CN101734654A - Transparent graphene oxide film and method for regulating transmittance - Google Patents
Transparent graphene oxide film and method for regulating transmittance Download PDFInfo
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- CN101734654A CN101734654A CN200910312043A CN200910312043A CN101734654A CN 101734654 A CN101734654 A CN 101734654A CN 200910312043 A CN200910312043 A CN 200910312043A CN 200910312043 A CN200910312043 A CN 200910312043A CN 101734654 A CN101734654 A CN 101734654A
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Abstract
The invention relates to a transparent graphene oxide film and a method for regulating transmittance. The method comprises the following steps: using waste liquid or common graphene oxide solution in the graphite oxide preparation process as a raw material, obtaining graphene oxide solution with different transmittances through addition of appropriate amount of acid or alkali with appropriate concentration to regulate the pH value of the solution; and preparing the graphene oxide solution into graphene oxide films with different transmittances, wherein the thickness of the graphene oxide film is between 0.01 and 100 mu m. The method for regulating the optical property of the transparent graphene oxide film comprises that: the graphene oxide film can be prepared when the pH value of the solution is between 1 and 13; with the increase of the pH value of stock solution, the transmittance of the prepared graphene oxide film is reduced; and when the pH value is smaller, the transmittance of the prepared film is relatively high and the transmissivity on near infrared reaches over 80 percent. The method for regulating the optical property of the graphene oxide film has the characteristics that the method is simple and easy to implement, can better regulate the transmittance of the graphene oxide film, and the like.
Description
Technical field
The present invention relates to a kind of transparent graphene oxide film and method for regulating transmittance, belong to the preparation and the optical property control technique of special film.
Background technology
Graphene is that the carbon atom number of plies is less than 10 layers graphite, is the elementary cell that constitutes soccerballene, carbon nanotube and graphite, and Graphene has a lot of peculiar character.Graphene is a kind of material that does not have energy gap, shows metallicity; In the Graphene of individual layer, each carbon atom all has the not electronics of Cheng Jian, therefore has extraordinary electroconductibility; Hole and electronics in the Graphene are separated from each other, and have caused the generation of new electronic conduction phenomenon, for example irregular quantum hall effect.Graphene has boundless application prospect, its peculiar character provides good Physical Experiment platform, still make the best materials of nano electron device-high-frequency transistor and single-electronic transistor, very wide application prospect is also being arranged aspect micro-filter screen and the superconduction.Existing preparation method of graphene has mechanically peel method, heating SiC and graphite oxide to peel off reduction method.The amount of the Graphene that the mechanically peel method obtains is fewer, and is difficult to isolate pure individual layer or which floor Graphene; Heating SiC method can be controlled the number of plies of the Graphene that obtains by the control Heating temperature, but can not mass production, and the condition harshness; Graphite oxide is peeled off the reduction rule and is had many advantages, can realize a large amount of production, and the number of plies of the product that obtains comparison homogeneous, and the cost of raw material is also lower.From graphite prepare graphite oxide (GraphiteOxide, GO) be considered to extensive synthesizing graphite alkene strategic starting point [Yang Yonggang, Chen Chengmeng, Wen Yuefang etc. novel charcoal material .2008,23 (3)].Yet prepare the process of graphite oxide from graphite, water washing process after oxidizing reaction finishes will make a certain amount of graphite oxide be dissolved in the water and form the graphite oxide aqueous solution, and in the operating process in the past, be as waste liquid with these aqueous solution, suitably utilization, thus the invisible waste of raw material caused.And the present invention can be a raw material with common graphene oxide solution (aqueous solution that the supersound process graphite oxide obtains) both, also can prepare " waste liquid " that form in the graphite oxide process with graphite (in fact also to be
A kind of graphite oxide aqueous solution) is the graphene oxide film of the different light transmissions of feedstock production.
