CN108249424A - A kind of preparation method of the highly conductive ultra-thin graphene film of bromine doping - Google Patents
A kind of preparation method of the highly conductive ultra-thin graphene film of bromine doping Download PDFInfo
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- CN108249424A CN108249424A CN201810061894.3A CN201810061894A CN108249424A CN 108249424 A CN108249424 A CN 108249424A CN 201810061894 A CN201810061894 A CN 201810061894A CN 108249424 A CN108249424 A CN 108249424A
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- graphene film
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention discloses a kind of bromine doping highly conductive ultra-thin graphene film preparation method, the graphene film by graphene oxide it is filtered be pumped into film, electronation, solid-liquid synchronize transfer, high temperature graphitization, bromine doping and etc. obtain.The graphene film is made up of mono-layer oxidized/redox graphene physical crosslinking.Graphene film thickness is 10 2000 atomic layers.Graphene oxide film thickness very little, and inside there are it is a large amount of the defects of, thus have good transparency and fabulous flexibility.After electronation, most of functional group disappears, and graphene film starts conduction；High temperature reduction, graphene-structured reparation, electron mobility are promoted；Graphene carrier concentration is promoted after bromine doping.This graphene film can be used as high flexibility electrically conducting transparent device.
Description
Technical field
The present invention relates to the highly conductive ultra-thin stones that high-performance nano material and preparation method thereof more particularly to a kind of bromine adulterate
The preparation method of black alkene film.
Background technology
The graphene film of macroscopic view assembling graphene oxide or graphene nanometer sheet is the main application of nanoscale graphite alkene
Form, common preparation method is suction method, scrape embrane method, spin-coating method, spray coating method and dip coating etc..At further high temperature
The defects of managing, can repairing graphene, can effectively improve the electric conductivity and thermal conductance of graphene film, can be widely applied to
Smart mobile phone, intelligence are with oneself in the accompanied electronics equipment such as hardware, tablet computer, laptop.
But at present, the graphene film thickness that high temperature sintering is crossed is generally in more than 1um, many gas of enclosed inside,
During high pressure is suppressed, the stomata of closing is remained in the form of fold, the graphene film degree of orientation is caused to be deteriorated, density
Become smaller, and interlayer AB stacking degree is poor, seriously affected further improving for graphene film performance.
The graphene film conductivity reported at present is because fault of construction rests on 10 so far6S/m.Also have apart from metal very big
Distance.For this purpose, we are promoted graphene film conductivity to 18.9x10 by structure and the method for Composition Control6S/m, electricity
Conductance is promoted close to 20 times, and match in excellence or beauty metal.Graphene film prepared by the method can meet the highly conductive device of the overwhelming majority completely
Demand, the conductive design for graphene film opens new gate.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of highly conductive ultra-thin graphene film of bromine doping
Preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions：A kind of highly conductive ultra-thin graphene film of bromine doping
Preparation method comprises the following steps：
(1) graphene oxide is configured to a concentration of 0.5-10ug/mL graphene oxide water solutions, using AAO films as substrate
Filter film forming.
(2) graphene oxide membrane for being attached at AAO is placed in closed container, 80-100 degree HI high temperature is up smoked from bottom
Steam 0.1-1h.
(3) with the methods of vapor deposition, curtain coating by the solid transfer agent even application of thawing in redox graphene film surface,
And natural cooling at room temperature, until basilar memebrane comes off naturally.
(4) graphene film of solid transfer agent obtained above support is vapored away at a temperature of solid transfer agent volatilizees
Solid transfer agent obtains the graphene film of independent self-supporting.
(5) above-mentioned independent self-supporting graphene film is placed in high temperature furnace, is warming up to 3000 degrees Celsius, repair graphene film
Structure removes internal flaw.
(6) step 5 treated graphene film and a certain amount of bromine are placed in the container of same sealing, wherein bromine
Amount m and vessel volume v meet：M/v=1g/L is vacuumized after then whole container is freezed with liquid nitrogen until air is complete
It extracts.It is put into 30-40 degrees Celsius of baking oven and heats 12-24 hours after naturally to thaw under room temperature (20-30 DEG C), obtain bromine doping
Graphene film.
Further, the solid transfer agent, selected from following substance, such as paraffin, naphthalene, arsenic trioxide, camphor,
The small molecule solid matter not soluble in water that sulphur, norbornene, rosin etc. can distil or volatilize under certain conditions.
Further, the sublimation temperature of the solid transfer agent will be controlled below 320 degree；Sublimation pressure and environment
Oxygen content is depending on physical property.
Further, the temperature-rise period is as follows：0-2000 degrees Celsius, 5-20 centigrade per minutes；2000-3000 takes the photograph
Family name's degree, 2-5 centigrade per minutes.
