CN106946241A - The manufacture method of large-area graphene - Google Patents
The manufacture method of large-area graphene Download PDFInfo
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- CN106946241A CN106946241A CN201710061799.9A CN201710061799A CN106946241A CN 106946241 A CN106946241 A CN 106946241A CN 201710061799 A CN201710061799 A CN 201710061799A CN 106946241 A CN106946241 A CN 106946241A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 238000001237 Raman spectrum Methods 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 5
- 239000000956 alloy Substances 0.000 claims description 5
- 229910045601 alloy Inorganic materials 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910017052 cobalt Inorganic materials 0.000 claims description 3
- 239000010941 cobalt Substances 0.000 claims description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 239000011133 lead Substances 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 description 11
- 230000008018 melting Effects 0.000 description 11
- 150000001721 carbon Chemical group 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of manufacture method of large-area graphene, comprise the steps of：A reacting furnace is provided, the reacting furnace is equipped with the solvent of a molten state；Heating the solvent makes the solvent in forming between a high-temperature area and one and the high-temperature area low-temperature region with a temperature difference in the reacting furnace, and the temperature difference is at least 20 DEG C；One carbon source is inserted into the high-temperature area and the solvent is mixed to form an initial soln；And the initial soln flow to the low-temperature region by the high-temperature area and forms a supersaturated solution, and separate out in one large-area graphene of formation on a surface of the supersaturated solution, the number of plies of the large-area graphene is less than 20 layers and with diameters of the La between 1 μm to 1000 μm, and the La systems are by a value obtained by Raman spectrum.By the above method, the large-area graphene with more perfect graphene planes can be produced.
Description
Technical field
The present invention relates to a kind of manufacture method of graphene, espespecially one kind, which can be produced, has more perfect graphene planes
Large-area graphene manufacture method.
Background technology
Graphene is a kind of flat film for being made up of hexangle type honeycomb lattice with SP2 hybridized orbits carbon atom, is mesh
Most thin on former world is also most hard Nanometer material.Because the resistivity of graphene is low, and it is almost transparent, it is expected to use
In developing thinner, the conductive faster electronic component of speed to apply in the fields such as semiconductor, panel or battery.
Even if there is many expectations, also competitively input graphene is studied and is actively laid out, but graphite at this stage for international big factory
Alkene technology also fails to be widely applied, obvious to also have many technical problems to exist at present：Either graphene in itself or
Improved on formula, have more preferably effect when being applied to composite to make graphene.
The content of the invention
The main object of the present invention, is the mode for solving known manufacture graphene, and not only cost of manufacture is high, program is multiple
It is miscellaneous, it is not easy to the problem of large area is produced.
In order to reach above-mentioned purpose, the present invention provides a kind of manufacture method of large-area graphene, comprised the steps of：Carry
For a reacting furnace, the reacting furnace is equipped with the solvent of a molten state；Heating the solvent makes the solvent in forming one in the reacting furnace
There is the low-temperature region of a temperature difference, the temperature difference is at least 20 DEG C between high-temperature area and one and the high-temperature area；By a carbon source
Insert the high-temperature area and be mixed to form an initial soln with the solvent；And the initial soln flow to the low temperature by the high-temperature area
Region and form a supersaturated solution, and separate out on a surface of the supersaturated solution and formed a large-area graphene, should
The number of plies of large-area graphene is less than 20 layers and with diameters of the La between 1 μm to 1000 μm, and the La systems are one by drawing
The value that graceful spectrum is obtained.
Compared to the known method for carrying out volume production graphene with HTHP processing graphite, this method forces the carbon in graphite former
Son is rearranged into plane hexagonal lattice structure, therefore the hexagonal lattice structure of graphene often can not be in graphene planes direction
(La) obtain larger extended distance, and hexagonal ring structure also tend to it is broken can't bear, therefore the interplanar spacing of obtained graphene
(d (0002)) also upper many bigger than theoretical value, causes the physical property of manufactured graphene not as expected.System proposed by the invention
Method is made, the melting solvent forms the high-temperature area and the low-temperature region by the reaction stove heat, makes the initial soln
The supersaturated solution is formed in the low-temperature region and large-area graphene layer is separated out, and is not only reduced processing procedure difficulty, is reduced equipment
Expenditure cost, can also volume production, the shortcoming not only often produced without foregoing known techniques, and can pass through economic simple method system
Produce the large-area graphene with more perfect graphene planes.
Brief description of the drawings
Fig. 1 is the manufacture method flow chart of large-area graphene of the present invention.
Embodiment
Below, collocation schema is described in detail the present invention.
