CN107140625A - A kind of method that utilization vegetable oil prepares graphene film - Google Patents
A kind of method that utilization vegetable oil prepares graphene film Download PDFInfo
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- CN107140625A CN107140625A CN201710449456.XA CN201710449456A CN107140625A CN 107140625 A CN107140625 A CN 107140625A CN 201710449456 A CN201710449456 A CN 201710449456A CN 107140625 A CN107140625 A CN 107140625A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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Abstract
The invention discloses a kind of method that utilization vegetable oil prepares graphene film.The growth presoma and growth substrate of graphene are placed on quartz ampoule heating zone, then by the quartzy seal of tube and highest annealing temperature is warming up to, in the process, the atmospheric pressure in quartz ampoule is kept by the valve of opening.3 5min annealing completions are kept under highest annealing temperature, sample is removed from heating zone and cooled down, the sample after cooling is using polymethyl methacrylate auxiliary graphene transfer.Surface polymethyl methacrylate finally is removed with acetone, is washed, dries, obtains adhering to graphene film on a glass.The present invention is compared with the method for conventional synthesis graphene, under Atmospheric Condition, carbon source is used as without using pure gas, alternatively inexpensive reproducible vegetable oil, safety and it need not form vacuum environment, middle complicated tediously long processing procedure is eliminated, and the graphene generated under Atmospheric Condition shows good tuneable film characteristics.In addition the nickel foil of low-purity can reduce cost in terms of graphene film production.
Description
Technical field
It is more particularly to a kind of to utilize renewable presoma vegetable oil the present invention relates to a kind of preparation method of graphene film
The method for directly preparing graphene film.
Background technology
Graphene is sp2The thickness of hydbridized carbon atoms formation be only individual layer atom to be arranged in cellular hexaplanar brilliant
Body, in single-layer graphene, a length of 0.142nm of carbon-carbon bond, thickness only has 0.334nm.Graphene has excellent optical property,
Theoretical and experimental results show that it is 97.7% that single-layer graphene, which absorbs 2.3% visible ray, i.e. transmitance, and electronics is in graphene
Scattering is not susceptible to during middle transmission, its electrical conductivity is up to 104S/m, is the optimal material of electric conductivity at room temperature.The conduction of graphene
Property can be controlled by the method for chemical modification, and can obtain the various derivatives based on graphene simultaneously, bilayer graphene
Insulating properties can be also showed under certain condition.Graphene is intensity and hardness highest crystal structure in known materials simultaneously,
Its tensile strength and modulus of elasticity are respectively 125GPa and 1.1TPa, and the strength degree of graphene is 42N/m2.The room of graphene
It is about 5300W/mK to warm conductance, higher than CNT and diamond, is the thermal conductivity of copper at room temperature more than 10 times, graphene
Theoretical specific surface area up to 2630m2/g.Due to these excellent characteristics, graphene is considered as organic light of future generation
The preferred material of electric material, multifunctional composite and microelectronics original paper field.The method for preparing graphene at present is a lot, but often
The method of kind has its limitation, it is difficult to maximization and industrialized production are realized, so it is sustainable to explore a kind of stability and high efficiency
Synthetic method be particularly important.
The method of traditional making graphene has mechanical stripping method, oxidation-reduction method, chemical vapour deposition technique（CVD）And
Organic synthesis method, epitaxial growth method and the CNT occurred in recent years splits method etc..
Mechanical stripping method goes out graphene sheet layer using mechanical force from graphite crystal sur-face peeling, is initially to prepare graphene
Physical method.2004, Britain Manchester college professors Geim etc. published thesis title using the success of this method on Science
It is prepared for graphene film.Its specific method is as follows：Highly oriented pyrolytic graphite (HOPG) is fixed on SiO with photoresist first2/Si
In substrate and it is calcined, is then pasted repeatedly with adhesive tape, separate SiO2Unnecessary graphite flake in/Si substrates, will be stayed
Graphite flake on Si chips, which is immersed in acetone and distilled water, to be cleaned by ultrasonic, and obtains the lamella that thickness is less than 10nm, these
Thin layer passes through Van der Waals force or capillarity and SiO2Combine closely, individual layer is finally picked out or many using AFM
The graphene of layer.This method production dilute yield of graphite is very low, and the size of lamella is smaller, be only applicable to scientific research and can not
Put into large-scale practical application.
