CN104120402A - Preparation method of graphene-SiC film - Google Patents
Preparation method of graphene-SiC film Download PDFInfo
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- CN104120402A CN104120402A CN201410391805.3A CN201410391805A CN104120402A CN 104120402 A CN104120402 A CN 104120402A CN 201410391805 A CN201410391805 A CN 201410391805A CN 104120402 A CN104120402 A CN 104120402A
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- Prior art keywords
- graphene
- vacuum chamber
- preparation
- vacuum
- flow
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 8
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 3
- 150000003624 transition metals Chemical class 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 abstract description 21
- 239000004945 silicone rubber Substances 0.000 abstract description 7
- 239000005977 Ethylene Substances 0.000 abstract description 6
- 239000011159 matrix material Substances 0.000 abstract description 6
- 125000000524 functional group Chemical group 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 10
- 239000000463 material Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 1
- 229910001573 adamantine Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a graphene-SiC film, which is characterized by comprising the following steps: with ethylene and silicone rubber as a carbon source and a silicon source respectively, putting a transition metal substrate and the silicone rubber into a vacuum reaction system; under the condition of removing oxygen in the vacuum chamber, keeping the indoor vacuum degree at 1-500Pa, and heating to 600-1,100 DEG C; injecting hydrogen into the vacuum chamber, and injecting the carbon source gas into the vacuum chamber; preserving heat for 1-100 minutes; and cooling at a rate of 10-60 DEG C per minute. The silicone rubber is powder with a particle size of 100-1,000 microns, and is carried in through a gas flow at a supply speed of 1-10g/min. The ethylene flow is 5-100mL/min, and the hydrogen flow is 0-50mL/min. The preparation method is simple in process and can realize large-area growth; the prepared graphene film is very smooth and has controllable resistance; and moreover, since the prepared graphene contains a strong functional group, tight combination with a matrix can be realized.
Description
Technical field
The present invention relates to a kind of preparation method of stone film, particularly relate to a kind of preparation method of Graphene-SiC film.
Background technology
Newcomer in Graphene Shi Tan family, it is the only individual layer bi-dimensional cellular shape crystal of 0.35nm of thickness being formed with the tight storehouse of sexangle cellular by carbon atom.Graphene is that at present known the thinnest material in the world becomes the elementary cell of constituent material, and Graphene is also one of the most solid material, and its physical strength is 100 times of intensity of best in the world steel.Graphene is a kind of semi-conductor that there is no energy gap in addition, and current carrier mobility is therein up to 2 × 10
5cm
2/ V is higher 100 times than electronic mobility in silicon.Graphene also has thermal conductivity the fastest in known materials, and its thermal conductivity can reach 5000Wm
-1k
-1, be adamantine 3 times, also there is the special propertys such as room temperature quantum hall effect and ferromegnetism.Because Graphene has the many merits such as crystalline structure and excellent crystallographic properties workability with low cost of almost Perfect, will there is great application prospect in fields such as electronic information energy and material and biological medicines.
Document " Chinese patent that application number is 200910219530.4 " discloses a kind of photovoltaic cell based on graphene/silicon carbide Schottky junction and preparation method thereof, and the method adopts and directly shifts, gets rid of film, spraying, dipping, filtration, dry method and prepare graphene film the n-Si on itself and basal electrode is combined closely; This photovoltaic cell has the rate of utilization that reduces silicon, feature simple for assembly process, cost is low.But the prior art is only carried out simple blend by Graphene.Therefore blend is prepared into after matrix material the shortcomings such as Presence of an interface adhesive property is poor.
Document [Wenyi Huang, Jianfeng Yu, Kwang Joo Kwak, L James Lee, et al.Adv.Mater.2013,25,4668-4672] report a kind of method of preparing the Graphene that contains strong bond functional group, the method is by controlling function Graphene (GP-SO
3h) content of nanometer paper and silicon rubber makes, and has very strong covalent bonds between prepared Graphene and matrix, and what make it to be combined with silicon wafer is tightr.But function Graphene (GP-SO in the method
3h) the preparation difficulty of nanometer paper is large, cost is high, be not suitable for promoting, and due to its equipment quartz tube furnace that is horizontal structure, the ash content that silicon rubber produces easily affects the quality of Graphene, in the method, the prepared Graphene number of plies and homogeneity is difficult to control simultaneously, and prepared material property is declined.
