CN103086359B - A kind of method of continuous production Graphene - Google Patents
A kind of method of continuous production Graphene Download PDFInfo
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- CN103086359B CN103086359B CN201110339973.4A CN201110339973A CN103086359B CN 103086359 B CN103086359 B CN 103086359B CN 201110339973 A CN201110339973 A CN 201110339973A CN 103086359 B CN103086359 B CN 103086359B
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Abstract
The invention provides a kind of method of continuous production Graphene, comprise the following steps: (1) substrate to metal material cleans; (2) after cleaning substrate surface coating carbonaceous material; (3) substrate scribbling carbonaceous material is sent into this reaction chamber by transport sector by one end of reaction chamber, and heat scission reaction is carried out in silicon to 750 ~ 1100 DEG C, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate scribbling carbonaceous material is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.The present invention has the advantage of uninterrupted continuous production, and equipment is simple, and operation simple and feasible, easily is automated and suitability for industrialized production.The Graphene that the present invention obtains has the advantages such as the few and crystalline structure of defect is complete.
Description
Technical field
The present invention relates to the method for process for preparing graphenes by chemical vapour deposition, particularly relate to the method for continuous production Graphene under a kind of normal pressure.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal that strong K sea nurse (Andre K.Geim) of peace moral etc. of Univ Manchester UK in 2004 finds, is the very thin carbon material of single or multiple lift.Single-layer graphene has excellent conduction, heat conductivility and low thermal expansivity, and its theoretical specific surface area is up to 2630m
2/ g (A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), can be used for effect transistor, electrode materials, matrix material, liquid crystal display material, sensor.The structure of Graphene uniqueness and photoelectric property become the study hotspot in the fields such as carbon material, nanotechnology, Condensed Matter Physics and functional materials.
In enormous quantities, the low cost preparation of investigation and application to it of Graphene propose an urgent demand.The method preparing Graphene at present mainly contains graphite breakaway (Novoselov K S, Geim A K, et al.Science 2004,306,666), chemistry redox method (D A Dikin, et al.Nature 2007,448,457; SashaStankovich, Dmitriy A Dikin, Richard D Piner, et al.Carbon 2007,45,1558), ultrasonic stripping method (Guohua Chen, Wengui Weng, Dajun Wu, et al.Carbon.2004,42,753) etc.But the shape of Graphene that these methods are prepared is all irregular substantially, the number of plies is indefinite, and pattern is restive.
Chemical Vapor deposition process has achieved the batch production of carbon nanotube, is expected to utilize chemical Vapor deposition process to realize the batch production of Graphene.So people start to utilize process for preparing graphenes by chemical vapour deposition (Alexander N, Obraztsov.Nature nanotechnology.2009,4,212), but the method just a small amount of preparation.Publication number is a kind of method that the Chinese patent application of CN101285175A discloses process for preparing graphenes by chemical vapour deposition film, need catalyzer uniform deposition in this method on substrate, not only can introduce unnecessary impurity, but also the complicacy of operation and unnecessary equipment can be strengthened, cause high cost, and uninterrupted preparation can not be realized continuously.
Summary of the invention
For solving the problem, the present invention aims to provide a kind of method of continuous production Graphene, and the method has the advantage of uninterrupted continuous production at ambient pressure, and equipment is simple, and operation simple and feasible, easily is automated and suitability for industrialized production.
On the one hand, the method for a kind of continuous production Graphene provided by the invention, comprises the following steps:
(1) substrate of metal material is cleaned;
(2) after cleaning substrate surface coating carbonaceous material;
(3) substrate scribbling carbonaceous material is sent into this reaction chamber by transport sector by one end of reaction chamber, and heat scission reaction is carried out in silicon to 750 ~ 1100 DEG C, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate scribbling carbonaceous material is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
Step (1) is for clean the substrate of metal material.
Preferably, cleaning process comprises: use deionized water, ethanol, acetone to described substrate ultrasonic cleaning successively.
