CN115196621A - Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge - Google Patents
Method and device for preparing graphene by catalyst-assisted microwave excitation metal discharge Download PDFInfo
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Abstract
The invention provides a method and a device for preparing graphene by using a catalyst to assist microwave excitation metal discharge. The invention mixes the carbon source and the catalyst, then lays them in a high temperature resistant container, covers the cover with the metal wire array, and puts them into the microwave special equipment without oxygen. The catalyst absorbs the high temperature and the local plasma in the microwave forming area, the rapid discharge of the front end of the microwave-induced metal wire array can be enhanced, high-density and continuous electric explosion is generated, and the high-temperature and high-chemical-activity plasma rapidly converts a carbon source into graphene. The preparation device comprises catalyst powder, carbon source powder, a powder stirring module, a high-temperature resistant container module, a microwave reaction module and a powder screening module. The method adopts a low-cost carbon source as a raw material to replace expensive graphite oxide prepared by a chemical method, solves the problem of high energy consumption, and simultaneously, the price of microwave equipment is far lower than that of high-voltage pulse power supply equipment, so that the method not only realizes the low-cost graphene manufacturing, but also can realize mass production, and has market competitiveness.
Description
Technical Field
The invention belongs to the field of graphene synthesis, and particularly relates to a method for preparing graphene by using a catalyst to assist microwave excitation metal discharge.
Background
Graphene is a two-dimensional carbon material with a monoatomic layer thickness, and has excellent mechanical properties, high electrical conductivity, high thermal conductivity, high electron mobility and other excellent properties, so that the graphene has wide application prospects in the fields of integrated circuits, battery energy sources, electrode materials and the like. The high price of the graphene powder is one of the main factors limiting the application market.
Common methods for producing thin-layer graphene include: mechanical exfoliation, epitaxial growth, graphene oxide reduction, chemical vapor deposition, liquid phase exfoliation, and high temperature reduction. The size of graphene is difficult to control by a mechanical stripping method, and the method is not suitable for large-scale production; the epitaxial growth method and the chemical vapor deposition method can produce high-quality graphene, but the cost is too high; the liquid phase stripping method can cause a great amount of structural defects of the graphene in the preparation process, and influence partial performances of the graphene; the high-temperature reduction method can prepare the thin-layer graphene with fewer defects. Microwave heating is a more mode in a high-temperature reduction method, and has the advantages of high heating speed, uniform heating and the like. In chinese patent CN 109292761A, in the method reported in this patent, light source irradiation and microwave heating are used cooperatively, so that the problems of insufficient light irradiation area, no light irradiation of graphene oxide under the surface layer, and the like obviously exist, and the efficiency of graphene production is greatly affected. Similarly, in chinese patent CN 110127681A, a method for preparing graphene by catalysis and microwave method, the method reported in this patent can convert graphite into graphene, the whole process involves pretreatment of graphite by various chemical reagents and later-stage graphene pickling, the time consumption is long, and a large amount of chemical waste liquid is generated, which is obviously not suitable for mass production. The flash evaporation graphene technology is a simple and efficient graphene preparation technology, and Chinese invention patent CN 202010865177.3 proposes to fill a carbon source between two electrodes and convert the carbon source into graphene through high-voltage discharge at two ends of the electrodes under a certain condition. However, the method has the defects of large energy consumption, expensive power supply equipment, limited yield and the like. And the plasma generated by the method is in a form of stamping discharge by virtue of the electrodes, part of powder close to the electrodes is easy to form graphene, and the middle part of the powder is not acted by the plasma and is not converted into the graphene, so that the method has the defects of low yield and uneven reaction. Moreover, the high-pressure flash evaporation mode is complex in operation in the aspects of material changing, filling and other processes, and has a small challenge on capacity expansion. With the coming of a new round of growing demand for new energy materials in the market, a low-cost and efficient graphene production mode is urgently needed.
