CN108862253A - A kind of graphene growth method based on multilayer and large-area graphene growth quartz boat - Google Patents
A kind of graphene growth method based on multilayer and large-area graphene growth quartz boat Download PDFInfo
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- CN108862253A CN108862253A CN201810781188.6A CN201810781188A CN108862253A CN 108862253 A CN108862253 A CN 108862253A CN 201810781188 A CN201810781188 A CN 201810781188A CN 108862253 A CN108862253 A CN 108862253A
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- quartz
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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]
Abstract
The invention belongs to the technical fields of graphene growth, more particularly to based on graphene growth with one layer, multilayer, the graphene growth method of the Multifunctional supportings platform such as roll-to-roll, the platform includes quartz tubular boat, quartzy plate and quartzy sliding block；The quartz tubular boat is tubulose madreporic canal, and outer diameter is less than the quartzy bore of growth, and metal foil winding can be used in its quartz tubular boat outer wall, realizes the roll-to-roll graphene growth of large area；The quartzy plate be multilayer up and down parallel quartzy plate, it can be achieved that single-layer or multi-layer graphene growth, is connect with quartz tubular boat inner wall with spot welding；The quartzy sliding block is used to support quartz tubular boat in growth quartz ampoule internal slide.The beneficial effects of the invention are as follows：The multifunctional graphite vinyls growth demand such as the single layer of graphene growth, multilayer, roll-to-roll can be achieved at the same time in graphene growth platform based on design, solves the problem of single loads less metallic substrates and large-area graphene growth demand.
Description
Technical field
The present invention relates to the technical fields of graphene growth, more particularly to one kind is based on the growth of a large amount of and large-area graphene
The graphene preparation method of quartz boat.
Background technique
Graphene is a kind of two-dimentional carbon nanomaterial being made of carbon atom with sp2 hybridized orbit, due to graphene spy
Different chemistry and physical structure, make its sound, light, electricity, power, in terms of all have very excellent property.Graphene production
Flexible transparent electrode compared with general ordinary electrode, have stronger light transmittance, energy consumption is lower, optoelectronic transformation efficiency is higher,
Thermal conductivity is more preferable, so that single-layer graphene has very big application potential in the electrode field of electrically conducting transparent, but this needs large area
Technology of preparing support.The graphene of single layer functionalization at present, with regard to how to realize the doping modulation of large area pn-junction, or preparation multilayer stone
Black alkene, both openable graphene band gap, can also increase light absorption, be that current graphene studies the goal in research captured, this also makes
Obtaining a large amount of graphenes batch preparations and large area technology of preparing seems very crucial, also shows graphene as two-dimensional material, in light
Electronic material application field possesses extremely wide prospect.
A large amount of and large-area high-quality graphene technology of preparing, still chemical gas phase growth methods main at present.Graphene
It can be based on precious metal catalyst growing technology, grow, be then transferred into specified in copper foil or nickel foil surface large area and in high quality
Substrate, chemical vapor-phase growing growth at present and transfer techniques are quite mature.The graphene prepared using chemical gas phase growth methods
Not only area is larger, and its number of plies and quality can control, and has been increasingly becoming the main stream approach of graphene preparation.
Chemical vapor-phase growing graphene growth metal substrate foil needs to be placed on a platform, to provide in high temperature
Under the conditions of metal foil soften platform.The preparation of a large amount of and large-area graphene is used in quartzy platform technology, specially such as China
Sharp document CN203451615 U is provided《Graphene is grown with quartzy platform》, there is provided a large amount of graphite the advantages of this platform
The possibility of alkene preparation.The disadvantage is that being supported between adjacent quartz plate with quartz column, technique production is complicated, and after multiple welding not
It centainly can guarantee adjacent quartzy flatbed horizontal or parallel；It can not provide large area roll-to-roll graphene preparation.Chinese patent
Document CN102517633 B is provided《A kind of bracket and method growing graphene》, this mold provides a kind of screw type
Winding-structure.The disadvantage is that the continuous winding-structure complex manufacturing technology of quartz, and the temperature deviation in coiled structure is big, this mold
It can not be used for smooth metal foil growth support platform.In addition, these patents do not account for the temperature field inside quartz ampoule yet
Distribution.Because the temperature uniformity inside furnace body quartz ampoule also influences the uniformity of graphene growth, need to consider metal
Foil is located at the uniform isothermal level region of temperature, so as to graphene uniform growth.
