CN105948030A - Device and method for quickly preparing graphene under synergistic actions of electric field and magnetic field - Google Patents
Device and method for quickly preparing graphene under synergistic actions of electric field and magnetic field Download PDFInfo
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Abstract
The invention provides a device and method for quickly preparing graphene under synergistic actions of an electric field and a magnetic field. The technical scheme is as follows: the device comprises a graphite rod used as a negative electrode, a graphite cylinder used as a positive electrode, a ceramic crucible and a water tank, wherein the graphite rod is suspended in the graphite cylinder; the graphite cylinder is suspended in the ceramic crucible; an induction coil is arranged around the graphite cylinder; a high-frequency induction coil is wound outside the ceramic crucible; and the water tank is filled with cooling water. The method comprises the following steps: an electrolyte solution is added into the ceramic crucible, a 5-10V voltage is applied between the graphite rod and the graphite cylinder, and meanwhile, the induction coil around the graphite cylinder is electrified to generate an electromagnetic field, so that an inductive loop is generated on the graphite cylinder surface, and the graphene is stripped from the graphite cylinder surface under the interactions of the electric field and magnetic field generated on the graphite cylinder surface. No concentrated sulfuric acid, strong alkali or strong oxidizer is added in the whole preparation process, so the method is green and environment-friendly, and is simple in technique and convenient for industrialized production.
Description
Technical field:
The present invention relates to the preparation field of Graphene, be specifically related to a kind of electric field and magnetic field synergism and quickly prepare the device and method of Graphene.
Background technology:
Since English physicist finds and disclose the character that Graphene is unique, Graphene, thence into the popular visual field, becomes pearlescent nova in material family, more has people referred to as " changing the material of 21 century ".In recent years, Graphene, as the advanced material with carbon element of a kind of uniqueness, was starting a subversiveness Industrial Revolution have swept the globe.It is the unique Two Dimensional Free state atomic crystal existed having now been found that in the world, it it is the basic cell structure constructing the sp2 hydridization carbon such as zero dimension fullerene, one-dimensional CNT, said three-dimensional body phase graphite, also being the thinnest, the nano material that intensity is the highest having been found that in the world, its intensity is 10 times of ordinary steel iron material.There is superpower electric conductivity simultaneously, be the material that known resistivity is minimum in the world, additionally, Graphene also has outstanding room temperature heat conductivity and light transmission.Unique and the excellent characteristic of Graphene makes industrial circle see its application potential in fields such as electronics, space flight, military project, biology, new forms of energy, quasiconductors, becomes international study hotspot and focus of the competition.
2004, the scientist of Univ Manchester UK uses mechanical stripping method prepare first and observe single-layer graphene, open the research boom of grapheme material, new graphene preparation method emerges in an endless stream, such as chemical stripping method, chemical vapour deposition technique, plasma etching method, epitaxial growth method, electrochemical process, arc process, solvent-thermal method etc..But, low cost, large area, high-quality Graphene magnanimity technology of preparing are still ought main difficulty that up till now field was faced and challenge.The most conventional preparation method mainly has four kinds: mechanical stripping method, chemical vapour deposition technique, epitaxial growth method, oxidation-reduction method.
Micromechanics stripping method can prepare high-quality graphene, but can not meet the production requirement of industrialization, scale.Two British scientists separate graphite flake from graphite, are then bonded on a kind of special adhesive tape on the two sides of thin slice, tear adhesive tape, just graphite flake can be divided into two.The most so operating, then thin slice is more and more thinner, and finally, they have obtained the thin slice being only made up of one layer of carbon atom, here it is Graphene, method is only used for laboratory at present and prepares.
Chemical vapour deposition technique (CVD) is that reacting substance issues biochemical reaction at gaseous condition, generates solid matter and is deposited on the solid matrix surface of heating, and then the Technology of prepared solid material.Concrete grammar is first to form one layer of transiting metal film at substrate surface, with this metal film as catalyst, with CH4 as carbon source, forms graphene sheet layer on transition metal films surface, obtain Graphene finally by acid liquid corrosion metal film after gas phase is dissociated.Chemical vapour deposition technique can prepare the graphene film material of large area and excellent performance, and existing technique is immature and relatively costly its large-scale application that all limits, and therefore also needs to explore further, perfect.
SiC epitaxy can get monolayer or the ideal Graphene of minority layer, but relatively costly.The semi-conducting material of a kind of excellent performance of SiC, compatible (need not transfer) mutually with current Si base semiconductor technique, the Graphene of the most this method growth is one of effective way most possibly realizing C base integrated circuit.But monocrystal SiC is expensive, the cost of manufacture of Graphene is the highest, and growth conditions is the harshest, is the most also difficult to large area and prepares, and is unfavorable for the transfer of follow-up Graphene.