Fig. 1 is refer to, is the manufacture method flow chart of large-area graphene of the present invention, comprises the following steps S1 to S4：
S1：A reacting furnace is provided, the reacting furnace is equipped with the solvent of a molten state.The melting solvent can be iron (Fe), cobalt
(Co), nickel (Ni), lithium (Li), tantalum (Ta), palladium (Pd), platinum (Pt), lanthanum (La), cerium (Ce) or europium (Eu), or its alloy, for example with
Iron, cobalt, nickel or its alloy form the melting solvent, furthermore, in S1, can also be added in the melting solvent inhibitor with
The activity of the melting solvent is reduced, the inhibitor can be selected on demand, golden (Au), silver-colored (Ag), copper (Cu), lead may be selected in citing
(Pb), zinc (Zn), its alloy or above-mentioned any combination.
S2：Heating the solvent makes the solvent in being formed in the reacting furnace between a high-temperature area and one and the high-temperature area
Low-temperature region with a temperature difference, the temperature difference is at least 20 DEG C.In the present embodiment, the reacting furnace can pass through a primary heater
The melting solvent is heated and the high-temperature area is formed, and the melting solvent is heated through a secondary heater and to form this low
Temperature area, makes the high-temperature area have a temperature between 450 DEG C to 1400 DEG C, and the low-temperature region has one less than this
Temperature between 10 DEG C to 100 DEG C of high-temperature area, preferably with the temperature being less than between 20 DEG C to 80 DEG C of the high-temperature area, and
And, the reacting furnace optionally has one to be spaced the high-temperature area and the distance piece of the low-temperature region, and the distance piece is set
It is located at the position of the bottom away from the reacting furnace between the high-temperature area and the low-temperature region in the reacting furnace, and makes the high temperature
Region is connected with the low-temperature region in the part of the bottom close to the reacting furnace, and the part away from the bottom is then separated.
S3：One carbon source is inserted into the high-temperature area to be mixed to form in an initial soln, the present embodiment with the solvent, the reaction
Stove can pass through a feed arrangement and supply the high-temperature area carbon source, and the feed arrangement be arranged on the reacting furnace bottom it is neighbouring should
The position of high-temperature area, thus the carbon source is introduced directly into the high-temperature area, the convection current of the melting solvent is driven, promotes the carbon source
Mix evenly with the melting solvent, but in the present invention, the feed arrangement is not limited with being arranged near the bottom
System, as long as the carbon source can be made to import the high-temperature area.In other embodiment, also the high-temperature area can be carried out simultaneously
Stir to promote the dissolving of the carbon source.In the present invention, the carbon source can be a gaseous carbon sources or a solid carbon source, such as use the gas
Body carbon source, then can be oil gas, hydrocarbon, water-gas etc., such as use the solid carbon source, the solid carbon source can be then
Plastic cement, rubber, carbohydrate, pitch, gasoline, carbon black, graphite, hydrocarbon etc., so when selecting carbonaceous gas as the carbon source,
Such as organic hydrocarbon gas, including methane, ethane or its analog etc., due at high temperature, oxygen easily combined with carbon atom and
Carbon dioxide is formed, can make it that melt solvent is reduced in the phosphorus content of the high-temperature area, causes yield to decline, therefore, in this feelings
Under condition, the feed arrangement can more include a deaerating plant, consequently, it is possible to which the carbon source first removes the oxygen included through the deaerating plant
Composition, then the high-temperature area is given by feed arrangement supply, you can it is prevented effectively from generation yield and declines situation.
S4：The initial soln flow to the low-temperature region by the high-temperature area and forms a supersaturated solution, and separates out in this
A large-area graphene is formed on one surface of supersaturated solution, the number of plies of the large-area graphene is less than 20 layers and with one
Diameters of the La between 1 μm to 1000 μm, the La systems are by a value obtained by Raman spectrum.In the present embodiment, this is first
Beginning solution flow to the low-temperature region by cooling of the high-temperature area through the temperature difference, and forms the supersaturation in the low-temperature region
Solution, when the carbon atom in the supersaturated solution is separated out in the low-temperature region, due to the carbon atom, to compare the supersaturation molten
The density of liquid is come low, the carbon atom separated out can floating to the supersaturated solution the surface, and form the large area graphite
Alkene layer.In other embodiments, in the process for forming large-area graphene layer, still the melting solvent of the reacting furnace is applied
An externally-applied magnetic field is given, consequently, it is possible to the crystal structure that large-area graphene layer will be can control, with expected orientation.
And in large-area graphene layer after being formed on the surface, the present embodiment also can further include step S5：
The reacting furnace is made to collect large-area graphene layer in the low-temperature region with a collection device, here, the collection device can be to set
Be placed in a top of the neighbouring reacting furnace and close to the position of the low-temperature region, and can according to large-area graphene layer an output
Aspect carries out batch collection or continuous collection.