Summary of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, providing a kind of high production efficiency, and meet simultaneously smooth
The support platform of planar support platform and Reel-to-reel type solves the technology of a large amount of and rolling large-area graphene growth in plane not
Foot.
Realizing the technical solution of the object of the invention is：A kind of multilayer and large-area graphene growth quartz boat, the platform
It is placed in quartz tubular pipe and carries out graphene growth, the quartz tubular boat, horizontal positioned of quartzy bore is less than including outer diameter
The quartzy sliding block that muti-piece quartz plate, support tubulose quartz boat are slided in quartzy inside pipe wall.
In order to realize the growth of Reel-to-reel type graphene, the quartz tubular boat outer wall of perfect mouth may be used as winding gold
Belong to foil support platform.
In order to guarantee that smooth graphene is grown individually or in batches, quartzy plate can be set to odd-level, to provide metal foil
Support platform.
In order to realize that heating quartz ampoule and the center line of the quartz tubular boat of loading are coaxial, to promote graphene large area
Homoepitaxial, metal foil should be placed in the isothermal level inside quartz ampoule；It is sliding by the quartz for being welded on quartz tubular boat outer wall
Block adjusts the diameter of quartzy sliding block or quartz pushrod cylinder, it is made to support quartz tubular boat inside quartz ampoule, realizes quartz ampoule
It is overlapped with the center line of quartz tubular boat.To adjust in the isothermal level that metal foil is set inside quartz ampoule.
In order to realize one layer of metal foil growth demand, metal foil can be set on the most intermediate quartzy plate of quartz tubular boat；
The quartz ampoule and quartz tubular boat coaxial to center line, one block of most intermediate in quartz tubular boat quartz of horizontal cross-section diameter
Plate upper surface, and the section center of circle O of quartz ampoule and quartz boat is overlapped.
In order to realize a large amount of smooth graphene growths, the interval of multilayer quartz plate can be set to 3 mm-10 mm, so as to
It is placed or taken out in rectangular or square metal foil, and the width of metal foil is slightly smaller than the width of quartzy plate.
Easy to operate for Reel-to-reel type graphene growth, metal foil is wrapped among quartz tubular boat without quartzy sliding block
Region；And foldable part divides edge metal foil in the inner wall of quartz tubular boat.The quartz pushrod of cylindrical body can be used in quartzy sliding block, rises
To supporting role, the both ends of quartz tubular boat outer wall are welded to, length can be cut into 0.5 cm-5 cm, convenient for quartz boat in quartz
Pipe internal slide.
In order to realize the growth of a large amount of and large-area graphene, the outer wall of multilayer quartz plate and quartz tubular boat can be simultaneously
As the support platform of metal foil, while being used to graphene growth.
In order to stablize support tubulose quartz boat, can outer wall of the spot welding quartz sliding block 2 ~ 3 in quartz tubular boat both ends, and stone
English sliding block one side and quartz tubular boat outboard alignment；And the angle α for adjusting quartzy sliding block is 90 ° ~ 120 °.
In order to which the manufacture craft of graphene growth platform is simple, multilayer quartz plate and quartzy sliding block can be welded to tubulose stone
English boat inner and outer wall both ends.
To realize controllable graphene growth, metal foil substrate can be cut into length less than or equal to quartz tubular boat
Length, and width is slightly smaller than the width of quartzy plate is placed in the quartz of the middle layer of quartz boat, any one layer or any multilayer
On plate.One circle of metal foil winding be can satisfy simultaneously in the outer wall of quartz tubular boat, to realize a large amount of and large-area graphene
The demand of growth.
Quartz boat of the invention is suitable for chemical gaseous phase product system, including low-pressure system, normal pressure system, plasma increase
Strong system etc..Wherein low pressure chemical phase growing system can realize the growth demand of high-quality graphene.And pass through control graphite
The growth conditions of alkene, such as growth temperature, heating rate, hydrocarbon gas flow, hydrogen flowing quantity, growth time accurately to control stone
The number of plies of black alkene is grown and large-area high-quality growth.
The invention has the advantages that graphene growth quartz boat of the invention, the processing is simple, easy to clean and more
Function growth is complete, and cost is relatively low；And it can be based on this newly-designed quartz boat, provide large area uniform graphene growth side
Method.Whether one layer of scientific research demand explores the growth of multilayer batch or large area large scale after growth or technical maturity
Reel-to-reel type growth, the present invention solve the problems, such as few useful load, multifunctional use and growth uniformity.