Substrate can be tinsel, also can be wire netting.Preferably, substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications, when substrate is grid, and the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
Step (2) is substrate surface coating carbonaceous material after cleaning.
Preferably, carbonaceous material is one in camphor, glucose, decolorizing carbon and sucrose or its arbitrary combination.
The continuous production process that step (3) is Graphene in reaction chamber.
Preferably, protective gas is one in hydrogen, nitrogen and argon gas or its arbitrary combination.
Preferably, the airshed passing into protective gas in reaction chamber is 10 ~ 1000sccm.
Preferably, transport sector is transport tape, and described transport tape carries out transmission under the effect of driving motor.Also preferably, transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
On the other hand, as the improvement of technique scheme, present invention also offers a kind of method of continuous production Graphene, comprise the following steps:
(1) substrate of metal material is cleaned;
(2) substrate after cleaning is sent into this reaction chamber by transport sector by one end of reaction chamber, and by silicon to 750 ~ 1100 DEG C, pass into carbonaceous gas, carry out heat scission reaction, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
Step (1) is for clean the substrate of metal material.
Preferably, cleaning process comprises: use deionized water, ethanol, acetone to described substrate ultrasonic cleaning successively.
Substrate can be tinsel, also can be wire netting.Preferably, substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications, when substrate is grid, and the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
In step (2), the mode of input carbonaceous material is directly to passing into carbonaceous gas in reaction chamber, carries out the continuous production of Graphene.
Preferably, carbonaceous gas is one in methane, ethane and acetylene or its arbitrary combination.
Preferably, protective gas is one in hydrogen, nitrogen and argon gas or its arbitrary combination.
Preferably, the airshed passing into protective gas in reaction chamber is 10 ~ 1000sccm.
Preferably, transport sector is transport tape, and described transport tape carries out transmission under the effect of driving motor.Also preferably, transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
The method of continuous production Graphene provided by the invention, has the advantage of uninterrupted continuous production, and equipment is simple, and operation simple and feasible, easily is automated and suitability for industrialized production.In addition, there is compared with Graphene prepared by the Graphene obtained by preparation method of the present invention and common reduction method the advantages such as the few and crystalline structure of defect is complete.
Accompanying drawing explanation
Fig. 1 is one of process flow sheet of continuous production Graphene of the present invention;
Fig. 2 is the process flow sheet two of continuous production Graphene of the present invention;
The SEM Electronic Speculum figure of the Graphene of Fig. 3 prepared by the embodiment of the present invention one.
Embodiment
The present invention aims to provide a kind of method of continuous production Graphene, as shown in Figure 1, comprises the following steps:
(1) carry out ultrasonic cleaning with deionized water, ethanol, acetone to the substrate of metal material successively, the ultrasonic cleaning time is respectively about 15 minutes;
(2) after cleaning substrate surface coating carbonaceous material, as the one in camphor, glucose, decolorizing carbon and sucrose or its arbitrary combination;
(3) substrate scribbling carbonaceous material is sent into this reaction chamber by transport sector by one end of reaction chamber, and heat scission reaction is carried out in silicon to 750 ~ 1100 DEG C, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate scribbling carbonaceous material is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
The method of above-mentioned continuous production Graphene, in step (1), preferably, substrate can be tinsel, also can be wire netting.Preferably, substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications, when substrate is grid, and the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
The method of above-mentioned continuous production Graphene, in step (3), preferably, protective gas is one in hydrogen, nitrogen and argon gas or its arbitrary combination, and the airshed passing into protective gas in reaction chamber controls at about 10 ~ 1000sccm; In this step, preferably, transport sector is transport tape, and described transport tape carries out transmission under the effect of driving motor.Also preferably, transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
The method of above-mentioned continuous production Graphene, in step (3), working cycle prepared by Graphene can be persistence successive processes, also can intermittent type successive processes; Wherein, the successive processes of persistence is: whole substrate is a continuous endless being laid on transport sector, this substrate slowly enters reaction chamber with transmission rig, carries out the preparation of Graphene, simultaneously obtained Graphene sending with transport sector also by persistence; Intermittent type successive processes is: substrate be some independently, be laid on transport sector by compartment, sending into reaction chamber at substrate with transport sector prepares in Graphene process, guarantee Graphene preparation fully, its Graphene preparation time cycle can control as required voluntarily, in Graphene preparation process, transport sector operation suspension, after prepared by Graphene, transport sector is startup optimization again, sends the Graphene prepared, next substrate is sent into reaction chamber simultaneously, so circulate.