Disclosure of Invention
Aiming at the technical defects of the graphene prepared by the existing microwave method and flash evaporation method, the invention provides a method and a device for preparing graphene by catalyst-assisted microwave excitation metal discharge. The invention mixes the carbon source and the catalyst, then lays them in a high temperature resistant container, covers the cover with the metal wire array, and puts them into the microwave special equipment without oxygen. The catalyst absorbs the high temperature and the local plasma in the microwave forming area, the rapid discharge of the front end of the microwave induced metal wire array can be enhanced, the high-density and continuous electric explosion is generated, and the high-temperature and high-chemical-activity plasma rapidly converts the carbon source into the graphene. The method adopts a low-cost carbon source as a raw material to replace expensive graphite oxide prepared by a chemical method, solves the problem of high energy consumption, and simultaneously, the price of microwave equipment is far lower than that of high-voltage pulse power supply equipment, so that the method not only realizes the low-cost graphene manufacturing, but also can realize mass production, and has market competitiveness.
The invention provides a method and a device for preparing graphene by catalyst-assisted microwave-excited metal discharge, wherein the method comprises the following steps: in an oxygen-free closed microwave radiation environment, a high-conductivity carbon quantum material absorbs microwaves to generate local high temperature and local plasma, the microwaves induce the metal-carbon quantum material to discharge to enhance the local plasma, and finally, carbon atoms of the carbon-containing raw material are reduced and gasified in the generated high-temperature high-activity plasma flow environment to be recombined into graphene.
The invention provides a method and a device for preparing graphene by catalyst-assisted microwave-excited metal discharge, wherein the device comprises the following steps: the device comprises catalyst powder, carbon source powder, a powder stirring module, a high-temperature resistant container module, a microwave reaction module and a powder screening module. The powder stirring module is used for uniformly mixing catalyst powder and carbon source powder to prepare a raw material; the high-temperature resistant container module comprises a cover containing a metal wire array, a high-temperature resistant container and a heat insulation layer, is used as a container for containing raw materials and is arranged in the microwave reaction module; the microwave reaction module comprises a special microwave oven and anaerobic environment maintaining equipment, the special microwave oven is used for exciting a metal wire and a catalyst to discharge to generate high-temperature and high-activity plasma, so that raw materials are converted into graphene powder under the action of high-temperature plasma flow, and the anaerobic environment maintaining equipment is used for maintaining the interior of the special microwave oven in an anaerobic environment. The powder screening module is used for physically filtering out graphene with coarse grain size and graphene with micro grain size.
The invention provides a method and a device for preparing graphene by using a catalyst to assist microwave excitation metal discharge, which are characterized by comprising the following specific steps:
(1) The catalyst material and the carbon source are uniformly mixed through a powder stirring module according to the mass ratio of 1.
(2) And (2) paving a layer of catalyst material with the thickness of about 1mm at the bottom of the high-temperature resistant container to serve as a bottom auxiliary discharge material, and then uniformly paving the mixed powder of the catalyst and the carbon source in the step (1) on a bottom auxiliary material, wherein the thickness of the mixed powder is about 5-20 mm. Covering with a cover with a metal wire array, and placing the container in a microwave special device in an oxygen-free environment.
(3) Starting the oxygen-free environment maintaining equipment to enable the oxygen concentration in the microwave special furnace to be lower than 5%, then starting a power supply of the microwave special furnace, exciting electrons in the metal wire array to actively move after the microwaves are radiated for about 1 second to cause point discharge, absorbing the microwaves by the catalyst material at the bottom, not only quickly heating the carbon source to be more than 500 ℃, but also generating plasma and guiding the plasma generated by the metal wire array at the top to act on the carbon source. And (3) the strong plasma flow causes the carbon chemical bonds in the carbon source to break, and recombination arrangement is carried out to form graphene.
(4) And (4) turning off the microwave power supply, taking out the powder after the discharge reaction in the high-temperature resistant container, and separating the powder in the crucible by using a micron-sized fine sieve. The powder with fine particle size reaches the preparation standard, and then the materials are discharged and bagged; collecting powder with coarse grain size for the mixing operation in the step (1).
The catalyst material in the step (1) can be a carbonaceous material with high conductivity, high microwave absorption efficiency, such as vermicular graphite, graphene and the like, or metal/metal oxide nanoparticle powder. The mass ratio is not limited to the mixing ratio of 1.
The carbon source in the step (1) can be carbon materials such as bamboo charcoal, graphite, charcoal, activated carbon and the like, and can also be biomass materials such as straw and the like.
The powder stirring module in the step (1) can be a sand mill, a ball mill, a pulverizer and the like, and the stirring mode can be dry grinding or wet grinding.