Detailed description of the invention
In order that the present invention can be more clearly and readily understood, in the following with reference to the drawings and specific embodiments, the present invention is made
Further details of explanation, wherein
Fig. 1 is the lateral cross schematic diagram of quartz boat of the present invention.
Fig. 2 is facing structure figure of the quartz boat of the present invention in tube furnace.
In figure：1, quartz ampoule（Inner wall）, 2, quartz tubular boat, 3, quartzy plate, 4, quartzy sliding block.
Specific embodiment
To keep technological means, design feature, the purpose of design of the invention realized concise, now in conjunction with attached drawing to the present invention
It is described in further detail, these attached drawings are simplified schematic diagram.
It as shown in Figure 1, 2, is the embodiment of the multi-functional growth quartz boat of graphene of the present invention, it is sliding which is based on quartz
Block is slidably in heating quartz ampoule, and quartzy sliding block is simply placed at quartz tubular boat outer wall both ends, and quartz tubular boat is smooth
Most of region among outer wall, can be used as the support platform of rolled metallic paillon, because being in the identical radial position of quartz boat,
The temperature difference that can be achieved on metal foil is uniform.Horizontal quartzy plate quantity is arranged to odd-level, and the upper table of middle layer
Face has the center line of quartz boat to pass through, it ensures that the upper surface of middle layer quartz plate is placed exactly in quartz boat center
In plane, this is also the isothermal level of quartz boat uniformity of temperature profile.The quartzy plate quantity of odd-level depends on the interior of quartz boat
The distance between diameter size and quartzy plate, it is however generally that, the distance between quartzy plate is arranged to 3 mm-10 mm, in order to
The loading and taking-up of metal foil.Quartzy plate spacing is equal, and intermediate quartzy plate width is maximum, and the quartz of upper and lower two sides is flat
The width of plate gradually successively decreases to upper and lower ends.Quartzy plate and quartzy sliding block all can spot welding be connected to quartz tubular boat inner wall and
Outer wall both ends.
The quartz boat used in the present invention can use in the following manner：（i）It will be used for the metal foil of graphene growth extremely
In in the growth platform in quartz tubular boat；（ii）The metal foil for being used for graphene growth is wrapped in the outer of quartz tubular boat
Wall；（iii）It is both above-mentioned to carry out simultaneously.Growing method of the invention is suitable for chemical gaseous phase product system.
Embodiment
The present invention is illustrated by the following examples, but the scope of the present invention is not limited thereto.
Embodiment 1
Using Fig. 1 and quartz boat shown in Fig. 2, the metal foil of graphene growth is placed on the quartzy plate of quartz boat or is twined
It is around in the outer wall of quartz boat.
It takes out the vacuum degree inside quartz ampoule and is evacuated to 10 Pa or so, start to be passed through hydrogen, gas flow is 50 sccm, is continued
Hydrogen flow rate can be increased after being passed through 5 min, inside and outside pipe when pressure equilibrium, vacuum pump is again turned on and vacuumizes.Repeat above-mentioned pumping
After vacuumizing two ~ three times, be passed through 2 sccm of hydrogen again, and quartz ampoule internal pressure is extracted into 5.3 Pa, start starting plus
Heat.15 DEG C/min is arranged in the rate of heat addition, and the temperature for stablizing quartz ampoule is passed through methane after 30 min of constant temperature, adjusts it to 1000 DEG C
Flow continues 1000 DEG C of temperature of holding and continues one hour, carry out graphene growth to 35 sccm.After start to cool down, Zhi Daowen
Degree is down to room temperature, and growth is completed, this process be always maintained at be passed through hydrogen and methane flow velocity it is constant.It again will pipe after the completion of growth
Inside vacuumize, after be passed through protective gas argon gas.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.It should be understood that this hair
Bright to be not restricted to the described embodiments, without departing from the spirit and scope of the invention, the present invention also has various change
And improvement, these changes and improvements all fall within the protetion scope of the claimed invention.
Claims (6)
1. a kind of graphene growth method based on multilayer and large-area graphene growth quartz boat, it is characterised in that：Quartz
Boat includes quartz tubular boat（2）, quartzy plate（3）With quartzy sliding block（4）；The quartz tubular boat（2）Positioned at quartz tubular pipe
（1）It is interior；The quartzy plate（3）It is horizontally inserted into quartz tubular boat（2）It is interior；The quartzy sliding block（4）Positioned at quartz tubular
Boat（2）The both ends of outer wall；Based on this Novel quartz boat, graphene growth can carry out in tubulose chemical gas-phase deposition system.
