CN110182796A - A kind of bromine doping graphene oxide preparation method - Google Patents
A kind of bromine doping graphene oxide preparation method Download PDFInfo
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- CN110182796A CN110182796A CN201910534816.5A CN201910534816A CN110182796A CN 110182796 A CN110182796 A CN 110182796A CN 201910534816 A CN201910534816 A CN 201910534816A CN 110182796 A CN110182796 A CN 110182796A
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Abstract
The present invention relates to photoelectric field, especially hydro-thermal reactions, and bromine doping graphene oxide is made.Not only consumptive material is more and complex steps for existing doping type graphene oxide synthetic technology by the present invention, the problem of being not suitable for batch production, provide a kind of doping by heterogeneous bromine atom, the energy level for effectively to modulate graphene oxide, the semi-conductor type bromine doping graphene oxide technology of preparing for optimizing the photoelectric properties of graphene oxide.Bromine of the invention adulterates graphene oxide preparation method, it is characterized in that the preparation method uses graphene oxide, pure hydrobromic acid is analyzed than addition by certain carbon bromine atom and disposably generates bromine doping graphene oxide through hydro-thermal reaction, including is prepared graphene oxide, obtained graphene oxide and three hydrobromic acid solution, hydro-thermal reaction steps.
Description
Technical field
The present invention relates to photoelectric field, especially hydro-thermal reactions, and bromine doping graphene oxide is made.
Background technique
The graphene oxide of doping type, except inherit graphene oxide is hydrophilic, surface area is big, carrier mobility rate is high,
Except many excellent performances such as mechanical flexibility is good and optical property is stablized, due to its also have significant quantum confinement effect and
Edge effect possesses special optical property, characteristic electron etc., gets more and more people's extensive concerning and study in recent years.Aoxidize stone
Black alkene technology of preparing multiplicity, wherein mainly include Hummers method and numerous modified Hummers methods, electrochemical oxidation process, from lower and
Upper growth method etc..
Currently, doping type graphene oxide is not yet widely applied the reason is that stably producing oxidation in optoelectronic areas
The technology of graphene is not mature enough, and main reason is the absence of the band structure that can effectively modulate graphene oxide and optical
The means of matter.Currently, synthesizing doped type graphene oxide all uses the synthetic technologys such as high vacuum, ion implanting, high temperature, this is not only
At high cost and complex steps are not suitable for batch production.
It is intended to graphene oxide just to need to modulate graphene oxide with from electronic field expanding to optoelectronic areas
Energy level, optical property, electrical properties.Since graphene oxide contains numerous hydrophilic functional groups, such as hydroxyl, carboxyl etc., therefore it has
There is good surface graft, more functional group can be mixed by specially treated, and different officials can be mixed by doping
Level structure, the optical property, electrical properties for effectively modulating graphene oxide afterwards can be rolled into a ball.
It wants to produce graphene oxide composite material in enormous quantities, it just must be from low cost, technology is simple and environmentally-friendly, can give birth in batches
The preparation method of force of labor is started with.Obviously, Hummers method prepares graphene oxide presoma and prepares bromine doping through hydro-thermal reaction again
Graphene oxide, not only has that equipment and technical process are simple, reaction disposable the features such as completing but also aggregate velocity are fast, yield
It is high.
Summary of the invention
Not only consumptive material is more and complex steps for existing doping type graphene oxide synthetic technology by the present invention, is not suitable for batch
The problem of production, provides a kind of doping by heterogeneous bromine atom, effectively to modulate the energy level of graphene oxide, makes to aoxidize
The semi-conductor type bromine that the photoelectric properties of graphene are optimized adulterates graphene oxide technology of preparing.
