CN107128904A - A kind of method that metal catalytic prepares graphene - Google Patents
A kind of method that metal catalytic prepares graphene Download PDFInfo
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- CN107128904A CN107128904A CN201710330061.8A CN201710330061A CN107128904A CN 107128904 A CN107128904 A CN 107128904A CN 201710330061 A CN201710330061 A CN 201710330061A CN 107128904 A CN107128904 A CN 107128904A
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- C01B2204/00—Structure or properties of graphene
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Abstract
A kind of method that metal catalytic prepares graphene, the present invention relates to grapheme material preparing technical field, the problem of it is in order to solve low using the graphene electrical conductivity of oxidation-reduction method preparation in existing industrial production.Preparation method：After metal material is heated to being completely melt under inert gas shielding, it is passed through after decomposing including inert gas and the gaseous mixture of growth gasses, growth gasses and generates graphene, graphene leaves with air-flow, separate gas, obtain graphene.The method that the present invention is vapor-deposited using growth gasses in the metallic catalyst of molten state, obtain graphene powder, this method, which has, can prepare quality height, the graphene powder that yield conducts electricity very well greatly, the advantages of environment will not being polluted simultaneously, easily realize industrialized production, it is adapted to produce in enormous quantities, the conductance of the graphene prepared can reach 105~106S/m, piece footpath is in 2 μm~1cm.
Description
Technical field
The present invention relates to grapheme material preparing technical field, graphene is prepared in particular to a kind of metal catalytic
Method.
Background technology
The two-dimensional structure material that graphene is made up of cellular single layer of carbon atom；In physical characteristic, it is generally recognized that
The material of more than ten layers of graphene accumulation, is exactly the graphite of three-dimensional structure.CNT is one that tubbiness is rolled into by graphene
Dimension nano material.Graphene has remarkable two-dimentional electricity, optics, calorifics, mechanical property and chemical stability, its uniqueness
Two-dimensional structure and excellent crystallographic characteristics cause it to have important make in fields such as opto-electronic device, sensor and solar energy
With value.Such as, graphene can show quantum hall effect and ballistic transport phenomenon at normal temperatures, can be for preparation room
Warm ballistic transport transistor, is the important foundation new material of Future Information nano-device；The electric transmission speed of graphene is silicon
150 times, be expected to prepare the supper-fast computer that speed surmounts existing level.
At present, the method for preparing powder graphene the most frequently used in industrial production is oxidation-reduction method, is added using graphite
In solution containing strong oxidizer, graphite be oxidized after on interlayer band the group such as carbonyl, hydroxyl, graphite layers is become away from becoming big
For graphite oxide, after graphite oxide is reduced by reducing agent, further further removed using the concentrated sulfuric acid after product is filtered
The oxygen-containing functional group of graphene film layer surface.Pyrolysis reduction, obtains graphene at high temperature.The graphite that this mode is prepared
Alkene, still can contain oxygen-containing functional group after reduction, while graphene has a large amount of defects, can have a strong impact on the electric conductivity of graphene
Energy.Needed to use during oxidation-reduction method in the chemical reagent such as strong oxidizer, such as the potassium permanganate concentrated sulfuric acid, processing procedure
Waste liquid can be polluted to environment.
The content of the invention
The present invention is the waste liquid in order to which the graphene electrical conductivity for solving to use oxidation-reduction method to prepare in existing industrial production is low
The problem of environment being polluted, and a kind of method that metal catalytic prepares graphene is provided.
The method that metal catalytic of the present invention prepares graphene follows these steps to realize：
Metal material is heated under inert gas shielding to be completely melt, then will be by inert gas and carbon source for growth gas
The gaseous mixture of body composition is passed into molten metal, and carbon source for growth gas is reduced in the molten metal obtains graphene and with air-flow
Leave, separated from gas, obtain graphene.
The preparation method of graphene provided by the present invention, using growth gasses in the metallic catalyst of molten state gas phase
The method of deposition, obtains graphene.In the process, reaction environment is protected using inert gas, growth gasses are in melting
Reduction obtains graphene in metal, and graphene overflows with inert gas flow from liquid metal, and graphite is obtained after separation gas
Alkene.This method, which has, can prepare quality height, the graphene powder that yield conducts electricity very well greatly, while will not be polluted to environment
The advantages of.Also, the production equipment needed for this method easily realizes industrialized production, it is adapted to produce in enormous quantities.
Metal catalytic of the present invention prepares the graphene obtained by the method for graphene, and the graphene is 1~5 layer high-quality
Graphene, it is conductive can it is good the advantages of, its conductance can reach 105~106S/m, piece footpath is in 2 μm~1cm, size model
Enclose selection space big.
