CN105645389A - Method for preparing graphene from amorphous carbon - Google Patents
Method for preparing graphene from amorphous carbon Download PDFInfo
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- CN105645389A CN105645389A CN201511007793.0A CN201511007793A CN105645389A CN 105645389 A CN105645389 A CN 105645389A CN 201511007793 A CN201511007793 A CN 201511007793A CN 105645389 A CN105645389 A CN 105645389A
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Abstract
The invention discloses a method for preparing graphene from amorphous carbon. The method comprises the following steps: preheating the amorphous carbon; adding a catalyst to the preheated amorphous carbon; pyrolyzing the amorphous carbon under the action of the catalyst; depositing cracked carbon atoms on a layered carrier to obtain graphene containing the carrier; and removing the carrier to obtain graphene. The method for preparing graphene from amorphous carbon with wide sources has the advantages of low cost, convenient obtaining of the above raw material, and high resource utilization rate; and the method is directly realized through a screw extruder, and has great industrial prospect.
Description
Technical field
The present invention relates to the technical field of the preparation of Graphene.
Background technology
Graphene is that a kind of carbon atom is closely arranged as cellular plane atomic crystal structure by regular hexagon, the distinctive planar structure of Graphene makes it possess the characteristic that many three-dimensional crystals do not possess, if specific surface area is up to 2.6 �� 103m2/g, heat conductivity is up to 3 �� 103W/(m.K), mechanical property is 1.06 �� 103Gpa, Young's modulus is 1.0TPa, and its mechanical strength, up to 130Gpa, is more than 100 times of steel. Graphene has stable regular hexagon lattice structure makes it have the electric conductivity of excellence, and electron mobility is up to 1.5 �� 104cm2/ (V.s), higher than the maximum mobility of semiconductor indium antimonide 2 times, higher than the maximum mobility of commercial silicon chip 10 times, Graphene also has significantly high light transmission, room-temperature quantum tunnel-effect, unusual quantum hall effect etc. in addition.
Mechanical stripping method is mainly included at present: peel off as monolayer carbon atomic structure by mechanism by graphite in the preparation method of Graphene; Epitaxial growth method, high-temperature heating large area monocrystal SiC, make graphene growth thereon, under ultrahigh vacuum or normal pressure, remove Si leave C, then obtain and the Graphene thin layer of the similar area of SiC, material as graphene substrate is divided into non-metal kind substrate (such as SiC, SiO2, GaAs etc.) and metal substrate (such as Cu, Ni, Co, Ru, Au, Ag etc.), and the Graphene that epitaxial growth method prepares still is unable to reach homogeneous thickness; Metal catalysed processes: the method that the carbon source of solid-state or gaseous state directly generates Graphene under the effect of certain temperature, pressure and catalyst in substrate, including chemical vapour deposition technique and metal catalysed processes two kinds; Quenching method: produce stress by the internal-external temperature difference caused in quickly cooling down, makes Graphene depart from from graphite surface, also includes direct combustion method, electrochemical process, in-situ authigenic template etc.
Carbon is one of element that on the earth, content is the abundantest, pure carbonizable substance can be divided into crystal form and amorphism according to structure, crystal form carbon includes graphite, diamond and fullerene etc., wherein amorphous carbon wide material sources, can be easily separated, it is possible to prepare, by suitable physics, chemical method, the crystal form carbon that performance is more excellent.
But in current graphene preparation method, amorphous carbon is really utilized to prepare the research of Graphene and few, trace it to its cause, prepare in the method for crystal form carbon utilizing amorphous carbon, a kind of in the two kinds of thinkings that can infer enable carbon atom to recombinate to be grown to crystal form carbon for the structure of former amorphous carbon being destroyed completely, the another kind of structure for not exclusively breaking amorphous carbon, but induce its crystal formation to change and continue to grow as crystal form carbon, no matter which kind of method, its preparation will be all a complexity, fine process, need to carry out in highly controllable environment, it is unfavorable for the industrialization of Graphene, therefore research in this respect or report are all less.