Early in 1958, graphite oxide was made using the concentrated sulfuric acid and potassium permanganate oxidation graphite in Hummers etc..Wang etc. exists
Improved on the basis of Hummers, before the oxidation, use K2S2O8And P2O5Graphite is pre-processed, before oxidation effectiveness ratio
Person is more preferable（Wang Z, Zhou X, Zhang J, et al. Direct Electrochemical Reduction of
Single-Layer Graphene Oxide and Subsequent Functionalization with Glucose
Oxidase[J]. Journal of Physical Chemistry C, 2009, 113(32):14071-14075）.
Stankovich etc. handles graphite oxide with hydrazine hydrate, and 24h is reacted at 100 DEG C, it is to avoid reunion finally gives graphene product
（Stankovich S, Dikin D A, Piner R D, et al. Synthesis of graphene-based
nanosheets via chemical reduction of exfoliated graphite oxide[J]. Carbon,
2007, 45(7):1558-1565）.Oxidation-reduction method is broadly divided into three steps：The first step is existed using oxidizing species
Graphite surface adds oxy radical, increases the interfloor distance of graphite, weakens Van der Waals force, is conducive to the stripping of second step；Second
Step accelerates the stripping of graphite by the way of sonic oscillation, forms graphite oxide solution；3rd step uses reducing agent reduction-oxidation
Graphite obtains graphene product.Graphene made from this method has more fault of construction, so as to have a strong impact on its electrical property
Energy.
Organic synthesis method refers to simple aromatic ring organic matter or derivatives thereof for elementary cell, passes through hyperbranched, dehydrogenation etc.
Reaction prepares graphene, and this method is only in laboratory stage at present.
Epitaxial growth method（Epitaxial Growth）Refer to that SiC causes carbon under conditions of ultravacuum by high-temperature heating
Silicon molecule evaporation removing in SiClx, carbon atom, which is rearranged, is combined into graphene platelet, and graphene product made from this method is thick
Degree is uneven, and the graphene number of plies is difficult to control to.
CNT (CNTs) is the one-dimentional structure that curls into of carbon atom of single or multiple lift.CNT splits method
From longitudinally slit CNT, single or multiple lift graphene is then obtained.Carbon nanometer is splitted method and typically carried out in a heated condition,
The quality of graphene that is prepared by the method is good, efficiency high.But the method is using CNT as raw material, source is not enriched, cost
It is higher, limit the application of the method.
Chemical vapour deposition technique（CVD）It is a kind of most common method of controllable preparation large-area graphene.It main
Method is, by the use of planar metal as substrate and catalyst, a certain amount of carbon source presoma and hydrogen to be passed through in hot environment,
Deposited after interaction in metal surface and to obtain graphite dilute.Generally to ensure that the security of experiment, should also connect in system
Argon gas is passed through to be protected by.The pure gas used in this method is expensive, and danger coefficient is high, while application of vacuum is required, because
This seriously hinders the commercialized development that graphene is made in such a method.
The method of traditional production graphene has the restraining factors for hindering its development so that the development prospect of graphene becomes
And it is pessimistic, therefore find one kind and prepare the sustainable method of simple, cheap, efficient stable and prepare graphene and become ten
Divide urgent.
The content of the invention
The problem of being existed based on above method, it is an object of the invention to provide it is a kind of efficiently, stably, it is sustainable using planting
The method that thing oil prepares graphene film.
The present invention is in conventional chemical vapor sedimentation（CVD）Prepare and be improved on the basis of graphene, using it is cheap, can
The vegetable oil of regeneration is as presoma, the graphene film of quick thermal synthesis uniformly continuous, do not need during this pure gas and
Application of vacuum.
