CN109485035A - A kind of double-deck or three layers of graphene preparation method - Google Patents
A kind of double-deck or three layers of graphene preparation method Download PDFInfo
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- CN109485035A CN109485035A CN201811338738.3A CN201811338738A CN109485035A CN 109485035 A CN109485035 A CN 109485035A CN 201811338738 A CN201811338738 A CN 201811338738A CN 109485035 A CN109485035 A CN 109485035A
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- metal foil
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- 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
Abstract
The invention discloses double-deck or three layers of graphene preparation methods, are growth preparation system with chemical gas-phase deposition system, and copper or corronil foil are that growth substrates carry out the uniform double-deck and three layers of graphene of growing large-area；And the metal foil substrate is placed in a confinement space, this confinement space is realized that double-deck or three layers of graphene can be by vapor deposition growth in metal foil substrate by another same metal foil folding or the metal foil pocket being curled into or metal foil tube；For grow graphene gas source be methane, ethylene or acetylene and hydrogen, 900-1050 DEG C of growth temperature；Growth time 30-600 minutes；System pressure range is from 0.1Torr to atmospheric pressure.
Description
Technical field
The present invention relates to a kind of preparation method of grapheme material, especially double-deck and three layers of graphene preparation methods.
Background technique
Graphene is the monoatomic layer carbon material of SP2 hydridization, and carrier mobility is more than 10,000cm at room temperature2V-1s-1,
Two orders of magnitude higher than the mobility of the silicon in conventional microelectronic circuit, therefore graphene may in following electronic device
It plays a significant role.However graphene is the semimetal of zero band gap, it means that graphene electronic device cannot achieve complete pass
Closed state, this is the intrinsic defect that graphene realizes application in person in electronics, can not still be solved at present.
The three layers of graphene and single-layer graphene of bilayer and " ABC stacking " with " AB stacking " only differ in structure
1-2 layers of carbon atom, theoretical and experiment is it has been found that if apply one on the device being processed by double-deck and three layers of graphene
When a electrostatic field perpendicular to its channel plane, graphene can open one 250 milli in the case where keeping its high mobility
The band gap of electron-volt, this makes double-deck and three layers of graphene just have very much prospect in the application of person in electronics.It is double-deck
Or multi-layer graphene preparation is the hot issue of research.
Summary of the invention
Object of the present invention is to using chemical gas-phase deposition system as growth apparatus, copper foil or corronil foil are growth substrates
Carry out the uniform double-deck and three layers of graphene of growing large-area.
The technical scheme is that double-deck or three layers of graphene preparation method, are growth with chemical gas-phase deposition system
Preparation system, metal foil (copper or corronil foil) are that growth substrates carry out the uniform double-deck and three layers of stone of growing large-area
Black alkene；And the metal foil substrate is placed in a confinement space, this confinement space is rolled over by another same metal foil
The folded or metal foil pocket that is curled into or metal foil tube realize (specific structure is see schematic diagram), double-deck or three layers of graphite
Alkene can be by vapor deposition growth on same metal foil substrate (copper foil or corronil foil etc.)；For growing graphene
Gas source be methane, ethylene or acetylene and hydrogen, 900-1050 DEG C of growth temperature；Growth time 30-600 minutes；System pressure
Range is from 0.1Torr to atmospheric pressure.
Metal foil pocket is in communication with the outside in the gap that interface has；Metal tube confinement space is connected by both ends and the external world
Logical, growth substrates are placed in the inside of pocket or pipe.
System pressure range (regulates and controls the pressure in growing system by argon gas) from 0.1Torr to atmospheric pressure.
And the metal foil growth substrates are placed in the metal foil pocket or metal foil tube being made by another metal foil,
Double-deck or three layers of graphene can be by being vapor-deposited on growth substrates copper foil；As shown below.
The utility model has the advantages that the present invention, using chemical gas-phase deposition system as growth apparatus, metal foil is to grow up in growth substrates next life
The uniform double-deck and three layers of graphene of area.The bilayer of growth on metal foil and three layers of graphene can be used as field effect
The channel material for answering transistor realizes the graphene field effect device of high on-off ratio.
Detailed description of the invention
Fig. 1 is the schematic diagram of growth substrates of the invention；The front view of Fig. 1 (a) metal foil pocket；(b) metal foil pocket
Sectional view；(c) front view of metal tube；(d) sectional view of metal tube
Note: being the sectional view of metal foil pocket shown in (b), in practical growth course, copper pocket side is not cut
It opens.
Fig. 2 and Fig. 3 is the photo of two layers and three layers graphene on copper foil substrate.