Summary of the invention
Technical scheme is as follows:
A kind of method utilizing amorphous carbon to prepare Graphene, comprises the following steps:
(1) amorphous carbon preheating;
(2) in the amorphous carbon after preheating, catalyst is added;
(3) amorphous carbon Pintsch process under catalyst action;
(4) carbon atom after cracking is deposited on layered vector, obtains the Graphene containing carrier;
(5) remove carrier, namely obtain Graphene.
In above-mentioned steps, the purpose of the preheating of amorphous carbon is in that to put aside energy for the Pintsch process of amorphous carbon thereafter on the one hand, also catalyst can be made on the other hand can to produce activity after adding at once, quickly react, the catalyst purpose added in step (2) is in that to promote the decomposition of amorphous carbon, particularly reduce its decomposition temperature, therefore optimal catalyst is that amorphous carbon can be promoted at normal temperatures to be cracked into the catalyst of atomic carbon completely, the effect of step (3) laminate carrier is in that the carrier of the carbon atom deposition after providing cracking on the one hand, further aspect is that the shaping ensureing Graphene crystal formation.
A kind of preferred implementation of above-mentioned preparation method is: being accompanied by layered carrier shaping controlling agent, described shaping controlling agent is fluorocarbon surfactant.
The two of the effect of layered vector are in that to ensure the shaping of Graphene crystal formation as previously mentioned, if therefore incidentally can control the regular arrangement of atomic carbon on carrier, the controlling agent of growth is clearly more excellent selection, first-selection of the present invention is found that fluorocarbon surfactant possesses such function, it can be uniformly distributed on the one hand on a solid support, can promote that single or multiple carbon atom is uniformly sprawled in its surface on the other hand.
Further preferred embodiment is: described fluorocarbon surfactant is one or more in N-N-dimethylpropyl, N-ethylperfluoro octyl group sulfonamide, N-propyl group perfluorinated octyl sulfuryl amine.
Another kind of further preferred embodiment is: the complex method of layered carrier and described shaping controlling agent is: be soaked in by layered carrier in the dispersion liquid of described shaping controlling agent.
Dispersion liquid described herein refers to and adds, by shaping controlling agent, the solution or mixed liquor that obtain in common solvent, shape controlling agent and need not be dissolved completely in these solvents, as long as it can be distributed than more uniform in these solvents, for aid dispersion effect, this further preferred embodiment can maintain continual stirring in carrying out.
The another kind of preferred implementation of the present invention is: described amorphous carbon is one or more in coal, gangue, activated carbon.
Certain amorphous carbon wide material sources, this preferred implementation is not really wanted to limit it and is only this several materials, and these several materials above-mentioned are that the several of discovery in process prepared by the present invention preferably select.
The another kind of preferred implementation of the present invention is: described catalyst is one or more in 3A, 4A, 5A molecular sieve.
3A ~ 5A molecular sieve bore diameter is less herein, single or several carbon atom can be passed through, and bigger molecule can not be passed through, therefore in the process of catalysis, it is simultaneously achieved the selection to the carbon atom forming amorphous carbon, do not limit structure or its constituent of concrete molecular sieve herein, as long as it can reach identical purpose, it can also be carried out suitable modifiying to improve catalytic capability by implementer in actual use.
The another kind of preferred implementation of the present invention is: the temperature of described Pintsch process is 500 ~ 1000 DEG C.
Purpose at this Pintsch process is in that to destroy the original structure of amorphous carbon, produces the single or multiple carbon atoms separated, so that it can recombinate in subsequent process.
The another kind of preferred implementation of the present invention is: layered carrier is one or more in borate, mica powder, perovskite, molybdenum bisuphide.
Above-mentioned preparation method and various preferred implementation thereof all can be realized by screw extruder.