Compared with prior art, metal catalytic of the present invention prepare graphene method include following beneficial effect：
1st, the method that metal catalytic provided by the present invention prepares graphene, the metal using growth gasses in molten state is urged
The method being vapor-deposited in agent, this method have need not introduce chemical reagent, the performance of graphene will not be produced influence,
Also the advantages of environment will not being impacted.
2nd, metal catalytic provided by the present invention prepares the graphene prepared by the method for graphene, is 1~5 floor height quality
Graphene, it is conductive can it is good the advantages of, its conductance can reach 105~106S/m, piece footpath is in 2 μm~1cm, size
Scope selection space is big.
Brief description of the drawings
Fig. 1 is the graphene lens test chart (TEM) that embodiment 1 is prepared；
Fig. 2 is the graphene lens test chart (TEM) that embodiment 2 is prepared；
Fig. 3 is the Raman spectrogram of Standard graphite alkene and the preparation-obtained graphene of embodiment 1~3；
Fig. 4 is the Raman spectrogram of the preparation-obtained graphene of embodiment 4~7；
Fig. 5 is the process schematic that metal catalytic of the present invention prepares graphene, wherein 1 represents airway tube, 2 represent crucible, 3
Molten metal is represented, 4 represent bubble, and 5 represent graphene.
Embodiment
Embodiment one：The method that present embodiment metal catalytic prepares graphene follows these steps to realize：
Metal material is heated under inert gas shielding to be completely melt, then will be by inert gas and carbon source for growth gas
The gaseous mixture of body composition is passed into molten metal, and carbon source for growth gas is reduced in the molten metal obtains graphene and with air-flow
Leave, separated from gas, obtain graphene.
After present embodiment metal material is heated to being completely melt under inert gas shielding, inert gas and growth are passed through
Graphene is generated after being decomposed including the gaseous mixture of gas, growth gasses, graphene leaves with air-flow, separate gas, obtain graphite
Alkene.
Present embodiment metal catalytic prepares the process schematic of graphene as shown in figure 5, metal material adds in crucible
Heat is to being completely melt, airway tube is inserted into molten metal, and the gaseous mixture being made up of inert gas and carbon source for growth gas passes through
Airway tube is passed into molten metal, when bubble rises to molten metal surface and ruptured, and graphene, which becomes, to fragmentate, so that molten
Melt metal surface and form a layer graphene, be then carried away to collection device with gas.The height of molten metal is 5 wherein in crucible
Centimetre to 40 centimetres.
Embodiment two：Present embodiment is nickel from metal material described unlike embodiment one,
One or more mixtures in cobalt, iron, platinum, copper, aluminium, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc, silver, indium, palladium.Other steps
And parameter is identical with embodiment one.
Present embodiment metal material can also for nickel, cobalt, iron, platinum, copper, aluminium, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc,
Metal alloy compositions between silver, indium, palladium.
Embodiment three：Present embodiment and carbon source for growth gas described unlike embodiment one or two
Body is methane, ethene, acetylene, carbon monoxide, ethanol, ethane, propylene, propane, butane, butadiene, pentane, amylene, benzene and first
One or more mixed gas in benzene.Other steps and parameter are identical with embodiment one or two.
Embodiment four：The inert gas unlike one of present embodiment and embodiment one to three
For nitrogen, helium, argon gas or carbon dioxide.Other steps and parameter are identical with one of embodiment one to three.
Embodiment five：The carbon source for growth unlike one of present embodiment and embodiment one to four
Gas is reduced in the molten metal to be obtained graphene and is left with air-flow, and wherein the temperature of molten metal is 500~1800 DEG C.Its
Its step and parameter are identical with one of embodiment one to four.
The reaction temperature that graphene is generated including present embodiment is 500~1800 DEG C.Growth gasses are carried out under high temperature
Reaction, it is ensured that the quality of prepared graphene.
Embodiment six：Carbon source for growth is controlled unlike one of present embodiment and embodiment one to five
The flow of gas is 50sccm~10000sccm.Other steps and parameter are identical with one of embodiment one to five.
Embodiment seven：Present embodiment is from controlling the flow of inert gas unlike embodiment six
5slm~50slm.Other steps and parameter are identical with embodiment six.
Present embodiment growth gasses and inert gas are passed through according to certain flow proportional, it is ensured that growth gasses are fully also
While former, production efficiency also ensure that.