On the other hand, as the improvement of technique scheme, present invention also offers a kind of method of continuous production Graphene, as shown in Figure 2, comprise the following steps:
(1) carry out ultrasonic cleaning with deionized water, ethanol, acetone to the substrate of metal material successively, the ultrasonic cleaning time is respectively about 15 minutes;
(2) substrate after cleaning is sent into this reaction chamber by transport sector by one end of reaction chamber, and by silicon to 750 ~ 1100 DEG C, pass into carbonaceous gas, carry out heat scission reaction, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
The method of above-mentioned continuous production Graphene, in step (1), preferably, substrate can be tinsel, also can be wire netting.Preferably, substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications, when substrate is grid, and the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
The method of above-mentioned continuous production Graphene, in step (2):
Preferably, carbonaceous gas is one in methane, ethane and acetylene or its arbitrary combination;
Preferably, protective gas is one in hydrogen, nitrogen and argon gas or its arbitrary combination, and the airshed passing into protective gas in reaction chamber is 10 ~ 1000sccm;
Preferably, transport sector is transport tape, and described transport tape carries out transmission under the effect of driving motor.Also preferably, transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
The method of above-mentioned continuous production Graphene, in step (3), working cycle prepared by Graphene can be persistence successive processes, also can intermittent type successive processes; Wherein, the successive processes of persistence is: whole substrate is a continuous endless being laid on transport sector, this substrate slowly enters reaction chamber with transmission rig, carries out the preparation of Graphene, simultaneously obtained Graphene sending with transport sector also by persistence; Intermittent type successive processes is: substrate be some independently, be laid on transport sector by compartment, sending into reaction chamber at substrate with transport sector prepares in Graphene process, guarantee Graphene preparation fully, its Graphene preparation time cycle can control as required voluntarily, in Graphene preparation process, transport sector operation suspension, after prepared by Graphene, transport sector is startup optimization again, sends the Graphene prepared, next substrate is sent into reaction chamber simultaneously, so circulate.
The method of continuous production Graphene provided by the invention, has the advantage of uninterrupted continuous production, and equipment is simple, and operation simple and feasible, easily is automated and suitability for industrialized production.In addition, there is compared with Graphene prepared by the Graphene obtained by preparation method of the present invention and common reduction method the advantages such as the few and crystalline structure of defect is complete.
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment one
A method for continuous production Graphene, comprises the following steps:
(1) with deionized water, ethanol, acetone, ultrasonic cleaning is carried out to iron foil successively;
(2) iron foil surface-coated camphor after cleaning;
(3) iron foil scribbling camphor is sent into this reaction chamber (described transport tape carries out transmission under the effect of driving motor) by transport tape by one end of reaction chamber, iron foil is heated to 750 DEG C and carries out heat scission reaction, keep 1 minute, obtained Graphene, then have the iron foil of Graphene to be sent by the other end of described reaction chamber by transport tape by obtained; Another iron foil scribbling camphor is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with argon gas 1000sccm.
The SEM Electronic Speculum figure of the Graphene of Fig. 3 prepared by the embodiment of the present invention one, obviously can find out from Fig. 3 and go out Graphene on iron foil surface successful growth, thickness is about 1 ~ 2nm, and length is about 0.5 ~ 5um.