Specific embodiment
Fig. 1 is the photo that metal foil growth substrates are respectively placed in the pocket or metal tube that are made by another metal foil,
Arrow is that (typically copper or corronil, wherein in corronil 20%) mass percent of nickel is not higher than substrate metal foil
Carry out the uniform double-deck and three layers of graphene of growing large-area for growth substrates；And the metal foil growth substrates are placed in
In one confinement space, this confinement space is rolled over by another same metal foil or piece (typically copper or corronil)
The pocket built up or the metal tube being curled into are realized.Metal foil pocket has the gap of several hundred nano-widths and outer in interface
Boundary's connection；Or metal tube confinement space is in communication with the outside by both ends.Schematic diagram is as follows.
Double-deck or three layers of graphene are being placed in metal foil pocket or in metal foil tube by chemical vapor deposition growth
Metal foil substrate surface；For growing the gas source of graphene by methane (methane can be replaced by ethylene or acetylene) and hydrogen,
900-1050 DEG C of growth temperature；Growth time 30-600 minutes；System pressure range is from 0.1Torr to atmospheric pressure.It needs exist for
It is emphasised that the feature of the bilayer/tri- layer graphene obtained using copper foil or corronil foil is similar.
Metal foil or the size of the pocket of piece preparation, the pipe of metal foil or piece preparation and metal foil substrate are only by growing system
Size determine, that is to say, that small growth substrates can only be accommodated in small system, big system space can accommodate big ruler
Very little growth substrates.
More specific growth conditions: the gas source of growth gasses be methane and hydrogen, about 900-1050 DEG C of growth temperature；
Growth time 30-600 minutes；System pressure about 0.1Torr is to atmospheric pressure.The flow volume of methane and hydrogen ratio is 0.1:1-
100:1；Copper foil or corronil foil surface in pocket and pipe can be with growing large-area monocrystalline bilayers and three layers of graphene.
The pressure (pressure) in growing system is separately adjusted by argon gas.
25-100 microns of metal foil thickness, purity 99.8%；Corronil etc. also has similar effect；Can also it grow.System
The metal foil thickness range for making metal foil pocket is 25 microns to 100 microns；
Growing system pressure 0.1Torr, higher or lower pressure also have similar effect, but it is common to need other parameters
Cooperation；
900-1050 degrees Celsius of growth temperature；Growth time 30-600 minutes；
Gas source is hydrogen, methane, and argon gas is used to regulator control system integral pressure, and hydrogen flowing quantity 0-500 standard cubic centimeter is every
Minute (s.c.c.m), methane flow 0-100s.c.c.m.
Bilayer graphene film average-size is greater than 200 microns (diameter), and three layers of graphene film average-size are greater than 200
Micron (diameter).
Double-deck or three layers of graphene can be by being vapor-deposited in growth substrates metal foil；
Copper or corronil foil.
Single layer on substrate in Fig. 2, two layers, three layers graphene growth conditions, that is, design parameter of photo obtain.
Fig. 3 be single layer on copper foil substrate, two layers and three layers graphene photo growth conditions it is i.e. specific by embodiment
Gain of parameter.SLG refers to that single-layer graphene, BLG refer to bilayer graphene in figure, and TLG refers to three layers of graphene.
Claims (6)
1. double-deck or three layers of graphene preparation method, characterized in that with chemical gas-phase deposition system be growth preparation system, copper or
Corronil foil is that growth substrates carry out the uniform double-deck and three layers of graphene of growing large-area；And the metal foil substrate is put
Be placed in a confinement space, metal foil pocket that this confinement space is folded or is curled by another same metal foil or
Metal foil tube realizes that double-deck or three layers of graphene can be by vapor deposition growth in metal foil substrate；For growing stone
The gas source of black alkene be methane, ethylene or acetylene and hydrogen, 900-1050 DEG C of growth temperature；Growth time 30-600 minutes；System
Pressure range is from 0.1Torr to atmospheric pressure.
2. double-deck or three layers of graphene preparation method according to claim 1, characterized in that metal foil pocket is in interface
It has the gap and is in communication with the outside；Metal tube confinement space is in communication with the outside by both ends.
3. double-deck or three layers of graphene preparation method according to claim 1 or 2, characterized in that by another metal foil
Pocket or the metal tube being curled into the metal foil pocket or metal foil tube being made into.
4. double-deck or three layers of graphene preparation method according to claim 1 or 3, characterized in that the stream of methane and hydrogen
Amount volume ratio is 0.1:1-1:100.
5. double-deck or three layers of graphene preparation method according to claim 1 or 3, characterized in that regulated and controled by argon gas
Pressure in growing system.
6. double-deck or three layers of graphene preparation method according to claim 1 or 3, characterized in that substrate is copper foil or copper
Nickel alloy foil.