Embodiment eight：Protected unlike one of present embodiment and embodiment one to seven in inert gas
The process for being heated to being completely melt by metal material under shield is that metal material is added in high-temperature resistant container and heating systems are taken out
Vacuum, is then charged to normal pressure using inert gas, is heated to metal material and is completely melt.Other steps and parameter and specific implementation
One of mode one to seven is identical.
Embodiment nine：Present embodiment is from the vacuum vacuumized unlike embodiment eight
50Pa.Other steps and parameter are identical with embodiment eight.
Embodiment ten：Present embodiment is pottery from the material of high-temperature resistant container unlike embodiment eight
Porcelain, tungsten or graphite.Other steps and parameter are identical with embodiment eight.
The high-temperature resistant container that present embodiment is selected avoids metal from being oxidized or anti-with reaction vessel in fusion process
Should, and catalytic effect is influenceed, so as to influence graphene quality.
Embodiment 11：The graphite obtained unlike one of present embodiment and embodiment one to ten
The piece footpath of alkene is 2 μm~1cm.Other steps and parameter are identical with one of embodiment one to ten.
Embodiment 1：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Copper powder is added in graphite crucible, container vacuum-pumping will be entirely heated, vacuum is 50Pa, then reuses argon gas
Normal pressure is charged to, container is heated, argon gas atmosphere is kept, being warming up to 1100 DEG C is completely melt copper powder；It is passed through methane and argon
Oxygen mixture (flow velocity is methane/argon gas=150sccm/10SLM), the graphene of generation leaves molten metal with air-flow, point
From gas, collection device persistent collection obtains graphene.
Embodiment 2：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Nickel powder is added in ceramic crucible, container vacuum-pumping will be entirely heated, vacuum is 10-3Pa, then reuses argon
Gas is charged to normal pressure, and container is heated, and keeps argon gas atmosphere, being warming up to 1300 DEG C is completely melt nickel powder；Be passed through methane and
Argon gas mixed gas (flow velocity is methane/argon gas=50sccm/20SLM), the graphene of generation leaves molten metal with air-flow, point
From gas, collection device persistent collection obtains graphene.
Embodiment 3：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Nickel cobalt (alloy) powder is added in graphite crucible, container vacuum-pumping will be entirely heated, vacuum is 10-2Pa, then
Reuse helium and be charged to normal pressure, container is heated, keep helium atmosphere, being warming up to 1800 DEG C makes nickel cobalt (alloy) melt completely
Change；Ethene and helium mix gas (flow velocity is ethene/helium=1000sccm/20SLM) are passed through, the graphene of generation is with air-flow
Molten metal is left, gas is separated, collection device persistent collection obtains graphene.
Embodiment 4：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Aluminium powder is added in ceramic crucible, container vacuum-pumping will be entirely heated, vacuum is 0.1Pa, is then reused
Nitrogen is charged to normal pressure, and container is heated, and keeps nitrogen atmosphere, being warming up to 1500 DEG C is completely melt aluminium powder；It is passed through an oxygen
Change carbon and nitrogen mixed gas (flow velocity is carbon monoxide/nitrogen=300sccm/20SLM), the graphene of generation leaves with air-flow
Molten metal, separates gas, and collection device persistent collection obtains graphene.
Embodiment 5：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Tin powder is added in tungsten alloy crucible, container vacuum-pumping will be entirely heated, vacuum is 20Pa, is then reused
Argon gas is charged to normal pressure, and container is heated, and keeps argon gas atmosphere, being warming up to 1200 DEG C is completely melt glass putty；It is passed through ethane
With argon gas mixed gas (flow velocity is ethane/argon gas=500sccm/10SLM), the graphene of generation leaves melting gold with air-flow
Category, separates gas, and collection device persistent collection obtains graphene.
Embodiment 6：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Ferrocobalt powder is added in ceramic crucible, container vacuum-pumping will be entirely heated, vacuum is 10Pa, Ran Houzai
Normal pressure is charged to using helium, container is heated, helium atmosphere is kept, being warming up to 1600 DEG C makes ferrocobalt powder melt completely
Change；Be passed through butadiene and helium mix gas (flow velocity is butadiene/helium=350sccm/20SLM), the graphene of generation with
Air-flow leaves molten metal, separates gas, and collection device persistent collection obtains graphene.