The present invention is adopted the following technical scheme that：
（1）The growth presoma and growth substrate of graphene are placed on to the quartz ampoule heating zone in CVD stoves；（2）By quartz ampoule
Seal and highest annealing temperature is simultaneously warming up to 30-50 DEG C/min speed, in the process, the valve opened by one end is kept
Pressure in quartz ampoule is an atmospheric pressure；（3）3-5min is kept under highest annealing temperature, then moves sample from heating zone
Remove, and cooled down with 25 DEG C/min speed；（4）Sample after cooling uses polymethyl methacrylate（PMMA）Aid in stone
Black alkene transfer；（5）Finally with acetone, immersion removes surface PMMA for a long time, with deionized water cyclic washing sample, dries naturally
After be placed in vacuum drying chamber 80-90 DEG C and dry 2-4 hours, obtain adhering to graphene film on a glass.
The graphene growth presoma is vegetable oil.
The vegetable oil is the one or several kinds in peanut oil, soya-bean oil, linseed oil, castor oil, rapeseed oil, sesame oil.
The growth substrate is polycrystalline nickel foil.
The highest annealing temperature is 600-750 DEG C.
The polymethyl methacrylate auxiliary graphene transfer refers to being spun to growth with polymethyl methacrylate
On the graphenic surface above nickel foil, then by sample drying, then by the nickel foil FeCl of bottom3Solution corrosion is fully to go
Remove, after repeatedly being washed with deionized water, be transferred in substrate of glass, and be dried.
Analysis on Mechanism in preparation process：
The growth of graphene is along with progressively heating and the process of rapid quenching.First, by in-furnace temperature with 30-50 DEG C/min's
Speed is increased to 600-750 DEG C, then keeps 3-5min.After this stage, sample is removed from heating zone immediately, fast quickly cooling
But（25℃/min）, the then graphene film of isolated continuous uniform.Temperature rise period, typically at 300 DEG C, in peanut oil
Long chain hydrocarbons are pyrolyzed as carbonaceous gas construction unit, such as methanol, ethanol, and other gases are also produced in succession, including hydrogen gas and water and
Carbon dioxide etc..Most vegetable oil is vaporized at 400 DEG C or so, while the quality of vegetable oil is quickly reduced.When temperature liter
Height arrives 600-750 DEG C, and these construction units begin to decompose into carbon atom while being deposited on nickel foil surface, and then sample is in annealing 3-
Further promote carbon atom in 5min time in the deposition on nickel foil surface.
During temperature is raised, the long chain hydrocarbons in oil are decomposed to form vapor in the presence of oxygen, and water steams
Gas can promote the corrosion of the surface amorphous carbon of nickel foil, so the shape of amorphous carbon atom is not observed in we in the sample
Into simultaneously this also contributes to the catalytic activity that nickel foil surface is maintained when decomposing vegetable oil.In addition excessive vegetable oil can cause
There is substantial amounts of Carbon deposition in nickel foil surface, the crystallization for then having graphene on nickel foil surface is formed.
Annealing temperature is an important parameter for significantly affecting graphene growth under Atmospheric Condition.In annealing temperature
Under conditions of 450 DEG C, the formation of an incomplete graphene film is observed, and it is not enough that this may be attributed to energy, it is difficult to
Realize to the free of precursor material and integrate.Conversely in higher annealing temperature（More than 750 DEG C）Under, thick graphene film is seen
Measure, this is probably the increase and the elevated result of graphitization temperature due to carbon spread speed.Additionally due to generally requiring stone
Black alkene be placed on specific matrix characterized, physical measurement and application study, therefore graphene transfer techniques are certain
The development prospect of graphene is determined in degree.