Preferably: the preheating section for amorphous carbon preheating that described screw extruder includes being sequentially connected to rear end from front end, seal processing sections for what the Graphene containing carrier was formed, strengthen the morphogenetic cooling section of Graphene and the discharging opening discharged for the Graphene containing carrier, wherein seal and processing sections also include near first charge door for catalyst addition of preheating section and be positioned at second charge door for carrier addition of seal section postmedian.
Prepare in the process of Graphene utilizing this screw extruder, above-mentioned each section all maintains screw rod rotation, temperature at preheating section is preferably 100 ~ 400 DEG C, amorphous carbon is carried out preliminary mechanical damage at this section, followed by sealing processing sections, catalyst amorphous carbon put into the shape that fragmentates from the first charge door mixes, seal section preferably passes into noble gas, to avoid this process occurs other side reaction, after catalyst enters, temperature in seal section is optimally maintained at 500 ~ 1000 DEG C, to ensure the lytic effect of amorphous carbon, to its back segment, carrier enters from the second charge door, single or multiple carbon atoms after catalyzed cracking are at deposited on supports, form the basic structure of Graphene, thereafter cooling section is entered, the slewing rate of screw rod can somewhat slow down herein, to ensure the formation of Graphene form, this section of temperature is preferably less than 25 DEG C, after this section, the Graphene containing carrier is discharged from discharging opening, after the method using the carrier of physics stripping or chemistry to dissolve, namely finished product Graphene is obtained.
The invention have the benefit that
(1) amorphous carbon utilizing wide material sources prepares Graphene, with low cost, and raw material obtains convenient, and data utilization rate is high;
(2) carbon source using solid carbon to prepare as Graphene, produces controllability high;
(3) present invention can realize either directly through screw extruder, has great industrialization prospect;
(4) the Graphene pattern that the present invention prepares is more regular, and the number of plies is uniform, and its quality has bigger room for promotion.
Detailed description of the invention
Embodiment 1
Utilize screw extruder that amorphous carbon is processed, comprise the following steps:
(1) being added from charge door in screw extruder by the less block coal carrying out screening, coal enters preheating section, and preheating temperature is 200 DEG C, and it is 5min in the time of staying of preheating section;
(2) coal after preheated enters seal section, seal section temperature is 600 DEG C, it is connected with argon, 3A molecular sieve is added from the first charge door, mix with the coal after preheating, being added after a while from the second charge door by borate carrier, coal is 50min in the time of staying of seal section, with N-N-dimethylpropyl on this borate carrier;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 10 DEG C, and screw speed slows down 2/3, and it is 30min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 60% ~ 70% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial coal put into) is 20%.
Embodiment 2
Utilize screw extruder that amorphous carbon is processed, comprise the following steps:
(1) being added from charge door in screw extruder by the less block coal carrying out screening, coal enters preheating section, and preheating temperature is 300 DEG C, and it is 5min in the time of staying of preheating section;
(2) coal after preheated enters seal section, seal section temperature is 800 DEG C, it is connected with argon, 4A molecular sieve is added from the first charge door, mixing with the coal after preheating, added after a while from the second charge door by mica powder carrier, coal is 40min in the time of staying of seal section, with N-ethylperfluoro octyl group sulfonamide on this mica powder carrier, its preparation method obtains for being soaked in N-ethylperfluoro octyl group sulfonamide-alcohol dispersion liquid by mica powder;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 5 DEG C, and screw speed slows down 2/3, and it is 20min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 65% ~ 75% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial coal put into) is 23%.
Embodiment 3
Utilize screw extruder that amorphous carbon is processed, comprise the following steps:
(1) being added from charge door in screw extruder by the less lumped coal spoil carrying out screening, coal enters preheating section, and preheating temperature is 400 DEG C, and it is 5min in the time of staying of preheating section;
(2) gangue after preheated enters seal section, seal section temperature is 900 DEG C, it is connected with argon, 4A molecular sieve is added from the first charge door, mixing with the gangue after preheating, added after a while from the second charge door by mica powder carrier, gangue is 40min in the time of staying of seal section, with N-propyl group perfluorinated octyl sulfuryl amine on this mica powder carrier, its preparation method obtains for being soaked in N-propyl group perfluorinated octyl sulfuryl amine-alcohol dispersion liquid by mica powder;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 5 DEG C, and screw speed slows down 2/3, and it is 30min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 70% ~ 80% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial gangue put into) is 28%.
