CN103668447B - A kind of preparation has the identical or preparation facilities of closer crystal lattice orientation Graphene and method - Google Patents
A kind of preparation has the identical or preparation facilities of closer crystal lattice orientation Graphene and method Download PDFInfo
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- CN103668447B CN103668447B CN201210328087.6A CN201210328087A CN103668447B CN 103668447 B CN103668447 B CN 103668447B CN 201210328087 A CN201210328087 A CN 201210328087A CN 103668447 B CN103668447 B CN 103668447B
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Abstract
The present invention relates to a kind of preparation there is the identical or preparation facilities of closer crystal lattice oriented single crystal Graphene and method.First at monocrystalline silicon surface by the standby metal of the method (sample temperature is 196 DEG C to 250 DEG C) of low-temperature epitaxy (copper, aluminium, etc.) monocrystalline or pseudo-crystal film (thickness is 1nm 500 μm).Then (CVD) mode is deposited by graphene growth to metal film surfaces by chemical gaseous phase.CVD process sample temperature is 600 1100 degrees Celsius, and vacuum is 10 10mbar to 2bar.Then sample is cooled to room temperature.So having the orientation of base silicon monocrystalline due to metallic film, same Graphene has the crystal orientation of metallic film.Prepared Graphene has single crystalline nature.Size is only limited by the size of silicon single crystal.Size is up to several tens cm.
Description
Technical field
The invention discloses and a kind of preparation there is the identical or preparation facilities of closer crystal lattice orientation Graphene and method.More
Body ground, relate to a kind of have cheap, step simple, etc. feature large scale, there is identical or closer crystal lattice orientation, high-quality
The preparation equipment of Graphene and method, belong to electric thin Material Field.
Background technology
Since within 2004, being prepared single-layer graphene for the first time by Novoselov and Gein, various kinds are born it
The method preparing Graphene.Chemical vapour deposition technique (Nature 457 (7230): 706.) is considered as to be hopeful at present most system
For large area, the method for the graphene film of high-quality.But due to metallic film is generally polycrystalline, the graphite grown thereon
Alkene does not the most have any orientation.The Graphene farmland of different orientation can form domain boundary in junction, reduces the matter of graphene film
Amount.Utilize metal single crystal substrate to prepare and there is the graphene film that approximation is single-orientated.But the price of metal single crystal is non-
Chang Gao, thus improve and there is the single or manufacturing cost of approximation oriented single crystal graphene film.
Summary of the invention
In order to overcome the difficulty of prior art, the invention provides following technical scheme:
1. prepare there is the identical or preparation facilities of closer crystal lattice oriented single crystal Graphene and method for one kind.Its feature exists
In, this system is by (1) substrate heater, (2) substrate cooling device, (3) substrate monocrystalline silicon, (4) vacuum pump system, (5) gas
Bottle group, (6) gas circuit and control valve, (7) vacuum chamber and (8) source metal composition.Vacuum pump system (4) keeps the low of vacuum chamber (7)
Air pressure.Under environment under low pressure, the base material monocrystalline silicon (3) of cleaning is cooled down by cooling device (2).Source metal (8) is utilized to exist
It is deposited with monocrystalline, pseudo-crystal in the base silicon of cooling or there is the metallic film of closer crystal lattice orientation.When thickness of metal film reaches to want
Stop metal evaporation after asking and utilize heater (1) to promote base reservoir temperature to chemical gaseous phase depositing temperature.By gas circuit and control
Valve processed (6) regulates gas componant and air pressure that gas cylinder group (5) supplied in vacuum chamber to complete the growth of Graphene.Finally
Reduce substrate (3) temperature and take out from vacuum chamber (7).
2. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that described catalytic metal source (8)
The metal of middle energy evaporation is: copper (Cu), aluminium (Al), nickel (Ni), cobalt (Co), iron (Fe), platinum (Pt), gold (Au), chromium (Cr), magnesium
(Mg), a kind of or the most two or more in manganese (Mn), molybdenum (Mo), ruthenium (Ru), tantalum (Ta), titanium (Ti), rhodium (Rh) and tungsten (W)
Combination.Evaporation form can be: the one in thermal evaporation, magnetron sputtering, chemical gaseous phase deposition or any combination.
3. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that described gaseous carbon source is each
Gas molecule contains the gas of 1～8 carbon atom.
4. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that described heater (1) can
Think resistance heating, thermoelectron bombardment, electromagnetic wave heating, LASER HEATING, in one or any combination.
5. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that the gas in described gas cylinder group (5)
Body can be hydrocarbon, hydrogen (H2), oxygen (O2), nitrogen (N2), argon gas (Ar), helium (He), in neon (Ne) one
Kind or the most two or more combinations.
6. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that described vacuum pump system (4) can
Think combinations a kind of or the most two or more in molecular pump, ionic pump, mechanical pump, diffusion pump.
7. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that the metallic film of described growth is
Monocrystalline, pseudo-crystal or have closer crystal lattice orientation metallic film.
8. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that the graphene film of described growth
There is approximation or identical crystal lattice orientation.
9. the closer crystal lattice orientation that the Graphene described in explanation 8 is had, it is characterised in that the rotation between different farmlands
Differential seat angle is less than 10 °.
10. preparation facilities and the method for the Graphene described in 1 are described, it is characterised in that described vacuum chamber (7) can be
Any materials and shape.Other annexes can be installed.As long as meeting the vacuum environment ensured in metal thin film growth process.
The preparation facilities of the Graphene described in 11. explanations 1 and method, it is characterised in that the cleaning of described base silicon (3)
Process includes any process that silicon face can be made to show lattice structure.Such as, the high annealing in vacuum chamber (7), or
Person is in the outer Chemical cleaning of vacuum chamber (7).
It is an advantage of the invention that owing to silicon substrate is less expensive monocrystalline.Its price general is far smaller than same area gold
Belong to monocrystalline.Utilize the crystal lattice orientation that it is single to guide the orientation of metallic film thereon.Then the list of metallic film is utilized
The crystal lattice orientation of one guides the taxis on it by the Graphene of chemical vapor deposition growth.Thus reach cheap system
Standby identical or closer crystal lattice is orientated the purpose of Graphene.
Accompanying drawing explanation
Accompanying drawing is for providing a further understanding of the present invention, and constitutes a part for specification, is not intended that this
The restriction of invention.
In the accompanying drawings:
Fig. 1 is that preparation disclosed in this invention has the identical or preparation facilities of closer crystal lattice orientation Graphene and technique
Schematic flow sheet.
Fig. 2 is the enlarged drawing of cooling device；
Fig. 3 is the enlarged drawing of heater；
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
As it is shown in figure 1, the present invention is to have identical or the preparation facilities of closer crystal lattice orientation Graphene, this dress a kind of preparation
Put main by (1), substrate heater (2), substrate cooling device (3), substrate monocrystalline silicon (4), vacuum pump system (5), gas cylinder
Group (6), gas circuit and control valve (7), vacuum chamber (8), source metal composition.
Production procedure is: place monocrystal silicon substrate (3) in vacuum chamber (7).This substrate can utilize chemistry before placement
Method is cleaned.Vacuum pump system (5) is utilized to keep the low pressure of vacuum chamber (7).If substrate (3) is not yet cleaned, it is possible to use
Heater (1) carries out high-temperature heating to substrate (3), thus cleans its surface.Under environment under low pressure, cooling device (2) is to cleaning
Base material monocrystalline silicon (3) cool down.Chilling temperature is-196 DEG C to-250 DEG C.Utilize source metal (8) at the base of cooling
It is deposited with monocrystalline, pseudo-crystal on end silicon or there is the metallic film of closer crystal lattice orientation.Stop after thickness of metal film reaches requirement
Metal evaporation.Evaporation thickness of metal film be thickness be 1nm-500 μm.Heater (1) is utilized to promote base reservoir temperature to chemistry
Vapour deposition temperature.Now base reservoir temperature is 600 DEG C-1100 DEG C.By gas circuit and control valve (7) regulate gas cylinder group (6) to
The gas componant supplied in vacuum chamber and air pressure are to complete the growth of Graphene.Air pressure is 10-10mbar to 2bar.Finally drop
Low substrate (4) temperature is also taken out from vacuum chamber (8).