Oxidation-reduction method is that native graphite and strong acid and oxidizing species react generation graphite oxide (GO), it is prepared as graphene oxide (mono-layer graphite oxide) through ultrasonic disperse, add reducing agent and remove the oxy radical on graphite oxide surface, such as carboxyl, epoxy radicals and hydroxyl, obtain Graphene.Oxidation-reduction method can prepare substantial amounts of Graphene with relatively low cost, becomes at present and prepares the method that the efficiency of Graphene is the highest.But in oxidation-reduction process, it is very easy to irreversible agglomeration, and the electronic structure of Graphene and perfection of crystal are easily subject to the destruction of strong oxidizer, even if after being reduced by strong reductant, the prototype structure of Graphene can not be recovered completely, and then limits the Graphene application at accurate microelectronic to a certain extent.The more important thing is, due to strong acid and the use of strong oxidizer, strong reductant etc., Graphene preparation process produces substantial amounts of waste liquid, serious environmental pollution can be caused.
Summary of the invention:
The present invention is for overcoming above-mentioned deficiency, it is provided that a kind of electric field and magnetic field synergism quickly prepare the device and method of Graphene, and it is quality controllable, is suitable for industrialization and produces.
The electric field of the present invention and magnetic field synergism quickly prepare the device of Graphene, the technical scheme used is: include the graphite rod as negative pole, graphite cylinder, ceramic crucible and tank as positive pole, described graphite rod suspends and is located in graphite cylinder, described graphite cylinder suspends and is located in ceramic crucible, described graphite cylinder is provided around induction coil, being wound with radio-frequency induction coil outside described ceramic crucible, described tank is built with cooling water.
Further, the distance between described graphite rod and graphite cylinder is 20-50mm, is arranged such, and has suitable electric field intensity, and the peeling rate of Graphene is fast.
The method that the electric field of the present invention and magnetic field synergism quickly prepare Graphene, the technical scheme used is: add electrolyte solution in ceramic crucible, the voltage of 5-10V is applied between graphite rod and graphite cylinder, produce electromagnetic field to the induction coil energising around graphite cylinder simultaneously, make graphite cylinder surface produce inductive loop, occur on graphite cylinder surface electric field to make Graphene from graphite cylinder sur-face peeling with the interaction in magnetic field.
Further, the frequency of described induction coil is 4000-10000HZ, and the power of radio-frequency induction coil is 10-20KW.So essence, the peeling rate making Graphene is fast.
Further, graphite used by described graphite rod and graphite cylinder is the isostatic pressed high purity graphite of 99.9%, and its pressure direction is consistent, quality good, and the peeling rate making Graphene is fast.
Further, described electrolyte solution is potassium sulfate and dilute sulfuric acid aqueous solution, and both ratios are 1:4, and its electrolysis effectiveness is good.
Further, the spacing between described graphite cylinder and ceramic crucible is more than 100mm, is arranged such, and the peeling rate of Graphene is fast.
The invention has the beneficial effects as follows: the present invention uses isostatic pressed high purity graphite to make graphite rod and graphite cylinder as two electrodes, graphite rod is negative pole, graphite cylinder is positive pole, electrode is placed in ceramic crucible container, certain proportion potassium sulfate is put into and electrolyte solution that dilute sulfuric acid is configured in ceramic crucible container, ceramic crucible container exterior installs radio-frequency induction coil, graphite cylinder connects the positive pole of power supply, graphite cylinder connects power cathode, the electric field synergistic effect produced between the eddy current and the both positive and negative polarity that are produced by radio-frequency induction coil, graphite cylinder graphite is made quickly to peel off in making the electrolyte solution in solution enter graphite cylinder surface, finally give thin graphene.The present invention does not add concentrated sulphuric acid, highly basic and strong oxidizer in whole preparation process, and environmental protection, technique is simple, be easy to industrialization produces.
Accompanying drawing illustrates:
Fig. 1 is the structural representation of device in the present invention.
Detailed description of the invention:
Embodiment one
With reference to Fig. 1, the electric field of the present invention and magnetic field synergism quickly prepare the device of Graphene, including the graphite rod 1 as negative pole, the graphite cylinder 2 as positive pole, ceramic crucible 3 and tank 5, described graphite rod 1 suspends and is located in graphite cylinder 2, described graphite cylinder 2 suspends and is located in ceramic crucible 3, and spacing between the two is more than 100mm, and described graphite cylinder 2 is provided around induction coil, being wound with radio-frequency induction coil 4 outside described ceramic crucible 3, described tank 5 is built with cooling water.Distance between described graphite rod 1 and graphite cylinder 2 is 20mm.
The method that the electric field of the present invention and magnetic field synergism quickly prepare Graphene, electrolyte solution is added in ceramic crucible 3, the voltage of 5V is applied between graphite rod 1 and graphite cylinder 2, produce electromagnetic field to the induction coil energising around graphite cylinder 2 simultaneously, make graphite cylinder 2 surface produce inductive loop, occur on graphite cylinder 2 surface electric field to make Graphene from graphite cylinder 2 sur-face peeling with the interaction in magnetic field.The frequency of described induction coil is 4000HZ, and the power of radio-frequency induction coil 4 is 20KW.Graphite used by described graphite rod 1 and graphite cylinder 2 is the isostatic pressed high purity graphite of 99.9%.Described electrolyte solution is potassium sulfate and dilute sulfuric acid aqueous solution, and both ratios are 1:4.