Summary of the invention
Object of the present invention is intended to overcome graphene film and has the defect poor with basal body interface adhesive property, and a kind of preparation method of Graphene-SiC film of the interface binding power that can effectively improve Graphene and matrix is provided.
For realizing the technical scheme that object of the present invention adopts be: a kind of preparation method of Graphene-SiC film, it is characterized in that adopting ethene and silicon rubber as carbon source and silicon source, transition metal substrate and silicon rubber are placed in to vacuum reaction system, in the situation that removing in vacuum chamber oxygen, maintain indoor vacuum tightness 1-500Pa, and be warming up to 600-1100 DEG C, hydrogen is injected to vacuum chamber, again carbon-source gas is injected to vacuum chamber, keep hydrogen flowing quantity simultaneously, insulation 1-100 minute, rate of temperature fall is 10-60 DEG C/min.Described silicon rubber is powder, and particle size is 100 microns-1000 microns, is written into by air-flow, and feed speed is 1g-10g/min.Ethene flow is 5-100mL/min, and hydrogen flowing quantity is 0-50mL/min.
Beneficial effect of the present invention: 1. technique is simple, can realize large area deposition; 2. prepared graphene film is very smooth, and resistance is controlled, and because prepared Graphene is containing strong functional group, can realizes with matrix and combining closely.
Brief description of the drawings
Fig. 1 prepares Graphene-SiC membrane equipment schematic diagram:
10 is metal substrate;
Fig. 2 is the structural representation of prepared Graphene-SiC film:
20 is matrix; 30 is Graphene-SiC film; 40 is functional group site.
Embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, should understand these embodiment is only not used in and limits the scope of the invention for the present invention is described, after having read the present invention, those skilled in the art all fall within the application's claims to the amendment of the various equivalent form of values of the present invention and limit.
Embodiment 1
As shown in Figure 1, a kind of preparation method of Graphene-SiC film, adopts ethene and silicon rubber as carbon source and silicon source, and nickel metal substrate is placed in to vacuum reaction stove, and silicone rubber powder particle size is 100 microns, is written into by ethylene gas.First maintain indoor vacuum tightness 100Pa, then be warming up to 1000 DEG C, again hydrogen is injected to vacuum chamber, flow is 5mL/min, again ethylene gas is injected to vacuum chamber, flow is 50mL/min, and silicone rubber powder feed speed is 5g/min, be incubated cooling after 10 minutes, rate of temperature fall is 40 DEG C/min.
Embodiment 2
A kind of preparation method of Graphene-SiC film, it is characterized in that adopting ethene and silicon rubber as carbon source and silicon source, copper metal substrate is placed in to vacuum reaction stove, silicone rubber powder particle size is 200 microns, be written into by ethylene gas, maintain indoor vacuum tightness 100Pa, be warming up to 950 DEG C, hydrogen is injected to vacuum chamber, and flow is 10mL/min, then ethylene gas is injected to vacuum chamber, flow is 40mL/min, silicone rubber powder feed speed is 2g/min, is incubated 10 minutes, and rate of temperature fall is 10 DEG C/min.
Above are only two embodiments of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading the scope of protection of the invention.In every case be the content that does not depart from technical solution of the present invention, any type of simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (4)
1. the preparation method of Graphene-SiC film, it is characterized in that adopting ethene and silicon rubber as carbon source and silicon source, transition metal substrate and silicon rubber are placed in to vacuum reaction system, in the situation that removing in vacuum chamber oxygen, maintain indoor vacuum tightness 1-500Pa, and be warming up to 600-1100 DEG C, hydrogen is injected to vacuum chamber, then carbon-source gas is injected to vacuum chamber, keep hydrogen flowing quantity simultaneously, insulation 1-100 minute, rate of temperature fall is 10-60 DEG C/min.