Embodiment two
A method for continuous production Graphene, comprises the following steps:
(1) with deionized water, ethanol, acetone, ultrasonic cleaning is carried out to Copper Foil successively;
(2) after cleaning copper foil surface coating glucose;
(3) Copper Foil scribbling glucose is sent into this reaction chamber (described transport tape carries out transmission under the effect of driving motor) by transport tape by one end of reaction chamber, Copper Foil is heated to 1100 DEG C and carries out heat scission reaction, keep 30 minutes, obtained Graphene, then have the Copper Foil of Graphene to be sent by the other end of described reaction chamber by transport tape by obtained; Another Copper Foil scribbling glucose is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with hydrogen 10sccm.
Embodiment three
A method for continuous production Graphene, comprises the following steps:
(1) with deionized water, ethanol, acetone, ultrasonic cleaning is carried out to nickel foil successively;
(2) nickel foil surface-coated decolorizing carbon after cleaning;
(3) nickel foil scribbling decolorizing carbon is sent into this reaction chamber (described transport tape carries out transmission under the effect of driving motor) by transport tape by one end of reaction chamber, nickel foil is heated to 950 DEG C and carries out heat scission reaction, keep 200 minutes, obtained Graphene, then have the nickel foil of Graphene to be sent by the other end of described reaction chamber by transport tape by obtained; Another nickel foil scribbling decolorizing carbon is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with argon gas 500sccm.
Embodiment four
(1) ultrasonic cleaning is carried out with deionized water, ethanol, the copper mesh of acetone to 50 order specifications successively;
(2) copper mesh surface-coated sucrose after cleaning;
(3) copper mesh scribbling sucrose is sent into this reaction chamber (described roller rotates according to same direction under the effect of driving motor) by the roller be arranged side by side by one end of reaction chamber, copper mesh is heated to 1000 DEG C and carries out heat scission reaction, keep 300 minutes, obtained Graphene, the copper mesh of Graphene is had to be sent by the other end of described reaction chamber by the roller that is arranged side by side by obtained again, the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene; Another copper mesh is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with hydrogen: argon gas is the mixed gas 50sccm of 1:1.
Embodiment five
A method for continuous production Graphene, comprises the following steps:
(1) with deionized water, ethanol, acetone, ultrasonic cleaning is carried out to cobalt paper tinsel successively;
(2) the cobalt paper tinsel after cleaning is sent into this reaction chamber (described transport tape carries out transmission under the effect of driving motor) by transport tape by one end of reaction chamber, and cobalt paper tinsel is heated to 900 DEG C and passes into methane carry out heat scission reaction, keep 60 minutes, obtained Graphene, then have the cobalt paper tinsel of Graphene to be sent by the other end of described reaction chamber by transport tape by obtained; Another cobalt paper tinsel scribbling carbonaceous material is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with hydrogen 10sccm.
Embodiment six
A method for continuous production Graphene, comprises the following steps:
(1) ultrasonic cleaning is carried out with deionized water, ethanol, the iron net of acetone to 325 order specifications successively;
(2) roller bearing be arranged side by side is crossed by the iron Netcom after cleaning and send into this reaction chamber (described roller bearing rotates according to same direction under the effect of driving motor) by one end of reaction chamber, and iron net is heated to 1050 DEG C and passes into acetylene carry out heat scission reaction, keep 60 minutes, obtained Graphene, the iron net of Graphene is had to be sent by the other end of described reaction chamber by the roller bearing that is arranged side by side by obtained again, the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene; Another iron net is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with nitrogen 1000sccm.