Embodiment 4
(1) being added from charge door in screw extruder by the activated carbon carrying out screening, activated carbon enters preheating section, and preheating temperature is 200 DEG C, and it is 5min in the time of staying of preheating section;
(2) activated carbon after preheated enters seal section, seal section temperature is 900 DEG C, it is connected with argon, 5A molecular sieve is added from the first charge door, mixing with the activated carbon after preheating, added after a while from the second charge door by perovskite oxide, activated carbon is 30min in the time of staying of seal section, with N-propyl group perfluorinated octyl sulfuryl amine on this perovskite oxide, its preparation method obtains for being soaked in N-propyl group perfluorinated octyl sulfuryl amine-alcohol dispersion liquid by perovskite;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 3 DEG C, and screw speed slows down 2/3, and it is 20min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 70% ~ 80% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial activated carbon put into) is 30%.
Embodiment 5
(1) being added from charge door in screw extruder by the activated carbon carrying out screening, activated carbon enters preheating section, and preheating temperature is 300 DEG C, and it is 8min in the time of staying of preheating section;
(2) activated carbon after preheated enters seal section, seal section temperature is 900 DEG C, it is connected with argon, 3A molecular sieve is added from the first charge door, mixing with the activated carbon after preheating, added after a while from the second charge door by perovskite oxide, activated carbon is 30min in the time of staying of seal section, with N-propyl group perfluorinated octyl sulfuryl amine on this perovskite oxide, its preparation method obtains for being soaked in N-propyl group perfluorinated octyl sulfuryl amine-alcohol dispersion liquid by perovskite;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 5 DEG C, and screw speed slows down 2/3, and it is 10min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 65% ~ 70% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial activated carbon put into) is 30%.
Embodiment 6
(1) being added from charge door in screw extruder by the activated carbon carrying out screening, activated carbon enters preheating section, and preheating temperature is 400 DEG C, and it is 6min in the time of staying of preheating section;
(2) activated carbon after preheated enters seal section, seal section temperature is 1000 DEG C, it is connected with argon, 4A molecular sieve is added from the first charge door, mixing with the activated carbon after preheating, added after a while from the second charge door by molybdenum bisuphide carrier, activated carbon is 40min in the time of staying of seal section, with N-propyl group perfluorinated octyl sulfuryl amine on this molybdenum bisuphide carrier, its preparation method obtains for being soaked in N-propyl group perfluorinated octyl sulfuryl amine-alcohol dispersion liquid by molybdenum bisuphide;
(3) from seal section out after complex namely enter cooling section, this section of temperature is 1 DEG C, and screw speed slows down 2/3, and it is 20min in the time of staying of this section;
(4) cooled section of complex out is discharged from discharging opening, namely obtains the Graphene containing carrier;
After being removed by carrier, this Graphene single layer of crystalline degree is 75% ~ 85% after tested, and Graphene integral thickness is evenly distributed, and for non-single-layer graphene, Graphene productivity (relative to the initial activated carbon put into) is 38%.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, above-described embodiment is only the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, should be appreciated that, those skilled in the art can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (10)
1. one kind utilizes the method that amorphous carbon prepares Graphene, it is characterised in that: comprise the following steps:
Amorphous carbon preheats;
Catalyst is added in the amorphous carbon after preheating;
Amorphous carbon is Pintsch process under catalyst action;
Carbon atom after cracking is deposited on layered vector, obtains the Graphene containing carrier;
Remove carrier, namely obtain Graphene.
2. the method utilizing amorphous carbon to prepare Graphene according to claim 1, it is characterised in that: being accompanied by layered carrier shaping controlling agent, described shaping controlling agent is fluorocarbon surfactant.