Embodiment two
Unlike embodiment one, the distance between graphite rod 1 and graphite cylinder 2 in the present embodiment is 30mm, and the frequency of induction coil is 8000HZ.
Embodiment three
Unlike embodiment one, the distance between graphite rod 1 and graphite cylinder 2 in the present embodiment is 40mm, applies the voltage of 8V between graphite rod 1 and graphite cylinder 2, and the frequency of induction coil is 10000HZ, and the power of radio-frequency induction coil 4 is 10KW.
Embodiment four
Unlike embodiment one, the distance between graphite rod 1 and graphite cylinder 2 in the present embodiment is 50mm, applies the voltage of 10V between graphite rod 1 and graphite cylinder 2, and the frequency of induction coil is 10000HZ, and the power of radio-frequency induction coil 4 is 10KW.
Various embodiments above makes the frequency of the radial distance between graphite rod 1 and graphite cylinder 2 and two kinds of induction coils be mutually matched to make equipment preferably work.
Claims (8)
1. an electric field and magnetic field synergism quickly prepare the device of Graphene, it is characterised in that: include the stone as negative pole
Inker (1), graphite cylinder (2), ceramic crucible (3) and tank (5) as positive pole, described graphite rod (1) suspends
Being located in graphite cylinder (2), described graphite cylinder (2) suspends and is located in ceramic crucible (3), described graphite cylinder (2)
Being provided around induction coil, be wound with radio-frequency induction coil (4) outside described ceramic crucible (3), described tank (5) is built-in
There is cooling water.
A kind of electric field the most as claimed in claim 1 and magnetic field synergism quickly prepare the device of Graphene, it is characterised in that:
Radial distance between described graphite rod (1) and graphite cylinder (2) is 20-50mm.
3. the method that an electric field quickly prepares Graphene with magnetic field synergism, it is characterised in that: to ceramic crucible (3)
Interior addition electrolyte solution, applies the voltage of 5-10V between graphite rod (1) and graphite cylinder (2), gives graphite simultaneously
Radio-frequency induction coil (4) energising that the induction coil of cylinder (2) surrounding and ceramic crucible (3) are wound around outward produces electromagnetic field,
Make graphite cylinder (2) surface produce inductive loop, occur on graphite cylinder (2) surface electric field to make with the interaction in magnetic field
Graphene is from graphite cylinder (2) sur-face peeling.
A kind of electric field the most as claimed in claim 3 and magnetic field synergism quickly prepare the device of Graphene, it is characterised in that:
The frequency of described induction coil is 4000-10000HZ, and the power of radio-frequency induction coil (4) is 10-20KW.
The method that a kind of electric field the most as claimed in claim 3 and magnetic field synergism quickly prepare Graphene, its feature exists
In: graphite used by described graphite rod (1) and graphite cylinder (2) is the isostatic pressed high purity graphite of 99.9%.
The method that a kind of electric field the most as claimed in claim 3 and magnetic field synergism quickly prepare Graphene, its feature exists
In: described electrolyte solution is potassium sulfate and dilute sulfuric acid aqueous solution.
A kind of electric field the most as claimed in claim 1 and magnetic field synergism quickly prepare the device of Graphene, it is characterised in that:
Spacing between described graphite cylinder (2) and ceramic crucible (3) is more than 100mm.
The method that a kind of electric field the most as claimed in claim 6 and magnetic field synergism quickly prepare Graphene, it is characterised in that:
The ratio of potassium sulfate and dilute sulfuric acid aqueous solution is 1:4.
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| CN107032336A (en) * | 2017-06-16 | 2017-08-11 | 成都新柯力化工科技有限公司 | The alternating electric field method that continuously stripping prepares graphene is utilized under a kind of dry powder state |
| CN107311154A (en) * | 2017-07-21 | 2017-11-03 | 鄢平 | A kind of method for preparing nanometer three-dimensional grapheme |
| CN107364847A (en) * | 2017-06-28 | 2017-11-21 | 闫守文 | A kind of preparation method of graphene and its graphene being prepared |
| CN107364848A (en) * | 2017-06-28 | 2017-11-21 | 闫守文 | Method and the graphene that is prepared using preparing graphite alkene |
| CN109019580A (en) * | 2018-09-27 | 2018-12-18 | 深圳天元羲王材料科技有限公司 | A kind of graphene purifying plant and method |
| CN114195140A (en) * | 2021-12-31 | 2022-03-18 | 江苏大学 | Method for preparing controllable graphene through electrode and magnetic field regulation and control ion intercalation |
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| CN114195140A (en) * | 2021-12-31 | 2022-03-18 | 江苏大学 | Method for preparing controllable graphene through electrode and magnetic field regulation and control ion intercalation |
| CN114195140B (en) * | 2021-12-31 | 2024-02-09 | 江苏大学 | Method for preparing controllable graphene by electrode and magnetic field regulation ion intercalation |
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Application publication date: 20160921 |