A kind of bromine of the invention adulterates graphene oxide preparation method, it is characterised in that the preparation method uses graphite oxide
Alkene analyzes pure hydrobromic acid than addition by certain carbon bromine atom and disposably generates bromine doping graphene oxide through hydro-thermal reaction, including
It prepares graphene oxide, obtain graphene oxide and three hydrobromic acid solution, hydro-thermal reaction steps, specific as follows:
1) it prepares graphene oxide: the 23ml concentrated sulfuric acid being taken to be placed in the beaker of ice bath, weigh 0.5g graphite powder and 0.25g sodium nitrate
It is poured into the concentrated sulfuric acid after mixing, after stirring half an hour with mechanical agitator, it is mixed that weighing 3g potassium permanganate is slowly added into the concentrated sulfuric acid
It closes in solution, so that the solution is continued ice bath one hour, then go to it in 35 DEG C of water-baths, after reacting one hour, then by it turn
Into 98 DEG C of water-baths, after 60ml deionized water is added, solution is kept to stir half an hour, property pours into 100ml deionization again
Water, and 10ml hydrogenperoxide steam generator is added, golden solution is finally obtained, this solution is washed using 10% hydrochloric acid solution centrifugation
It washs 3-5 times, until by golden yellow precipitate object, i.e. graphite oxide is dried in 60 DEG C in detection centrifuged supernatant after sulfate radical-free ion
It does spare；
2) graphene oxide and hydrobromic acid solution are prepared: weighing graphene oxide 0.1g obtained in step 1) in beaker,
100ml deionized water is added, ultrasound is prepared after three hours and obtains the graphene oxide solution of 1mg/ml, in molar ratio for 5:1's
Carbon bromine atom hydrobromic acid more analytically pure than the above-mentioned graphene oxide solution and 7.57ml for taking 32.43ml stirs ultrasonic mixing Cheng Jun
Even solution；
3) hydro-thermal reaction: graphene oxide and hydrobromic acid mixed solution that step 2 is prepared are placed in the reaction kettle of 50ml
In lining, be allowed in a kettle at 170 DEG C react 10h obtain bromine doping graphene oxide.
Bromine of the invention adulterates graphene oxide technology of preparing, in such a way that bromine adulterates, has modulated graphene oxide
Band structure, effectively changes the performance of graphene oxide, so that bromine doping graphene oxide prepared by the present invention be made to have
More excellent photoelectricity and luminance modulation performance, can be used for field of photodetectors.In addition to this, the present invention also has the following effects that
And advantage:
1, overall technology route is innovated, the disposable completion of reaction, with equipment and technical process, simple, the brief energy, speed are fast
The features such as high with yield.The graphene oxide solution that Hummers method is prepared is primary through hydro-thermal reaction after mixing with hydrobromic acid
Property reaction generate bromine adulterate graphene oxide；
2, the method prepares that bromine doping graphene oxide operation is feasible, and the bromine that is prepared doping graphene oxide has excellent
Photoelectric properties have modulated the energy level of graphene oxide by way of doping, effectively improve the performance of graphene oxide；
3, since hydro-thermal reaction method can amplify according to production scale, so suitable for mass production.
Detailed description of the invention
Fig. 1 is the Raman spectrum (Raman) that bromine adulterates graphene oxide；
Fig. 2 is the FTIR spectrum (FT-IR) that bromine adulterates graphene oxide；
Fig. 3 is the UV-vis absorption spectrum (UV-Vis) that bromine adulterates graphene oxide；
Fig. 4 is the photoluminescence spectra (PL) that bromine adulterates graphene oxide；
Fig. 5 is the atomic force microscope images (AFM) that bromine adulterates graphene oxide.