Claims (10)
1. a method for continuous production Graphene, is characterized in that, comprises the following steps:
(1) substrate of metal material is cleaned;
(2) after cleaning substrate surface coating carbonaceous material;
(3) substrate scribbling carbonaceous material is sent into this reaction chamber by transport sector by one end of reaction chamber, and heat scission reaction is carried out in silicon to 750 ~ 1100 DEG C, keep 1 ~ 300 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate scribbling carbonaceous material is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
2. the method for claim 1, is characterized in that, in step (1), described substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications; When described substrate is grid, the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
3. the method for claim 1, is characterized in that, in step (2), described carbonaceous material is one in camphor, glucose, decolorizing carbon and sucrose or its arbitrary combination.
4. the method for claim 1, is characterized in that, in step (3), protective gas is one in hydrogen, nitrogen and argon gas or its arbitrary combination.
5. the method for claim 1, is characterized in that, in step (3), the described airshed passing into protective gas in reaction chamber is 10 ~ 1000sccm.
6. the method for claim 1, it is characterized in that, in step (3), described transport sector is transport tape, described transport tape carries out transmission under the effect of driving motor, or described transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
7. a method for continuous production Graphene, is characterized in that, comprises the following steps:
(1) substrate of metal material is cleaned;
(2) substrate after cleaning is sent into this reaction chamber by transport sector by one end of reaction chamber, and by silicon to 750 ~ 1100 DEG C, pass into carbonaceous gas, carry out heat scission reaction 1 ~ 60 minute, obtained Graphene, then have the substrate of Graphene to be sent by the other end of described reaction chamber by transport sector by obtained; Another substrate is admitted in described reaction chamber and carries out heat scission reaction simultaneously, carries out the preparation process of next Graphene, and so circulation is carried out; Wherein, described reaction chamber continues to be connected with protective gas.
8. method as claimed in claim 7, is characterized in that, in step (1), described substrate is the grid of the paillon foil that obtains of metallic copper, iron, nickel or cobalt or 50 ~ 325 order specifications; When described substrate is grid, the bottom of described reaction chamber or be positioned at the collection device be provided with below described transport sector for collecting Graphene.
9. method as claimed in claim 7, it is characterized in that, in step (2), described transport sector is transport tape, and described transport tape carries out transmission under the effect of driving motor; Or described transport sector is the roller or roller bearing that are arranged side by side, and described roller or roller bearing rotate according to same direction under the effect of driving motor.
10. method as claimed in claim 7, is characterized in that, in step (2), described carbonaceous gas is one in methane, ethane and acetylene or its arbitrary combination.
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CN103232034A (en) * | 2013-05-23 | 2013-08-07 | 中国石油大学(北京) | Method and device for continuously preparing large-area graphene thin film |
CN103274394A (en) * | 2013-06-07 | 2013-09-04 | 新疆师范大学 | Method for preparing graphene by thermal decomposition |
CN105088335B (en) * | 2014-05-09 | 2018-01-05 | 理想能源设备(上海)有限公司 | A kind of device and its growing method for growing graphene film |
CN103993297A (en) * | 2014-06-09 | 2014-08-20 | 中国科学院宁波材料技术与工程研究所 | Vapor deposition device for continuously and quickly growing graphene |
CN105734525A (en) * | 2014-12-10 | 2016-07-06 | 黑龙江鑫达企业集团有限公司 | Method for preparing graphene thin film through chemical vapor deposition |
CN104817072A (en) * | 2015-03-27 | 2015-08-05 | 中国科学技术大学 | High mechanical strength multilayer graphene and preparation method thereof |
CN104843691B (en) * | 2015-04-30 | 2017-01-11 | 深圳市德方纳米科技股份有限公司 | Graphene and preparation method thereof |
CN106653924B (en) * | 2017-01-20 | 2018-02-06 | 郑州航空工业管理学院 | A kind of Schootky scolar cell and preparation method thereof |
CN108190864B (en) * | 2018-01-16 | 2021-07-06 | 电子科技大学 | Graphene preparation method |
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CN102134067A (en) * | 2011-04-18 | 2011-07-27 | 北京大学 | Method for preparing single-layer graphene |
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