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| CN201811338738.3A CN109485035A (en) | 2018-11-12 | 2018-11-12 | A kind of double-deck or three layers of graphene preparation method |
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| CN201811338738.3A CN109485035A (en) | 2018-11-12 | 2018-11-12 | A kind of double-deck or three layers of graphene preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106549A (en) * | 2019-05-21 | 2019-08-09 | 电子科技大学 | A kind of growing method of multi-layer graphene monocrystal thin films |
| CN111606323A (en) * | 2020-06-17 | 2020-09-01 | 南方科技大学 | Three-layer graphene and preparation method thereof |
| CN112429724A (en) * | 2020-12-31 | 2021-03-02 | 南通晶锐新型碳材料科技有限公司 | Preparation method of five-layer graphene |
| CN112919454A (en) * | 2021-01-29 | 2021-06-08 | 南京大学 | Method for controlling stacking angle of double-layer graphene |
| CN113106417A (en) * | 2021-03-30 | 2021-07-13 | 西安电子科技大学 | Preparation method of hexagonal boron nitride film and hexagonal boron nitride film |
| CN115806288A (en) * | 2022-12-19 | 2023-03-17 | 南京大学 | Method for promoting secondary growth of graphene and application of method in preparation of double-layer graphene |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130089666A1 (en) * | 2011-10-07 | 2013-04-11 | International Business Machines Corporation | Substrate Holder for Graphene Film Synthesis |
| CN103466609A (en) * | 2013-09-25 | 2013-12-25 | 电子科技大学 | Preparation method of double-layer graphene films |
| US20140312421A1 (en) * | 2013-03-15 | 2014-10-23 | University Of Southern California | Vapor-Trapping Growth of Single-Crystalline Graphene Flowers |
| KR20150106984A (en) * | 2014-03-12 | 2015-09-23 | 재단법인 나노기반소프트일렉트로닉스연구단 | Method for preparing graphene using overlapping and method for fabricating electronics comprising the graphene |
| CN105779964A (en) * | 2016-05-23 | 2016-07-20 | 中国科学院上海微系统与信息技术研究所 | Metal vapor-assisted preparation method of fast-growing few-layer graphene |
| CN108706574A (en) * | 2018-07-11 | 2018-10-26 | 无锡市惠诚石墨烯技术应用有限公司 | A method of the copper-based multi-layer graphene of growth |
-
2018
- 2018-11-12 CN CN201811338738.3A patent/CN109485035A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130089666A1 (en) * | 2011-10-07 | 2013-04-11 | International Business Machines Corporation | Substrate Holder for Graphene Film Synthesis |
| US20140312421A1 (en) * | 2013-03-15 | 2014-10-23 | University Of Southern California | Vapor-Trapping Growth of Single-Crystalline Graphene Flowers |
| CN103466609A (en) * | 2013-09-25 | 2013-12-25 | 电子科技大学 | Preparation method of double-layer graphene films |
| KR20150106984A (en) * | 2014-03-12 | 2015-09-23 | 재단법인 나노기반소프트일렉트로닉스연구단 | Method for preparing graphene using overlapping and method for fabricating electronics comprising the graphene |
| CN105779964A (en) * | 2016-05-23 | 2016-07-20 | 中国科学院上海微系统与信息技术研究所 | Metal vapor-assisted preparation method of fast-growing few-layer graphene |
| CN108706574A (en) * | 2018-07-11 | 2018-10-26 | 无锡市惠诚石墨烯技术应用有限公司 | A method of the copper-based multi-layer graphene of growth |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110106549A (en) * | 2019-05-21 | 2019-08-09 | 电子科技大学 | A kind of growing method of multi-layer graphene monocrystal thin films |
| CN111606323A (en) * | 2020-06-17 | 2020-09-01 | 南方科技大学 | Three-layer graphene and preparation method thereof |
| CN112429724A (en) * | 2020-12-31 | 2021-03-02 | 南通晶锐新型碳材料科技有限公司 | Preparation method of five-layer graphene |
| CN112919454A (en) * | 2021-01-29 | 2021-06-08 | 南京大学 | Method for controlling stacking angle of double-layer graphene |
| CN112919454B (en) * | 2021-01-29 | 2023-10-13 | 南京大学 | Method for controlling stacking angle of double-layer graphene |
| CN113106417A (en) * | 2021-03-30 | 2021-07-13 | 西安电子科技大学 | Preparation method of hexagonal boron nitride film and hexagonal boron nitride film |
| CN115806288A (en) * | 2022-12-19 | 2023-03-17 | 南京大学 | Method for promoting secondary growth of graphene and application of method in preparation of double-layer graphene |
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Application publication date: 20190319 |