film are transparent, and transmittance can reach 80%.Test its wetting property to water and show, the GO film is 24o to the contact angle of water, and film is placed on (253.7nm, 0.2 mW.cm under the ultraviolet lamp
-2) after the illumination, the transparency of GO film descends, transmittance is about 65%(Fig. 3), the GO film increases the contact angle of water and is 57o simultaneously, demonstrates photic hydrophobicity.
Embodiment 3: with commercially available Graphite Powder 99 is starting material, and (graphene oxide GO), takes by weighing the prepared GO of 0.2 g then, and being dissolved in 20 mL deionized water for ultrasonic, to obtain brown aaerosol solution standby to make graphene oxide by the Hummers oxidation style.
Adopt sol evenning machine to get rid of membrane prepare ITO/GO film at conductive glass surface, dry under the room temperature.The ITO/GO film is placed on (253.7nm, 0.2 mW.cm under the ultraviolet lamp
-2) after the illumination, test finds that the GO film increases the contact angle of water, demonstrates photic hydrophobicity.
The GO film of illumination different time is made into electrode, with silver conductive adhesive copper cash and conducting surface are sticked together, after the drying, then with exposed copper cash and elargol and the unnecessary conducting surface of monocomponent room-temperature cured silicon rubber encapsulation, and the area of steady job electrode is 0.25cm
2, dry in air at room temperature and to obtain the ITO/GO membrane electrode.
With the ITO/GO membrane electrode as working electrode, counter electrode metal Pt sheet, reference electrode is a saturated calomel electrode.Electrode is fixed in the homemade electrolyzer that has quartz window, measure the current curve of different membrane electrodes under the ultraviolet-visible rayed, at the cathode photo current that ultraviolet-visible illumination moment membrane electrode produces, be 0.62 μ A.cm for GO electrode photoelectric fluxion value
-2(Fig. 5 (a)).The electrode that ITO/GO film behind the ultraviolet lighting 0.5h is made produces cathode photo current and is reduced to 0.19 μ A.cm
-2(Fig. 5 (b)).With GO film ultraviolet irradiation 5 hours, photoelectric current was reduced to 0.02 μ A.cm
-2, photoelectric current almost disappears (Fig. 5 (c)), also shows that from another angle explanation variation has taken place the GO film.
Reference
[[1]]?Nakajima?A,?Hashimoto?K,?Watanabe?T?
et?al.?
Langmuir,?2000,?16(17):?7044
[2]?Feng?L,?Li?S?H,?Li?Y?S?
et?al.?
Adv?Mater,?2002,?14:?1857
[3]?Jeong?H?K,?Lee?Y?P,?Lahaye?R,?et?al.?Evidence?of?graphitic?AB?stacking?order?of?graphite?oxides.?J?Am?Chem?Soc,?2008,?130:?1362—1366
[4]?Shiren?Wang,?Yue?Zhang,?Noureddine?Abidi,?and?Luis?Cabrales,?Wettability?and?Surface?Free?Energy?of?Graphene?Films,?Langmuir?2009,?25(18),?11078–11081
[5]Xiao-Yan?Zhang,?Hao-Peng?Li,?Xiao-Li?Cui?and?Yuehe?Lin,?Graphene/TiO
2?Nanocomposites:?Synthesis,?Characterization?and?Application?in?Hydrogen?Evolution?from?Water?Photocatalytic?Splitting,?J.?Mater.?Chem.,?2010,?20,?2801–2806
[6]?Hummers?W?S,?Offeman?R?E.?
J.?Am.?Chem.?Soc.,?1958,?80:?1339~1339。
Claims (1)
1. the preparation method of a photic hydrophobic film is characterized in that concrete steps are as follows: be raw material with the Graphite Powder 99, adopt the Hummers oxidation style to prepare graphite oxide; Then, obtain the colloidal solution of graphene oxide by ultra-sonic dispersion, the concentration of control graphene oxide colloidal solution is 1-10mg/ml; Utilize pulling machine or sol evenning machine to get rid of the method for film then at solids surface preparation graphene oxide film; At last, handle with UV-irradiation, light application time is 0.5-5 hour, promptly obtains hydrophobic film.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515560A (en) * | 2011-12-13 | 2012-06-27 | 江苏大学 | Method for preparing graphene/Ag composite conductive film |
| CN102730671A (en) * | 2012-06-14 | 2012-10-17 | 天津大学 | Copper-graphene composite material and method for preparation of graphene film on copper-based metal surface |
| CN103779081A (en) * | 2012-10-23 | 2014-05-07 | 海洋王照明科技股份有限公司 | Graphene/graphene oxide thin film and preparation method thereof, and usage |
| CN110201556A (en) * | 2019-05-21 | 2019-09-06 | 西南石油大学 | A kind of graphene oxide nanofiltration membrane, preparation method and applications slightly restored |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
| CN111653689A (en) * | 2020-06-15 | 2020-09-11 | 京东方科技集团股份有限公司 | Preparation method of lens array, display device and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101474897A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
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Patent Citations (2)
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| CN101474897A (en) * | 2009-01-16 | 2009-07-08 | 南开大学 | Grapheme-organic material layered assembling film and preparation method thereof |
| CN101941694A (en) * | 2010-09-07 | 2011-01-12 | 湘潭大学 | Preparation method of high-dispersivity graphene |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515560A (en) * | 2011-12-13 | 2012-06-27 | 江苏大学 | Method for preparing graphene/Ag composite conductive film |
| CN102730671A (en) * | 2012-06-14 | 2012-10-17 | 天津大学 | Copper-graphene composite material and method for preparation of graphene film on copper-based metal surface |
| CN102730671B (en) * | 2012-06-14 | 2014-02-05 | 天津大学 | Copper-graphene composite material and method for preparation of graphene film on copper-based metal surface |
| CN103779081A (en) * | 2012-10-23 | 2014-05-07 | 海洋王照明科技股份有限公司 | Graphene/graphene oxide thin film and preparation method thereof, and usage |
| CN110201556A (en) * | 2019-05-21 | 2019-09-06 | 西南石油大学 | A kind of graphene oxide nanofiltration membrane, preparation method and applications slightly restored |
| CN110201556B (en) * | 2019-05-21 | 2022-01-21 | 西南石油大学 | Slightly-reduced graphene oxide nanofiltration membrane, and preparation method and application thereof |
| CN110420567A (en) * | 2019-07-12 | 2019-11-08 | 中国工程物理研究院材料研究所 | A kind of preparation method of graphene hydrophobic membrane and the application method of membrane distillation |
| CN110420567B (en) * | 2019-07-12 | 2022-04-22 | 中国工程物理研究院材料研究所 | Preparation method of graphene hydrophobic membrane and application method of membrane distillation |
| CN111653689A (en) * | 2020-06-15 | 2020-09-11 | 京东方科技集团股份有限公司 | Preparation method of lens array, display device and preparation method thereof |
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Application publication date: 20110907 |