The preparation method of existing graphene oxide film and graphene film mainly contains filter method [Dikin D A, StankovichS, Zimney E J, et al.Nature 2007,448,457.], molecular template method [Wei Z, Barlow D E, Sheehan P E.Nano Lett.2008,8,3141.], LB film [Li X, Zhang G, Bai X, etal.Nat.Nanotech.2008,3,538.], chemical gaseous phase depositing process [Kim K S, Zhao Y, Jang H, etal.Nature 2009,457,706.], matrix coating method [Becerril H A, Mao J, Liu Z, et al.ACS Nano 2008,2,463.] and liquid-gas interface self-assembly method [Chen C M, Yang Q H, Yang Y G, et al.Adv.Mater.2009,21,3007-3011].Obtain graphene oxide film by general filter method, do not have light transmission, and could separate with matrix after thickness acquires a certain degree, can obtain not having matrix, graphene oxide that well-formed's character is good and graphene film by the liquid-gas interface self-assembling method.Therefore, the present invention by the pH value of regulation and control solution, regulates and control the light transmission of graphene oxide film on the preparation method's of graphene oxide film commonly used basis, and what obtain having different optical character has matrix or do not have the graphene oxide film of matrix.
Summary of the invention
The object of the present invention is to provide a kind of transparent graphene oxide film and method for regulating transmittance thereof.In the present invention, with waste liquid and common graphene oxide solution in the preparation graphite oxide process is stoste, the acid by adding an amount of proper concn or the pH value of alkali regulator solution, obtain having the graphene oxide solution of different light transmissions, adopt filter method, LB film, matrix coating method, solid-liquid interface to become embrane method or liquid-gas interface self-assembly method to prepare graphene oxide film with different light transmissions.
Transparent graphene oxide film of the present invention, along with the continuous increase of mother liquor pH value, the transparency of preparation-obtained graphene oxide film reduces gradually; Thickness is 0.01-100 μ m.
The method for regulating transmittance of transparent graphene oxide film of the present invention, step is as follows:
(1) mother liquor is the scrub raffinate in the preparation graphite oxide process, or with graphite oxide and solvent with 1～30: 1mg/mL puts into beaker, ultrasonic 0.5～10h, power is 20～300W, the graphene oxide solution that obtains;
(2) add acid or alkali, it is 1 ~ 13 graphene oxide solution that mother liquor is adjusted to the pH value;
(3) mother liquor with different pH values moves in the 5-98 ℃ of water-bath, keeps 5min-3h, and graphene oxide forms the different graphene oxide film of transparency in the self-assembly of gas-liquid face, and film is pulled out, and drying obtains the different graphene oxide film of transparency under the normal temperature.
Described solvent comprises water, dehydrated alcohol, acetone, ether or N, dinethylformamide.
Described transparent graphene oxide film and optical property regulate and control method are: the pH value of solution value can both be prepared graphene oxide film between 1-13 the time; Along with the pH value of stoste increases, the transparency of the graphene oxide film that makes reduces, and pH value, reaches more than 80% the transmitance of near infrared light than higher than the transparence of the film that hour makes.
It is simple that the regulate and control method of the optical property of graphene oxide film provided by the invention has method, is easy to realize, can be preferably the light transmission of graphene oxide film such as be regulated at characteristics.
Described transparent graphene oxide film, be meant and utilize certain method for manufacturing thin film, utilization has the waste liquid in the graphite oxide preparation process of different pH values or the graphene oxide film of graphene oxide formulations prepared from solutions, and its light transmission can utilize the pH value of solution to regulate and control between 1%-95%.
1. in certain density graphene oxide solution, add acid, the light transmission of graphene oxide solution is increased;
2. in certain density graphene oxide solution, add alkali, the light transmission of graphene oxide solution is reduced;
3. add a certain amount of acid or alkali in certain density graphene oxide solution, the pH value of regulator solution realizes the control to graphene oxide solution light transmission;
4. adopt graphene oxide solution, can prepare graphene oxide film, realize regulation and control the graphene oxide film optical property with different light transmissions by certain film with different light transmissions.
Described graphite oxide is to be raw material with graphite, by Brodie method, Hummers method, Staudemaier method and other graphite oxide preparation method commonly used preparations.