Still need supplementary notes, in order that the large-area graphene layer of institute's output has good lattice structure, should
One temperature range of high-temperature area, a temperature range of the low-temperature region and the scope of the temperature difference, can melt according to used this
Melt and dissolved dose of species carries out appropriate adjustment.But for generally, set the high-temperature area have one using the primary heater as
Align the first center line of benchmark, and the low-temperature region has one second center line, the melting solvent in the reacting furnace, this
One center line has a maximum temperature, and with make it that temperature is gradually reduced away from first center line, and until this is in second
Heart line has a relative low temperature, between the high-temperature area and the low-temperature region, with the change of the temperature difference declined, drives this first
Beginning solution forms the supersaturated solution and separates out the carbon atom to form large-area graphene layer.Wherein, with the side of the present invention
Large-area graphene layer obtained by method, its number of plies is less than 20 layers and size can preferably have a La between 1 μm to 1000 μ
Diameter between m, the La systems are by a value obtained by Raman spectrum.
Above-described embodiment is illustrated only for convenient explanation, and the interest field that the present invention is advocated certainly should be special to apply
It is defined described in sharp scope, rather than is only limitted to above-described embodiment.
Claims (7)
1. a kind of manufacture method of large-area graphene, it is characterised in that comprise the steps of：
A reacting furnace is provided, the reacting furnace is equipped with the solvent of a molten state；
Heat the solvent make the solvent in formed in the reacting furnace between a high-temperature area and one and the high-temperature area have one
The low-temperature region of the temperature difference, the temperature difference is at least 20 DEG C；
One carbon source is inserted into the high-temperature area and the solvent is mixed to form an initial soln；And
The initial soln flow to the low-temperature region by the high-temperature area and forms a supersaturated solution, and separates out molten in the supersaturation
A large-area graphene is formed on one surface of liquid, the number of plies of the large-area graphene is less than 20 layers and with a La between 1 μ
Diameter between m to 1000 μm, the La systems are by a value obtained by Raman spectrum.
2. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that there is the reacting furnace interval to be somebody's turn to do
The distance piece of high-temperature area and the low-temperature region.
3. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that the high-temperature area have one between
Temperature between 450 DEG C to 1400 DEG C.
4. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that the temperature difference is not higher than 80 DEG C.
5. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that the carbon source is first through a deaerating plant
An oxygen composition included is removed, then the high-temperature area is given through feed arrangement supply.
6. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that the solvent be selected from iron, cobalt,
The group that nickel, tantalum, palladium, platinum, lanthanum, cerium, europium and its alloy are constituted.
7. the manufacture method of large-area graphene as claimed in claim 1, it is characterised in that the solvent and one reduces activity
Inhibitor mixed, the inhibitor is the group that is constituted selected from gold, silver, copper, lead, zinc and its alloy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710061799.9A CN106946241A (en) | 2017-01-26 | 2017-01-26 | The manufacture method of large-area graphene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710061799.9A CN106946241A (en) | 2017-01-26 | 2017-01-26 | The manufacture method of large-area graphene |
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| CN106946241A true CN106946241A (en) | 2017-07-14 |
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| CN201710061799.9A Pending CN106946241A (en) | 2017-01-26 | 2017-01-26 | The manufacture method of large-area graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111439743A (en) * | 2020-01-17 | 2020-07-24 | 北京清烯科技有限公司 | Manufacturing method capable of continuously and stably producing large-area graphene |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102143908A (en) * | 2008-07-08 | 2011-08-03 | 宋健民 | Graphene and hexagonal boron nitride flakes and methods relating thereto |
| CN103663434A (en) * | 2012-09-12 | 2014-03-26 | 铼钻科技股份有限公司 | Method and device for mass production of graphene |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
-
2017
- 2017-01-26 CN CN201710061799.9A patent/CN106946241A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102143908A (en) * | 2008-07-08 | 2011-08-03 | 宋健民 | Graphene and hexagonal boron nitride flakes and methods relating thereto |
| CN103663434A (en) * | 2012-09-12 | 2014-03-26 | 铼钻科技股份有限公司 | Method and device for mass production of graphene |
| CN104860298A (en) * | 2015-03-25 | 2015-08-26 | 孙旭阳 | Method for preparing graphene by using molten state reaction bed |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108059153B (en) * | 2018-02-05 | 2021-02-09 | 苏州第一元素纳米技术有限公司 | Synthesizer and method for preparing graphene by synthesizer |
| CN111439743A (en) * | 2020-01-17 | 2020-07-24 | 北京清烯科技有限公司 | Manufacturing method capable of continuously and stably producing large-area graphene |
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