The beneficial effects of the present invention are：General solid transfer agent is macromolecule in common technology at present, because it has
There is characteristic easy to operate, easy to attach, and can be removed by solution etches or high temperature sintering.But surface during solution etches
Tension can tear graphene film, must also have substrate support when being taken out from solution.The presence of solution prevent graphene film from
Presence is self-supporting on their own, base surface can only be fitted in.High temperature sintering can cause graphene film to shrink, it is impossible to maintain graphene sheet
The pattern of body, and can graphene be bonded with substrate.By the present invention in that with surface tension, substrate is removed；And with easily
Distil solid-state transfer agent so that nanoscale graphite alkene film can be self-supporting on their own in air.In the process, according to distillation
Principle removes solid-state transfer agent, and there is no the problem of surface tension, therefore graphene film will not be mutually adhered with substrate.Graphite-based
Bottom carries graphene film, and auxiliary graphene film completes 3000 degree of high annealing.Obtained graphene film thickness is controllable, stone
Black alkene is height-oriented, and almost without defect in lamella, based on piece interlayer is stacked by AB, all these structures are excellent for graphene film
The opposite sex can lay the foundation.According to the thickness of graphene film, which has certain transparency, and thickness is smaller, the transparency
Better, this undoubtedly extends the potential application of graphene film.Further by the doping of bromine, bromine atoms are graphene conjugation knot
Structure provides electronics, on the one hand, graphene band gap is opened；On the other hand, the electron density of graphene film is increased, improves conductance
Rate, be highly advantageous to its application in photoelectric field.
Description of the drawings
Fig. 1 is the atomic force microscopy diagram of bromine doped graphene film prepared by embodiment 1；
Fig. 2 is the pictorial diagram of bromine doped graphene film prepared by embodiment 1；
Fig. 3 is bromine doped graphene film Raman figure prepared by embodiment 1.
Fig. 4 is the xps figures of bromine doped graphene film prepared by embodiment 1；
Fig. 5 is the conductivity of the graphene film of different bromine dopings.
Specific embodiment
Embodiment 1：
(1) graphene oxide is configured to a concentration of 0.5ug/mL graphene oxide water solutions, is filtered by substrate of AAO films
Film forming.
(2) graphene oxide membrane for being attached at AAO is placed in closed container, 80 degree of HI high temperature are up fumigated from bottom
1h。
(3) with the method for vapor deposition by the solid transfer agent camphor even application of thawing in redox graphene film surface,
And Slow cooling at room temperature, until basilar memebrane comes off naturally.
(4) graphene film that solid transfer agent obtained above supports slowly is vapored away into solid transfer at 60 c
Agent obtains the graphene film of independent self-supporting.
(5) above-mentioned independent self-supporting graphene film is placed in high temperature furnace, is warming up to the speed of 5 centigrade per minutes
2000 degrees Celsius, 3000 degrees Celsius then are warming up to the speed of 2 centigrade per minutes, to repair graphene film structure, removal
Internal flaw.
(6) bromine of step 5 treated graphene film and 0.5g is placed in the container that volume is 500 milliliters, then
It is vacuumized after whole container is freezed with liquid nitrogen until air is extracted completely.It is put into after naturally to thaw under room temperature (20-30 DEG C)
It is heated in 30 degrees Celsius of baking oven, obtains the graphene film of bromine doping.With the extension of heating time, bromine content is gradually increased,
When be heated to 12 it is small when after, bromine content reaches 0.07wt%, and test shows that its conductivity is 19.1MS/m.It is small when being heated to 24
Shi Hou, conductivity reach 19.9MS/m.As shown in Figure 5.The atomic force scanning figure of the graphene film is as shown in Figure 1, from figure
As can be seen that the thickness of the graphene film is 36nm, the graphene film that the thickness is 36nm is can be seen that from the pictorial diagram of Fig. 2
It completely can be with self-supporting.Xps data are shown, are shown in inside graphite film with the presence of bromine atoms, Raman data in 0-1000cm-1Position
Raman peaks there are three putting.
Embodiment 2：
A kind of preparation method of the highly conductive ultra-thin graphene film of bromine doping, comprises the following steps：
(1) graphene oxide is configured to a concentration of 10ug/mL graphene oxide water solutions, is filtered by substrate of AAO films
Film forming.
(2) graphene oxide membrane for being attached at AAO is placed in closed container, 100 degree of HI high temperature are up fumigated from bottom
0.1h。
(3) with the method for curtain coating by the solid transfer agent rosin even application of thawing in redox graphene film surface,
And natural cooling at room temperature, until basilar memebrane comes off naturally.
(4) graphene film that solid transfer agent obtained above supports under 120 degree is vapored away into solid transfer agent, obtained
The graphene film of independent self-supporting.
(5) above-mentioned independent self-supporting graphene film is placed in high temperature furnace, is warming up to the rate of 20 centigrade per minutes
2000 degrees Celsius, 3000 degrees Celsius then are warming up to the rate of 5 centigrade per minutes, to repair graphene film structure, removal
Internal flaw.