Waste liquid in the described preparation graphite oxide process is in the graphite oxide preparation, the washings that washing process obtains.
Described solvent is water, dehydrated alcohol, acetone, ether, N, all organic-inorganic solvents that can dissolved oxygen graphite such as dinethylformamide.
Described film comprises that filter method, LB film, matrix coating method, solid-liquid interface become commonly used matrix being arranged or do not have the matrix film such as embrane method or liquid-gas interface self-assembly method.
Described acid, all can regulate the inorganic or organic acid of graphene oxide pH value of solution value for hydrochloric acid, sulfuric acid, citric acid etc.
Described alkali is potassium hydroxide, Lithamide, and all can regulate the inorganic or organic bases of graphene oxide pH value of solution value quaternary ammonium hydroxide etc.
That the control method of this graphene oxide film transparency has is simple to operate, be easy to realize and advantages such as control.
Description of drawings
Fig. 1: the graphene oxide solution (a) that example 1 of the present invention makes and the photo of graphene oxide film (b),
Fig. 2: the graphene oxide solution (a) that example 2 of the present invention makes and the photo of graphene oxide film (b),
Fig. 3: the graphene oxide solution (a) that example 3 of the present invention makes and the photo of graphene oxide film (b),
Fig. 4: the graphene oxide solution (a) that example 4 of the present invention makes and the photo of graphene oxide film (b),
Fig. 5: the graphene oxide solution (a) that example 4 of the present invention makes and the photo of graphene oxide film (b),
Fig. 6: the graphene oxide film that example 1 of the present invention makes is at the extinction figure of full wavelength period.
Embodiment
Embodiment 1
Measure " waste liquid " 80ml that the Hummers legal system obtains in the water washing process when being equipped with graphite oxide, by adding an amount of H
2SO
4, obtain the graphite oxide aqueous solution (shown in Fig. 1 (a)) of pH=1.00.Then this graphite oxide aqueous solution is moved in 80 ℃ of water-baths, keep 45min, can form layer of even graphene oxide film at liquid level, graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature, obtaining unsupported thickness is the graphene oxide film (shown in Fig. 1 (b)) of 0.1 μ m.This film is done the absorbancy of full wavelength period and tested, the result illustrates that this film has very weak light absorptive in the near-infrared region as shown in Figure 6.
Embodiment 2
Measure " waste liquid " 80ml that the Brodie legal system obtains in the water washing process when being equipped with graphite oxide,, obtain the graphite oxide aqueous solution (shown in Fig. 2 (a)) of pH=4.00 by adding an amount of KOH.Then this graphite oxide aqueous solution is moved in 80 ℃ of water-baths, keep 15min, can form layer of even graphene oxide film at liquid level, graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature, the thickness that obtains support are the graphene oxide film (shown in Fig. 2 (b)) of 0.01 μ m.
Embodiment 3
Measure " waste liquid " 80ml that the Staudemaier legal system obtains in the water washing process when being equipped with graphite oxide,, obtain the graphite oxide aqueous solution (shown in Fig. 3 (a)) of pH=6.00 by adding an amount of NaOH.Then this graphite oxide aqueous solution is moved in 5 ℃ of water-baths, keep 48h, can form layer of even graphene oxide film, the graphene oxide film on the liquid level is pulled out at liquid level, dry 12h under the normal temperature obtains unsupported graphene oxide film (shown in Fig. 3 (b)).
Embodiment 4
Measure " waste liquid " 80ml that the Hummers legal system obtains in the water washing process when being equipped with graphite oxide,, obtain the graphite oxide aqueous solution (shown in Fig. 4 (a)) of pH=8.00 by adding an amount of KOH.Then this graphite oxide aqueous solution is moved in 98 ℃ of water-baths, keep 5min, can form layer of even graphene oxide film, the graphene oxide film on the liquid level is pulled out at liquid level, dry 12h under the normal temperature obtains unsupported graphene oxide film (shown in Fig. 4 (b)).