The advantage of the invention is that compared with the method for conventional synthesis graphene, under Atmospheric Condition, without using pure
Gas（Such as methane, ethene, acetylene）As carbon source, substituting is inexpensive reproducible vegetable oil；Plant used
Oil is very safe, without the need for vacuum environment is formed, and eliminates middle complicated tediously long processing procedure, and big compression ring
The graphene generated under the conditions of border shows good tuneable film characteristics.In addition the nickel foil of low-purity can be in graphite
Cost is reduced in terms of alkene film production.It is quick, simple and direct, safe that this method, which prepares graphene, potentially may be used while possessing
Autgmentability and integrated friendly, it is important that it goes to solve key obstacle there is provided a chance, make graphene production towards height
Effectization, the direction of maximization are developed.
Brief description of the drawings
Fig. 1 is the AFM metallographic spectrograms of graphene film prepared by the present invention.
Fig. 2 is thickness chart of the graphene film prepared by the present invention in Z axis.
Embodiment
Substantive distinguishing features of the present invention and advantage are described further below in conjunction with the accompanying drawings and by specific embodiment, but this
Invention is not limited to embodiment set forth below.
Embodiment 1：
The growth presoma peanut oil and growth substrate nickel foil of graphene are placed on quartz ampoule（Long 100cm, diameter 5cm）Heating
Area, then by the quartzy seal of tube and is to slowly warm up to 750 DEG C with 30 DEG C/min speed.In heating process, beaten by one end
The valve opened keeps the pressure in quartz ampoule to be an atmospheric pressure.When temperature is increased to 750 DEG C, presoma peanut oil starts point
Solution is deposited on nickel foil surface simultaneously into carbon atom, and annealing time is 3.5 minutes.After the completion of annealing stage, by sample from heating zone
Removal is cooled down with 25 DEG C/min speed at room temperature.Sample after cooling uses polymethyl methacrylate（PMMA）It is auxiliary
Transfer graphene film is helped, is revolved concentration with 3000r/min for 40mg/ml PMMA solution using KW-4A types whirler
It is coated onto and is grown on the graphene film on nickel foil surface.80 DEG C are placed in vacuum drying chamber after sample after spin coating is dried naturally
Drying 2 hours, is subsequently placed to 1mol/L FeCl3Nickel foil metallic substrates are fully removed in solution, then continuous several times are steamed
It is transferred to after distilled water cleaning in substrate of glass, the sample after processing is placed in 80 DEG C of drying 2 in vacuum drying chamber after drying naturally small
When, finally with acetone, immersion removes surface PMMA for a long time, and with deionized water cyclic washing sample, vacuum is placed in after drying naturally
Dried 2 hours for 80 DEG C in drying box, then obtain adhering to graphene film on a glass.
Embodiment 2：
The growth presoma rapeseed oil and growth substrate nickel foil of graphene are placed on quartz ampoule（Long 100cm, diameter 5cm）Heating
Area, then by the quartzy seal of tube and is to slowly warm up to 700 DEG C with 50 DEG C/min speed.In temperature-rise period, beaten by one end
The valve opened keeps the atmospheric pressure in quartz ampoule.When temperature is increased to 700 DEG C, it is former that presoma rapeseed oil begins to decompose into carbon
Son is deposited on nickel foil surface simultaneously, and then sample further promotes carbon atom on nickel foil surface within annealing 5min time
Deposition.After the completion of annealing stage, sample is removed from heating zone and cooled down with 25 DEG C/min speed.Sample after cooling is used
Polymethyl methacrylate（PMMA）Secondary transfer graphene film, be by the concentration of preparation using KW-4A types whirler
40mg/ml PMMA solution is spun to 3000r/min to be grown on the graphene film on nickel foil surface.By the sample after spin coating
Naturally 80 DEG C are placed in vacuum drying chamber after drying to dry 2 hours, are subsequently placed to 1mol/L FeCl3Fully removed in solution
Nickel foil metallic substrates, are transferred in substrate of glass after then continuous several times are cleaned with distilled water, after sample dries naturally after processing
It is placed in vacuum drying chamber 80 DEG C to dry 2 hours, finally with acetone, immersion removes surface PMMA for a long time, with deionized water repeatedly
Washing sample, is placed in vacuum drying chamber 80 DEG C and dries 2 hours, then obtain adhering to graphite on a glass after drying naturally
Alkene film.