(6) step 5 treated graphene film and 0.5g bromines are placed in 500 milliliters of container, then will entirely held
Device is vacuumized after being freezed with liquid nitrogen until air is extracted completely.Under room temperature (20-30 DEG C) 40 degrees Celsius are put into after naturally to thaw
Baking oven in heat 12 hours, obtain bromine doping graphene film.Its thickness is 40nm, it can be achieved that independent self-supporting, conductivity
For 16.9MS/m.
Embodiment 3：
A kind of preparation method of the highly conductive ultra-thin graphene film of bromine doping, comprises the following steps：
(1) graphene oxide is configured to a concentration of 1ug/mL graphene oxide water solutions, using AAO films as substrate filter into
Film.
(2) graphene oxide membrane for being attached at AAO is placed in closed container, 100 degree of HI high temperature are up fumigated from bottom
30 minutes.
(3) with the method for curtain coating by the solid transfer agent rosin even application of thawing in redox graphene film surface,
And natural cooling at room temperature, until basilar memebrane comes off naturally.
(4) graphene film that solid transfer agent obtained above supports at a temperature of 120 is vapored away into solid transfer agent, obtained
To the graphene film of independent self-supporting.
(5) above-mentioned independent self-supporting graphene film is placed in high temperature furnace, the rate of 10 centigrade per minutes is warming up to
2000 degrees Celsius, the speed of 4 centigrade per minutes is warming up to 3000 degrees Celsius, to repair graphene film structure, removes internal flaw.
(6) in the container of sealing that step 5 treated graphene film and 5g bromines are placed in same 500 milliliters, then
It is vacuumized after whole container is freezed with liquid nitrogen until air is extracted completely.It is put into after naturally to thaw under room temperature (20-30 DEG C)
It is heated 15 hours in 30-40 degrees Celsius of baking oven, obtains the graphene film of bromine doping.Its thickness is 50nm, it can be achieved that independently certainly
Support, conductivity 15.9MS/m.
Claims (5)
1. a kind of preparation method of the highly conductive ultra-thin graphene film of bromine doping, which is characterized in that comprise the following steps：
(1) graphene oxide is configured to a concentration of 0.5-10ug/mL graphene oxide water solutions, is filtered by substrate of AAO films
Film forming.
(2) graphene oxide membrane for being attached at AAO is placed in closed container, 80-100 degree HI high temperature is up fumigated from bottom
0.1-1h。
(3) by the solid transfer agent even application of thawing in redox graphene film surface, and natural cooling at room temperature, directly
It comes off naturally to basilar memebrane.
(4) graphene film of solid transfer agent obtained above support is vapored away into solid at a temperature of solid transfer agent volatilizees
Transfer agent obtains the graphene film of independent self-supporting.
(5) above-mentioned independent self-supporting graphene film is placed in high temperature furnace, is warming up to 3000 degrees Celsius, repair graphene film knot
Structure removes internal flaw.
(6) step 5 treated graphene film and a certain amount of bromine are placed in the container of same sealing, wherein the amount of bromine
M and vessel volume v meets：M/v=1g/L is vacuumized after then whole container is freezed with liquid nitrogen until air is taken out completely
It removes.It is put into 30-40 degrees Celsius of baking oven and heats 12-24 hours after naturally to thaw under room temperature (20-30 DEG C), obtain bromine doping
Graphene film.
2. the method as described in claim 1, which is characterized in that the solid transfer agent, selected from following substance, such as stone
Wax, naphthalene, arsenic trioxide, camphor, sulphur, norbornene, rosin etc. can distil or volatilize under certain conditions not soluble in water
Small molecule solid matter.
3. the method as described in claim 1, which is characterized in that the sublimation temperature of the solid transfer agent will be controlled 320
Below degree；Sublimation pressure and environment oxygen content are depending on physical property.
4. the method as described in claim 1, which is characterized in that the temperature-rise period in the step 5 is as follows：0-2000 is Celsius
Degree, 5-20 centigrade per minutes；2000-3000 degrees Celsius, 2-5 centigrade per minutes.
5. the method as described in claim 1, which is characterized in that in the step 3, will melt the methods of by being deposited, being cast
Solid transfer agent even application in redox graphene film surface.
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Cited By (16)
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| CN108821263A (en) * | 2018-07-10 | 2018-11-16 | 杭州高烯科技有限公司 | A kind of high-strength graphite alkene film and preparation method thereof |
| CN108821264A (en) * | 2018-07-10 | 2018-11-16 | 杭州高烯科技有限公司 | A kind of nanoscale sonic generator |
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| CN108892133B (en) * | 2018-07-10 | 2020-08-14 | 浙江大学 | Nanoscale sound wave generating film and nanoscale sound wave generator |
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