3. the method utilizing amorphous carbon to prepare Graphene according to claim 2, it is characterised in that: described fluorocarbon surfactant is one or more in N-N-dimethylpropyl, N-ethylperfluoro octyl group sulfonamide, N-propyl group perfluorinated octyl sulfuryl amine.
4. the method utilizing amorphous carbon to prepare Graphene according to claim 2, it is characterised in that: the complex method of layered carrier and described shaping controlling agent is: be soaked in by layered carrier in the dispersion liquid of described shaping controlling agent.
5. the method utilizing amorphous carbon to prepare Graphene according to claim 1, it is characterised in that: described amorphous carbon is one or more in coal, gangue, activated carbon.
6. the method utilizing amorphous carbon to prepare Graphene according to claim 1, it is characterised in that: described catalyst is one or more in 3A, 4A, 5A molecular sieve.
7. the method utilizing amorphous carbon to prepare Graphene according to claim 1, it is characterised in that: the temperature of described Pintsch process is 500 ~ 1000 DEG C.
8. the method utilizing amorphous carbon to prepare Graphene according to claim 1, it is characterised in that: layered carrier is one or more in borate, mica powder, perovskite, molybdenum bisuphide.
9. utilize, according to any one of claim 1 ~ 8, the method that amorphous carbon prepares Graphene, it is characterised in that: described method is realized by screw extruder.
10. the method utilizing amorphous carbon to prepare Graphene according to claim 9, it is characterized in that: the preheating section for amorphous carbon preheating that described screw extruder includes being sequentially connected to rear end from front end, seal processing sections for what the Graphene containing carrier was formed, strengthen the morphogenetic cooling section of Graphene and the discharging opening discharged for the Graphene containing carrier, wherein seal and processing sections also include near first charge door for catalyst addition of preheating section and be positioned at second charge door 2 for carrier addition of seal section postmedian.
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Cited By (3)
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| CN108203090A (en) * | 2016-12-16 | 2018-06-26 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene |
| CN109775691A (en) * | 2017-11-13 | 2019-05-21 | 新奥石墨烯技术有限公司 | Sulfur doping graphene and preparation method thereof and system, solar battery |
| CN111285371A (en) * | 2020-02-25 | 2020-06-16 | 中国科学院化学研究所 | Method for extruding activated carbon material by utilizing reactive double-screw extrusion system |
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| CN102693843A (en) * | 2012-06-06 | 2012-09-26 | 渤海大学 | Fluorine-containing surfactant modified graphene preparation method for electrode of electric double-layer capacitor |
| CN103288076A (en) * | 2013-06-08 | 2013-09-11 | 新疆师范大学 | Method for preparing multilayer graphene from coal-base raw material |
| CN103572247A (en) * | 2012-07-27 | 2014-02-12 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing thin layer graphene on surface of metal catalyst |
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| CN102502593A (en) * | 2011-10-11 | 2012-06-20 | 中国石油大学(北京) | Preparation method of grapheme or doped graphene or graphene complex |
| CN102693843A (en) * | 2012-06-06 | 2012-09-26 | 渤海大学 | Fluorine-containing surfactant modified graphene preparation method for electrode of electric double-layer capacitor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109775691A (en) * | 2017-11-13 | 2019-05-21 | 新奥石墨烯技术有限公司 | Sulfur doping graphene and preparation method thereof and system, solar battery |
| CN109775691B (en) * | 2017-11-13 | 2024-04-05 | 新奥集团股份有限公司 | Sulfur-doped graphene, preparation method and system thereof, and solar cell |
| CN111285371A (en) * | 2020-02-25 | 2020-06-16 | 中国科学院化学研究所 | Method for extruding activated carbon material by utilizing reactive double-screw extrusion system |
| CN111285371B (en) * | 2020-02-25 | 2021-08-31 | 中国科学院化学研究所 | Method for extruding activated carbon material by utilizing reactive double-screw extrusion system |
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