Embodiment 5
Measure " waste liquid " 80ml that the Staudemaier legal system obtains in the water washing process when being equipped with graphite oxide,, obtain the graphite oxide aqueous solution (shown in Fig. 5 (a)) of pH=13.00 by adding an amount of NaOH.Then this graphite oxide aqueous solution is moved in 80 ℃ of water-baths, keep 45min, can form layer of even graphene oxide film at liquid level, graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature, obtaining unsupported thickness is 100 μ m graphene oxide films (shown in Fig. 5 (b)).
Embodiment 6
According to the m graphene oxide: v distilled water=(1mg): proportionlity (1ml) adds graphite oxide and distilled water in the beaker, ultrasonic concussion 10h, and ultrasonic power is 20W, obtains finely disseminated graphene oxide solution; Measure this solution 80ml,, obtain the graphite oxide aqueous solution of pH=7.00 by adding an amount of NaOH aqueous solution.Then this graphite oxide aqueous solution is moved in 90 ℃ of water-baths, keep 40min, can form layer of even graphene oxide film at liquid level, the graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature obtains unsupported graphene oxide film.
Embodiment 7
According to m
Graphene oxide: v
Distilled water=(15mg): proportionlity (1ml) adds graphite oxide and distilled water in the beaker, ultrasonic concussion 5h, ultrasonic power is 160W, obtains finely disseminated graphene oxide solution; Measure this solution 80ml,, obtain the graphite oxide aqueous solution of pH=7.00 by adding an amount of NaOH aqueous solution.Then this graphite oxide aqueous solution is moved in 90 ℃ of water-baths, keep 40min, can form layer of even graphene oxide film at liquid level, the graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature obtains unsupported graphene oxide film.
Embodiment 8
According to m
Graphene oxide: v
Distilled water=(30mg): proportionlity (1ml) adds graphite oxide and distilled water in the beaker, ultrasonic concussion 0.5h, ultrasonic power is 300W, obtains finely disseminated graphene oxide solution; Again according to v
Graphene oxide solution: v
The vitriol oil: m
Potassium permanganate: m
SODIUMNITRATE=(100ml): (42ml): (8g): ratio (1g) is mixed graphene oxide solution, the vitriol oil, potassium permanganate and SODIUMNITRATE, places 98 ℃ of water-baths to react 3h, adds an amount of concentration and be 30% H
2O
2, centrifugation gets upper solution, i.e. and the graphene oxide solution of deep oxidation is according to v
The graphene oxide solution of deep oxidation: v
Distilled water=1: 3 ratio is with this solution dilution; Measure the solution 80ml after the dilution,, obtain the graphite oxide aqueous solution of PH=10.00 by adding an amount of NaOH aqueous solution.Then this graphite oxide aqueous solution is moved in 60 ℃ of water-baths, keep 60min, can form layer of even graphene oxide film at liquid level, the graphene oxide film on the liquid level is pulled out, dry 12h under the normal temperature obtains unsupported graphene oxide film.
Embodiment 9
Measure " waste liquid " 20ml that the Hummers legal system obtains in the water washing process when being equipped with graphite oxide, adding the 60ml distilled water and an amount of KOH aqueous solution, obtain the graphite oxide aqueous solution of pH=12.00.Use this solution of micropore filter paper filtering then, form one deck filter cake on filter paper, dry 24h under the normal temperature can obtain the graphene oxide film of support.
Embodiment 10
Measure " waste liquid " 20ml that the Staudemaier legal system obtains in the water washing process when being equipped with graphite oxide, adding an amount of HNO
3, obtain the graphite oxide aqueous solution of pH=3.00.Then an amount of this solution is coated on the plastics film, places 50 ℃ of baking ovens to dry, apply repeatedly again, drying operation 10 times, can obtain unsupported graphene oxide film.
In sum: utilize various acid or alkali, can make the graphene oxide mother liquor of different pH values, the transparency of these mother liquors reduces along with the increase of pH value, shown in (b) figure among the accompanying drawing 1-5 in the specification sheets; With different pH value mother liquors is raw material, and the graphene oxide film transparency for preparing is also inequality, and mother liquor pH value is big more, and preparation-obtained film clarity is low more, shown in (a) figure among the Figure of description 1-5.