2. the method for preparation according to claim 1, is characterized in that described silicon rubber is powder, and particle size is 100 microns-1000 microns, is written into by air-flow, and feed speed is 1g-10g/min.
3. the method for preparation according to claim 1, is characterized in that described ethene flow is 5-100mL/min.
4. the method for preparation according to claim 1, is characterized in that described hydrogen flowing quantity is 0-50mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410391805.3A CN104120402A (en) | 2014-08-08 | 2014-08-08 | Preparation method of graphene-SiC film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410391805.3A CN104120402A (en) | 2014-08-08 | 2014-08-08 | Preparation method of graphene-SiC film |
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| Publication Number | Publication Date |
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| CN104120402A true CN104120402A (en) | 2014-10-29 |
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| CN201410391805.3A Pending CN104120402A (en) | 2014-08-08 | 2014-08-08 | Preparation method of graphene-SiC film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636557A (en) * | 2021-07-30 | 2021-11-12 | 天津理工大学 | Silicon carbide/graphene anode-cathode composite material and preparation method and application thereof |
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|---|---|---|---|---|
| CN101285175A (en) * | 2008-05-29 | 2008-10-15 | 中国科学院化学研究所 | Method for preparing graphene by chemical vapor deposition |
| CN102001650A (en) * | 2010-12-28 | 2011-04-06 | 上海师范大学 | Method for preparing graphene through chemical vapor deposition under cold cavity wall condition |
| US20110117372A1 (en) * | 2008-03-10 | 2011-05-19 | Tohoku University | Graphene or graphite thin film, manufacturing method thereof, thin film structure and electronic device |
| CN102560414A (en) * | 2012-01-03 | 2012-07-11 | 西安电子科技大学 | Method for preparing graphene on 3C-SiC substrate |
| CN102600775A (en) * | 2012-03-15 | 2012-07-25 | 中国人民解放军国防科学技术大学 | SiC-graphene nano-composite and preparation method thereof |
| WO2014004514A1 (en) * | 2012-06-25 | 2014-01-03 | The Ohio State University | Covalently-bonded graphene coating and its applications thereof |
-
2014
- 2014-08-08 CN CN201410391805.3A patent/CN104120402A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110117372A1 (en) * | 2008-03-10 | 2011-05-19 | Tohoku University | Graphene or graphite thin film, manufacturing method thereof, thin film structure and electronic device |
| CN101285175A (en) * | 2008-05-29 | 2008-10-15 | 中国科学院化学研究所 | Method for preparing graphene by chemical vapor deposition |
| CN102001650A (en) * | 2010-12-28 | 2011-04-06 | 上海师范大学 | Method for preparing graphene through chemical vapor deposition under cold cavity wall condition |
| CN102560414A (en) * | 2012-01-03 | 2012-07-11 | 西安电子科技大学 | Method for preparing graphene on 3C-SiC substrate |
| CN102600775A (en) * | 2012-03-15 | 2012-07-25 | 中国人民解放军国防科学技术大学 | SiC-graphene nano-composite and preparation method thereof |
| WO2014004514A1 (en) * | 2012-06-25 | 2014-01-03 | The Ohio State University | Covalently-bonded graphene coating and its applications thereof |
Non-Patent Citations (1)
| Title |
|---|
| WENYI HUANG ET.AL.: "Atomic Carbide Bonding Leading to Superior Graphene Networks", 《ADVANCED MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636557A (en) * | 2021-07-30 | 2021-11-12 | 天津理工大学 | Silicon carbide/graphene anode-cathode composite material and preparation method and application thereof |
| CN113636557B (en) * | 2021-07-30 | 2023-04-25 | 天津理工大学 | Silicon carbide/graphene positive and negative electrode composite material and its preparation method and application |
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Application publication date: 20141029 |