As in figure 2 it is shown, cooling device includes: (1) metal dish, (2) metal cooling-pipe form.Liquid nitrogen can be by metal tube
(2) entrance (3) flows into and then flows out through outlet (4).Thus reach to cool down the purpose of (1) of metal dish.
As it is shown on figure 3, heater includes: (1) metal dish, (2) resistance metal silk form.Electric current is through wire (2)
Produce heat radiation metal dish (1) thus heat metal dish (1).Height can also be added between wire (2) and metal dish (1)
Pressure.Thermoelectron bombardment metal dish (1) utilizing wire (2) to be launched heats.
Last it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to
The present invention, although the present invention being described in detail with reference to previous embodiment, for a person skilled in the art, its
Still the technical scheme described in foregoing embodiments can be modified, or wherein portion of techniques feature is equal to
Replace.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (10)
1. prepare there is the identical or device of closer crystal lattice oriented single crystal Graphene for one kind, it is characterised in that this device is by substrate
Heater (1), substrate cooling device (2), substrate monocrystalline silicon (3), vacuum pump system (4), gas cylinder group (5), gas circuit and control
Valve (6), vacuum chamber (7) and source metal (8) composition.
2. prepare there is the identical or method of closer crystal lattice oriented single crystal Graphene for one kind, it is characterised in that vacuum pump system (5)
Keep the low pressure of vacuum chamber (7), utilize cooling device (2) to carry out cold to the substrate monocrystalline silicon (3) of cleaning under environment under low pressure
But, chilling temperature is-196 DEG C to-250 DEG C, utilizes source metal (8) be deposited with monocrystalline, pseudo-crystal in the base silicon of cooling or have
The metallic film of closer crystal lattice orientation, stops metal evaporation after thickness of metal film reaches requirement, utilizes heater (1) to carry
Rise base reservoir temperature temperature required to chemical gaseous phase deposition, and be passed through gaseous carbon source to vacuum chamber (7), utilize gas circuit and control valve
(6) regulate the gas componant supplied and air pressure, at high temperature complete the graphene film growth in metal substrate surface, finally
Reduce base reservoir temperature and take out from vacuum chamber (7).
Preparation the most according to claim 1 has the identical or device of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, described vacuum pump system (4) is combination a kind of or the most two or more in molecular pump, ionic pump, mechanical pump, diffusion pump.
Preparation the most according to claim 1 has the identical or device of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, described heater is the one in resistance heating, thermoelectron bombardment, electromagnetic wave heating, LASER HEATING or any combination.
Preparation the most according to claim 1 has the identical or device of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, described vacuum chamber (7) is any materials and shape, can be provided with other annexes, as long as can guarantee that metallic film grew
Vacuum environment in journey.
Preparation the most according to claim 2 has the identical or method of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, the cleaning process of described substrate monocrystalline silicon includes any process making silicon face show lattice structure, described cleaning process
For the high annealing in vacuum chamber (7), or in vacuum chamber (7) Chemical cleaning outward.
Preparation the most according to claim 2 has the identical or method of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, the metal being deposited with in described catalytic metal source is: copper (Cu), aluminium (Al), nickel (Ni), cobalt (Co), iron (Fe), platinum
(Pt), in gold (Au), chromium (Cr), magnesium (Mg), manganese (Mn), molybdenum (Mo), ruthenium (Ru), tantalum (Ta), titanium (Ti), rhodium (Rh) and tungsten (W)
A kind of or the most two or more combinations, evaporation form be thermal evaporation, magnetron sputtering, chemical gaseous phase deposition in one or appoint
Meaning combination.