Transparent graphene oxide film and method for regulating transmittance that the present invention proposes, be described by embodiment, person skilled obviously can be changed or suitably change and combination transparent graphene oxide film as herein described and preparation method thereof in not breaking away from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (5)
1. a transparent graphene oxide film is characterized in that the continuous increase along with mother liquor pH value, and preparation-obtained graphene oxide film transparence reduces gradually; Thickness is 0.01-100 μ m, and light transmission is regulated and control at 1%-95%.
2. the method for regulating transmittance of the described transparent graphene oxide film of claim 1 is characterised in that:
(1) scrub raffinate in preparation graphite oxide process adds acid or alkali in the perhaps common graphene oxide solution, and regulating the pH value is 1 ~ 13, and the mother liquor transparence increases with the pH value and reduces;
(2) utilize filter method, matrix coating method or liquid-gas interface self-assembly method to prepare the increase that has along with mother liquor pH value, the graphene oxide film that transparence reduces gradually.
3. the method for regulating transmittance of transparent graphene oxide film as claimed in claim 2 is characterised in that described acid comprises hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; Described alkali comprises sodium hydroxide, potassium hydroxide or ammoniacal liquor.
4. the method for regulating transmittance of transparent graphene oxide film as claimed in claim 2, be characterised in that described common graphene oxide solution, be with graphite oxide and solvent with 1～30: 1mg/mL puts into beaker, ultrasonic 0.5～10 h, ultrasonic power is 20～300W, obtains graphene oxide solution.
5. the method for regulating transmittance of transparent graphene oxide film as claimed in claim 4 is characterised in that described solvent comprises water, dehydrated alcohol, acetone, ether or N, dinethylformamide.
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| CN104445162A (en) * | 2014-11-12 | 2015-03-25 | 东莞市青麦田数码科技有限公司 | Graphene oxide aqueous solution and graphene oxide thin film as well as preparation method of graphene oxide thin film |
| WO2015061327A1 (en) * | 2013-10-21 | 2015-04-30 | The Penn State Research Foundation | Method for preparing graphene oxide films and fibers |
| CN110482538A (en) * | 2019-08-26 | 2019-11-22 | 上海利物盛纳米科技有限公司 | A kind of preparation method of the graphene oxide of controllable pH |
| CN112010290A (en) * | 2020-08-26 | 2020-12-01 | 兰州大学 | Method for industrially preparing graphene film |
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| WO2009143405A2 (en) * | 2008-05-22 | 2009-11-26 | The University Of North Carolina At Chapel Hill | Synthesis of graphene sheets and nanoparticle composites comprising same |
| CN101513998B (en) * | 2009-02-11 | 2011-01-05 | 中国科学院山西煤炭化学研究所 | Method for preparing ordered graphene oxide films |
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| WO2015061327A1 (en) * | 2013-10-21 | 2015-04-30 | The Penn State Research Foundation | Method for preparing graphene oxide films and fibers |
| US9284193B2 (en) | 2013-10-21 | 2016-03-15 | The Penn State Research Foundation | Method for preparing graphene oxide films and fibers |
| CN104445162A (en) * | 2014-11-12 | 2015-03-25 | 东莞市青麦田数码科技有限公司 | Graphene oxide aqueous solution and graphene oxide thin film as well as preparation method of graphene oxide thin film |
| CN110482538A (en) * | 2019-08-26 | 2019-11-22 | 上海利物盛纳米科技有限公司 | A kind of preparation method of the graphene oxide of controllable pH |
| CN112010290A (en) * | 2020-08-26 | 2020-12-01 | 兰州大学 | Method for industrially preparing graphene film |
| CN112267215A (en) * | 2020-10-21 | 2021-01-26 | 吉林大学 | Nanofiber membrane for alcohol detection and preparation method and application thereof |
| CN112267215B (en) * | 2020-10-21 | 2021-09-21 | 吉林大学 | Nanofiber membrane for alcohol detection and preparation method and application thereof |
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