Specific embodiment
Embodiment 1: a kind of technology of preparing of bromine doping graphene oxide analyzes pure hydrogen bromine than being added by certain carbon bromine atom
Acid disposably generates bromine doping graphene oxide through hydro-thermal reaction, including prepares graphene oxide, obtains graphene oxide and hydrogen
Three bromic acid solution, hydro-thermal reaction steps, specific as follows:
1) it prepares graphene oxide: the 23ml concentrated sulfuric acid being taken to be placed in the beaker of ice bath, weigh 0.5g graphite powder and 0.25g sodium nitrate
It is poured into the concentrated sulfuric acid after mixing, after stirring half an hour with mechanical agitator, it is mixed that weighing 3g potassium permanganate is slowly added into the concentrated sulfuric acid
It closes in solution, so that the solution is continued ice bath one hour, then go to it in 35 DEG C of water-baths, after reacting one hour, then by it turn
Into 98 DEG C of water-baths, after 60ml deionized water is added, solution is kept to stir half an hour, property pours into 100ml deionization again
Water, and 10ml hydrogenperoxide steam generator is added, golden solution is finally obtained, this solution is washed using 10% hydrochloric acid solution centrifugation
It washs three to five times, until by golden yellow precipitate, i.e. graphite oxide is dried in 60 DEG C in detection centrifuged supernatant after sulfate radical-free ion
It does spare；
2) graphene oxide and hydrobromic acid solution are obtained: weighing graphene oxide 0.1g obtained in step 1) in beaker,
100ml deionized water is added, ultrasound is prepared after three hours and obtains the graphene oxide solution of 1mg/ml, in molar ratio for 5:1's
Carbon bromine atom hydrobromic acid more analytically pure than the above-mentioned graphene oxide solution and 7.57ml for taking 32.43ml stirs ultrasonic mixing Cheng Jun
Even solution；
3) hydro-thermal reaction: graphene oxide and hydrobromic acid mixed solution that step 2 is prepared are placed in the reaction kettle of 50ml
In lining, it is allowed to obtain bromine doping graphene oxide in 170 DEG C of reaction 10h in a kettle.
As shown in Figure 1, the bromine doping graphene oxide solution drop coating obtained after hydro-thermal reaction is surveyed after silicon chip substrate drying
The Raman characterization figure of examination, hence it is evident that it can be seen that the peak G, the peak D and the peak 2D；
As shown in Fig. 2, the bromine doping graphene oxide solution drop coating obtained after hydro-thermal reaction scrapes it after silicon chip substrate drying
The Fourier infrared absorption spectrum measured after lower using pellet technique, hence it is evident that it can be seen that C=C, C-Br, C-H, C-O, etc.
The vibration peak of chemical bond；
As shown in figure 3, what the bromine doping graphene oxide solution drop coating obtained after hydro-thermal reaction measured after silicon chip substrate drying
UV-vis absorption spectrum, it can be seen that have apparent ultraviolet absorption peak；
As shown in figure 4, what the bromine doping graphene oxide solution drop coating obtained after hydro-thermal reaction measured after silicon chip substrate drying
Photoluminescence spectrum, it can be seen that have good optical property；
As shown in figure 5, what the bromine doping graphene oxide solution drop coating obtained after hydro-thermal reaction measured after silicon chip substrate drying
Atomic force microscopy diagram, it can be seen that it is about 20nm or so that this bromine, which adulterates graphene oxide quantum dot size,.