Embodiment 3：
The growth presoma sesame oil and growth substrate nickel foil of graphene are placed on quartz ampoule（Long 100cm, diameter 5cm）Heating
Area, then by the quartzy seal of tube and is to slowly warm up to 600 DEG C with 50 DEG C/min speed.In the temperature rise period, opened by one end
Valve keep the atmospheric pressure in quartz ampoule.When temperature is increased to 600 DEG C, presoma sesame oil begins to decompose into carbon atom
Nickel foil surface is deposited on simultaneously, then sample further promotes carbon atom in the heavy of nickel foil surface within annealing 5min time
Product.After the completion of annealing stage, sample is removed from heating zone and cooled down with 25 DEG C/min speed.Sample after cooling is using poly-
Methyl methacrylate（PMMA）Secondary transfer graphene film, be by the concentration of preparation using KW-4A types whirler
40mg/ml PMMA solution is spun to 3000r/min to be grown on the graphene film on nickel foil surface.By the sample after spin coating
Naturally 80 DEG C are placed in vacuum drying chamber after drying to dry 2 hours, are subsequently placed to 1mol/L FeCl3Fully removed in solution
Nickel foil metallic substrates, are dragged for substrate of glass after then continuous several times are cleaned with distilled water, and sample dries rearmounted naturally after processing
Dried 2 hours for 80 DEG C in vacuum drying chamber, finally with acetone, immersion removes surface PMMA for a long time, is washed repeatedly with deionized water
Sample is washed, 80 DEG C are placed in vacuum drying chamber after drying naturally and is dried 2 hours, then obtains adhering to graphene on a glass
Film.
The Z axis thickness chart of AFM metallographics spectrogram and Fig. 2 from Fig. 1 can be seen that the graphene film prepared by the present invention
Thickness is 1nm or so, and curve fluctuation pattern, shows that prepared graphene thickness is uniform, smooth.
Claims (6)
1. a kind of method that utilization vegetable oil prepares graphene film, it is characterised in that comprise the following steps：
（1）The growth precursors and growth substrate of graphene are placed on to the quartz ampoule heating zone in CVD stoves；（2）Quartz ampoule is close
Seal and highest annealing temperature is simultaneously warming up to 30-50 DEG C/min speed, in the process, the valve opened by one end keeps stone
Pressure in English pipe is an atmospheric pressure；（3）3-5min is kept under highest annealing temperature, then moves sample from heating zone
Remove, and cooled down with 25 DEG C/min speed；（4）Sample after cooling is turned using polymethyl methacrylate auxiliary graphene
Move；（5）Finally with acetone, immersion removes surface PMMA for a long time, with deionized water cyclic washing sample, is placed in after drying naturally
Dried 2-4 hours for 80-90 DEG C in vacuum drying chamber, obtain adhering to graphene film on a glass.
2. according to the method described in claim 1, it is characterised in that the graphene growth precursor is vegetable oil.
3. method according to claim 2, it is characterised in that the vegetable oil is peanut oil, soya-bean oil, linseed oil, castor-oil plant
One or several kinds in oil, rapeseed oil, sesame oil.
4. according to the method described in claim 1, it is characterised in that the growth substrate is polycrystalline nickel foil.
5. according to the method described in claim 1, it is characterised in that the highest annealing temperature is 600-750 DEG C.
6. according to the method described in claim 1, it is characterised in that the polymethyl methacrylate auxiliary graphene transfer refers to
Be to be spun to polymethyl methacrylate on the graphenic surface being grown in above nickel foil, then by sample drying, then will
The nickel foil of bottom, fully to remove, after repeatedly being washed with deionized water, is transferred in substrate of glass with FeCl3 solution corrosions, and
It is dried.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115650600A (en) * | 2022-10-14 | 2023-01-31 | 国家纳米科学中心 | Graphene glass and preparation method thereof |
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| CN115650600B (en) * | 2022-10-14 | 2024-06-25 | 国家纳米科学中心 | Graphene glass and preparation method thereof |
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