Embodiment 7：The method that the present embodiment metal catalytic prepares graphene follows these steps to implement：
Magnesium alloy powder is added in graphite crucible, container vacuum-pumping will be entirely heated, vacuum is 30Pa, Ran Houzai
Normal pressure is charged to using helium, container is heated, helium atmosphere is kept, being warming up to 1400 DEG C makes magnesium aluminum-alloy powder melt completely
Change；Benzene and helium mix gas (flow velocity is benzene/helium=350sccm/20SLM) are passed through, the graphene of generation leaves with air-flow
Molten metal, separates gas, and collection device persistent collection obtains graphene.
Graphene lens color is tested：
Lens test is carried out to the graphene obtained by embodiment 1 and embodiment 2, as a result as depicted in figs. 1 and 2.Can be with
Graphene powder is clearly seen, and its piece footpath is between 2 μm~1cm.
Graphene conductive performance test：
The electric conductivity of the graphene provided embodiment 1~7 is tested, and the graphite prepared with oxidation-reduction method
Alkene (comparative example) is contrasted.Experimental result is as shown in table 1 below.
The graphene conductive rate test result of table 1
| Sequence number | Conductance (S/m) |
| Embodiment 1 | 3.5×105 |
| Embodiment 2 | 4.8×105 |
| Embodiment 3 | 3.7×105 |
| Embodiment 4 | 6.5×105 |
| Embodiment 5 | 4.5×105 |
| Embodiment 6 | 7.1×105 |
| Embodiment 7 | 3.9×105 |
| Comparative example | 4800 |
Test result indicates that, the method for preparing graphene provided herein, due to it is no introducing oxygen-containing functional group and
Defect is very low, conducts electricity very well.Graphene electrical conductivity prepared by oxidation-reduction method is prepared in 3000-5000S/m or so, this method
Graphene powder bulk conductivity 105~106More than S/m.
Graphite Raman spectrum test：
The graphene provided embodiment 1~7 can carry out Raman spectrum test, and test result is as shown in Figure 3 and Figure 4.
Wherein, it is the Raman for the graphene that graphene standard Raman spectroscopy and embodiment 1,2,3 are provided successively from bottom to up in Fig. 1
Spectrum；It is the Raman spectrum for the graphene that embodiment 4,5,6,7 is provided successively from bottom to up in Fig. 2.
Test result indicates that, the method that metal catalytic provided by the present invention prepares graphene can prepare high-quality stone
Black alkene.
In summary, the method that a kind of metal catalytic provided by the present invention prepares graphene, using growth gasses in melting
The method being vapor-deposited in the metallic catalyst of state, obtains graphene powder, and this method is led greatly with that can prepare quality height, yield
The graphene powder of good electrical property, while the advantages of will not being polluted to environment.Also, the production equipment needed for this method is held
Industrialized production easily is realized, is adapted to produce in enormous quantities.Prepared graphene, is 1~5 layer of high-quality graphene, with leading
The advantages of good electrical property, its conductance can reach 105~106S/m, piece footpath is in 2 μm~1cm, and size range selection space is big.
Claims (9)
1. a kind of method that metal catalytic prepares graphene, it is characterised in that this method is to realize through the following steps：
Metal material is heated under inert gas shielding to be completely melt, then will be by inert gas and carbon source for growth gas group
Into gaseous mixture be passed into molten metal, carbon source for growth gas reduce in the molten metal obtain graphene and with air-flow from
Open, separated from gas, obtain graphene.
2. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that described metal material
Expect for one or more mixtures in nickel, cobalt, iron, platinum, copper, aluminium, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc, silver, indium, palladium.
3. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that described carbon source life
Long gas is methane, ethene, acetylene, carbon monoxide, ethanol, ethane, propylene, propane, butane, butadiene, pentane, amylene, benzene
With one or more mixed gas in toluene.
4. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that the inert gas
For nitrogen, helium, argon gas or carbon dioxide.
5. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that the carbon source for growth
Gas is reduced in the molten metal to be obtained graphene and is left with air-flow, and wherein the temperature of molten metal is 500~1800 DEG C.
6. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that control carbon source for growth
The flow of gas is 50sccm~10000sccm.
7. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that control inert gas
Flow be 5slm~50slm.
8. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that protected in inert gas
The process for being heated to being completely melt by metal material under shield is that metal material is added in high-temperature resistant container and heating systems are taken out
Vacuum, is then charged to normal pressure using inert gas, is heated to metal material and is completely melt.
9. the method that a kind of metal catalytic according to claim 1 prepares graphene, it is characterised in that obtained graphene
Piece footpath be 2 μm~1cm.
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| CN108059153A (en) * | 2018-02-05 | 2018-05-22 | 苏州第元素纳米技术有限公司 | A kind of synthesizer and its method for preparing graphene |
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