Claims (1)
1. a kind of bromine adulterates graphene oxide preparation method, it is characterised in that the preparation method uses graphene oxide, by certain
Carbon bromine atom analyzes pure hydrobromic acid than addition and disposably generates bromine doping graphene oxide, including preparation oxidation stone through hydro-thermal reaction
Black alkene obtains graphene oxide and three hydrobromic acid solution, hydro-thermal reaction steps, specific as follows:
1) it prepares graphene oxide: the 23ml concentrated sulfuric acid being taken to be placed in the beaker of ice bath, weigh 0.5g graphite powder and 0.25g sodium nitrate
It is poured into the concentrated sulfuric acid after mixing, after stirring half an hour with mechanical agitator, it is mixed that weighing 3g potassium permanganate is slowly added into the concentrated sulfuric acid
It closes in solution, so that the solution is continued ice bath one hour, then go to it in 35 DEG C of water-baths, after reacting one hour, then by it turn
Into 98 DEG C of water-baths, after 60ml deionized water is added, solution is kept to stir half an hour, property pours into 100ml deionization again
Water, and 10ml hydrogenperoxide steam generator is added, golden solution is finally obtained, this solution is washed using 10% hydrochloric acid solution centrifugation
It washs 3-5 times, until by golden yellow precipitate object, i.e. graphite oxide is dried in 60 DEG C in detection centrifuged supernatant after sulfate radical-free ion
It does spare；
2) graphene oxide and hydrobromic acid solution are prepared: weighing graphene oxide 0.1g obtained in step 1) in beaker,
100ml deionized water is added, ultrasound is prepared after three hours and obtains the graphene oxide solution of 1mg/ml, in molar ratio for 5:1's
Carbon bromine atom hydrobromic acid more analytically pure than the above-mentioned graphene oxide solution and 7.57ml for taking 32.43ml stirs ultrasonic mixing Cheng Jun
Even solution；
3) hydro-thermal reaction: graphene oxide and hydrobromic acid mixed solution that step 2 is prepared are placed in the reaction kettle of 50ml
In lining, be allowed in a kettle at 170 DEG C react 10h obtain bromine doping graphene oxide.
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| CN201910534816.5A CN110182796A (en) | 2019-06-20 | 2019-06-20 | A kind of bromine doping graphene oxide preparation method |
| CN201910964159.8A CN110562970A (en) | 2019-06-20 | 2019-10-11 | Preparation method of bromine-doped graphene oxide |
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| CN111682206A (en) * | 2020-07-07 | 2020-09-18 | 长沙三思新材料科技有限公司 | Lithium ion battery cathode slurry based on graphene-silicon dioxide composite aerogel and preparation method thereof |
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| CN102275902B (en) * | 2010-06-12 | 2013-04-17 | 中国科学院金属研究所 | Method for preparing graphene material by reducing graphene oxide |
| CN103145122A (en) * | 2013-03-25 | 2013-06-12 | 西北工业大学 | Preparation method of nitrogen-doped graphene |
| CN103726133B (en) * | 2014-01-02 | 2016-04-06 | 东华大学 | High strength, compact neat porous graphene fiber and continuous production method thereof |
| CN105036121A (en) * | 2015-07-07 | 2015-11-11 | 哈尔滨工业大学 | Preparation method for reinforced graphene surfactant |
| CN105633266A (en) * | 2015-12-31 | 2016-06-01 | 桂林电子科技大学 | Preparation method for composite thermoelectric film with flexible reduced graphene oxide and tellurium nano wires |
| CN106629674B (en) * | 2016-09-22 | 2019-02-22 | 林飘飘 | A kind of method of preparing grapheme through oxidation reduction |
| CN106602064A (en) * | 2016-12-27 | 2017-04-26 | 深圳市川马电子股份有限公司 | Preparation method and application of iodine-doped graphene |
| US10556798B2 (en) * | 2017-01-13 | 2020-02-11 | Lakehead University | Synthesis of fluorinated graphene oxide for electrochemical applications |
| CN107117599B (en) * | 2017-04-19 | 2020-11-13 | 东华大学 | Preparation method of chloro-hybrid graphene |
| CN107416800A (en) * | 2017-08-15 | 2017-12-01 | 东南大学 | A kind of method that hydro-thermal method prepares N and S codope three-dimensional grapheme materials |
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| CN111682206A (en) * | 2020-07-07 | 2020-09-18 | 长沙三思新材料科技有限公司 | Lithium ion battery cathode slurry based on graphene-silicon dioxide composite aerogel and preparation method thereof |
| CN111682206B (en) * | 2020-07-07 | 2021-11-05 | 江苏日御光伏新材料科技有限公司 | Lithium ion battery cathode slurry based on graphene-silicon dioxide composite aerogel and preparation method thereof |
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