2. a kind of graphene growth based on multilayer and large-area graphene growth quartz boat according to claim 1
Method, it is characterised in that：Quartz tubular boat（2）Positioned at quartz tubular pipe（1）It is interior, and quartz tubular boat（2）With quartz tubular pipe
（1）Center line main shaft be overlapped, the section center of circle is all in O point.
3. a kind of graphene growth based on multilayer and large-area graphene growth quartz boat according to claim 1
Method, it is characterised in that：The quartzy plate（3）It can be set to odd number multilayer, be horizontally inserted into quartz tubular boat（2）It is interior
Portion, and using quartzy spot-welded, and intermediate quartzy plate width is most wide, just there are center of circle O point, upper and lower stone in upper surface
English plate（3）Width successively successively decrease, horizontal layout is in quartz tubular boat（2）It is internal.
4. a kind of graphene growth based on multilayer and large-area graphene growth quartz boat according to claim 1
Method, it is characterised in that：The quartzy sliding block（4）Positioned at quartz tubular boat（2）The both ends of outer wall, quartzy sliding block（4）Using
The quartz pushrod of cylindrical body, length can be cut into 0.5 cm-5 cm；Quartzy sliding block（4）Quantity can be 2 ~ 3, and quartzy point
It is welded in quartz tubular boat（2）The both ends of outer wall, quartzy sliding block（4）Side and quartz tubular boat（2）The outboard alignment at both ends；Stone
English sliding block（4）Angle α be 90 ° ~ 120 °.
5. a kind of graphene growth based on multilayer and large-area graphene growth quartz boat according to claim 1
Method, it is characterised in that：1）, the growth of catalytic graphite alkene metal foil substrate, cut its length less than or equal to quartz tubular boat
（2）Length, width is slightly smaller than quartzy plate（3）Width, be placed in middle layer, any one layer or any multilayer of quartz boat
Quartzy plate（3）On；2）, metal foil substrate length be less than or equal to quartz tubular boat（2）Length, winding one circle in pipe
Shape quartz boat（2）Outer wall；
3）, metal foil substrate can be placed in quartzy plate simultaneously（3）Above or wound on quartz tubular boat（2）Outer wall on.
6. a kind of graphene growth based on multilayer and large-area graphene growth quartz boat according to claim 1
Method, it is characterised in that：In chemical gas-phase deposition system, the growth conditions of graphene is：900-1100 DEG C of depositing temperature；
Heating rate is 5-20 DEG C/min；Carbons gas is hydrocarbon gas, and flow is 10-100 sccm；Catalyzed gas is hydrogen, stream
Amount is 2-100 sccm；5 ~ 200 Pa of growth pressure；Growth time 5-60 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810781188.6A CN108862253A (en) | 2018-07-17 | 2018-07-17 | A kind of graphene growth method based on multilayer and large-area graphene growth quartz boat |
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| CN201810781188.6A CN108862253A (en) | 2018-07-17 | 2018-07-17 | A kind of graphene growth method based on multilayer and large-area graphene growth quartz boat |
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| CN203451615U (en) * | 2013-08-19 | 2014-02-26 | 常州二维碳素科技有限公司 | Quartz platform for growing graphene |
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2018
- 2018-07-17 CN CN201810781188.6A patent/CN108862253A/en active Pending
Patent Citations (6)
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| KR101458045B1 (en) * | 2013-05-15 | 2014-11-04 | 한국과학기술원 | A subsidiary equipment in chemical vapor deposition method for the reliable production of high quality and large sized graphene |
| CN203451615U (en) * | 2013-08-19 | 2014-02-26 | 常州二维碳素科技有限公司 | Quartz platform for growing graphene |
| CN103449428A (en) * | 2013-09-10 | 2013-12-18 | 常州二维碳素科技有限公司 | Graphene growing device and method |
| CN105174247A (en) * | 2014-05-30 | 2015-12-23 | 常州二维碳素科技股份有限公司 | Device and method for growing large-area graphene and graphene obtained therefrom |
| CN204281325U (en) * | 2014-11-27 | 2015-04-22 | 湖南东博墨烯科技有限公司 | A kind of shaped platform being suitable for graphene growth |
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