Preparation the most according to claim 2 has the identical or method of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, described gaseous carbon source is the gas in each gas molecule containing 1～8 carbon atom.
Preparation the most according to claim 2 has the identical or method of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, described gas componant is hydrocarbon, hydrogen (H2), oxygen (O2), nitrogen (N2), argon gas (Ar), helium (He), neon
(Ne) a kind of or the most two or more combination in.
Preparation the most according to claim 2 has the identical or method of closer crystal lattice oriented single crystal Graphene, and its feature exists
In, the graphene film of described growth has approximation or identical crystal lattice orientation, and the anglec of rotation difference between different farmlands is less than 10 °.
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| CN201210328087.6A CN103668447B (en) | 2012-09-01 | 2012-09-01 | A kind of preparation has the identical or preparation facilities of closer crystal lattice orientation Graphene and method |
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| CN105439126B (en) * | 2014-09-01 | 2017-12-22 | 华北电力大学 | A kind of grade single crystal graphene preparation method |
| CN108059367A (en) * | 2017-11-29 | 2018-05-22 | 吉林云亭石墨烯技术股份有限公司 | A kind of preparation and application of CVD graphenes compound glass |
| CN110501583B (en) * | 2019-04-29 | 2021-09-28 | 南京大学 | Method for calculating crystal lattice orientation and domain turnover angle of polycrystalline ferroelectric material domain |
| CN111883761A (en) * | 2020-08-05 | 2020-11-03 | 重庆信合启越科技有限公司 | Silicon graphene composite lithium battery negative electrode material and preparation method thereof |
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| JP2009091174A (en) * | 2007-10-04 | 2009-04-30 | Univ Of Fukui | Method for producing graphene sheet |
| CN102212794A (en) * | 2011-04-13 | 2011-10-12 | 中国科学院上海微***与信息技术研究所 | Copper plating substrate-based method for preparing large-area graphene film |
| CN102260858A (en) * | 2010-05-26 | 2011-11-30 | 中国科学院物理研究所 | Method for directly growing graphine on various substrates |
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| JP5453045B2 (en) * | 2008-11-26 | 2014-03-26 | 株式会社日立製作所 | Substrate on which graphene layer is grown and electronic / optical integrated circuit device using the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009091174A (en) * | 2007-10-04 | 2009-04-30 | Univ Of Fukui | Method for producing graphene sheet |
| CN102260858A (en) * | 2010-05-26 | 2011-11-30 | 中国科学院物理研究所 | Method for directly growing graphine on various substrates |
| CN102212794A (en) * | 2011-04-13 | 2011-10-12 | 中国科学院上海微***与信息技术研究所 | Copper plating substrate-based method for preparing large-area graphene film |
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| DBD等离子体制备石墨烯薄膜结构和性能研究;董良旭;《中国优秀硕士论文全文数据库（工程科技I辑）》;20110115;第B020-461页 * |
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Effective date of registration: 20170711 Address after: 213149 No. 6 Xiangyun Road, Wujin, Jiangsu, Changzhou Patentee after: Changzhou into a new Mstar Technology Ltd Address before: Tianning District 213000 Jiangsu city of Changzhou province Wu Road Luxuries Lanling Building 8 unit 1002 Patentee before: Dong Guocai |
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Address after: 213149 No. 6 Xiangyun Road, Wujin, Jiangsu, Changzhou Patentee after: Guocheng instrument (Changzhou) Co., Ltd Address before: 213149 No. 6 Xiangyun Road, Wujin, Jiangsu, Changzhou Patentee before: CHANGZHOU GUOCHENG NEW MATERIAL TECHNOLOGY Co.,Ltd. |
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