In the metal wire array in the step (2), the metal wire with a diameter smaller than 2mm is a high temperature resistant tungsten wire, or other metal or alloy materials with characteristics of high temperature resistance, low electron emission power, high microwave absorption rate and the like, or a mixture of metal and wave-absorbing materials.
The wire array of step (2), wherein the wires are vertically arranged on the cover like a wooden stake, and then one side of the wire array is covered on the mixed powder with a distance of about 1-3mm from the mixed powder.
The wire array in step (2) is not limited to the shape of a wire, and may be in various shapes such as a metal mesh, a mesoporous metal plate, and a foam metal plate.
The high-temperature resistant container in the step (2) can be a crucible made of high-temperature resistant materials such as a corundum crucible, a corundum mullite crucible, a fused quartz crucible, a ceramic crucible, an aluminum silicate crucible and the like.
The oxygen-free environment maintaining equipment in the step (3) can be nitrogen supplementing equipment or other inert gas supplementing equipment, and provides a gas atmosphere with low oxygen concentration in a microwave special oven; it can also be vacuum pumping equipment, and provides low-pressure environment in the microwave special oven. The oxygen-free environment maintaining equipment comprises an oxygen concentration monitor, and gas circulation is started when the oxygen concentration is higher than 0.1%.
The special microwave oven in the step (3) can be an industrial microwave oven with microwave power of ten thousand watts or a household microwave oven with microwave power of kilowatt.
The microwave special oven in the step (3) can be provided with a plurality of microwave tubes, and the directions of the microwaves emitted by the plurality of microwave tubes have a common intersection point.
The method of the invention has the following advantages:
(1) The microwave oven is used as main energy supply equipment, so that the energy consumption is low, the process of instruments and equipment is mature and common, and the price is substantial. And the microwave has penetrability and direction adjustability, is convenient to operate and is suitable for continuous production.
(2) The microwave-excited metal discharge method can be used for preparing high-quality graphene materials, and has the advantages of no chemical reagent, no toxicity, no pollution and the like in the production process. The microwave-excited metal discharge method assisted by the catalyst can quickly convert a carbon source into graphene within seconds, and has excellent microwave penetrability and spatial transmissibility, and the theoretical yield is far greater than that of a flash evaporation graphene technology.
(3) The microwave heating method is one of the technologies for rapidly obtaining high-quality carbon sources from biomass materials, and the method and the equipment can be used for preparing biomass charcoal and biomass graphene by combining with the method, so that the preparation time and the preparation cost from biomass to graphene are effectively shortened.
(4) The microwave excites electrons in the metal wire to actively move, and the electrons are instantaneously discharged at the tip of the metal wire to generate a large amount of high-temperature and high-chemical-activity plasma flow in a short time, so that carbon-carbon bonds can be easily broken by acting on a carbon source, and the carbon atoms are recombined at high temperature to form graphene.
(5) The catalyst is made of a highly conductive carbon quantum material, has the characteristic of high microwave absorption, can generate local high temperature under microwave heating, assists in heating carbon source powder, can generate electric sparks to guide high-temperature and high-activity plasma flow at the tip of a metal wire to act on the carbon source powder, enhances the local plasma, and increases the speed and uniformity of graphene preparation through microwave excitation metal discharge.
(6) The high-temperature and high-activity plasma generated by microwave excitation can rapidly reduce free radicals in the carbon source, strip the carbon layer, and expand to obtain few-layer graphene.
(7) The high-temperature and high-activity plasma generated by microwave excitation can be used for biomass carbonization, graphene synthesis and the like, and can also be used for synthesizing metal-carbon compounds or metal nanoparticle structures coated by graphene. When the starting material is a mixture of metal particles and carbon material, the high temperature, high activity plasma jet environment causes the bonding of metal atoms to carbon atoms to form metal carbides.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the steps required in the implementation case are shown in the form of drawings and described in detail below.
FIG. 1 is a diagram of an apparatus for preparing graphene by microwave-excited metal discharge assisted by a catalyst in an example;
FIG. 2 is a schematic diagram of microwave-induced wire discharge;
FIG. 3 is a diagram of a process for microwave-induced wire discharge;
fig. 4 is an appearance diagram of a graphene product prepared by a catalyst-assisted microwave excitation metal discharge device;
fig. 5 is an XRD data pattern of graphene products prepared by the catalyst-assisted microwave-excited metal discharge device;
fig. 6 is a raman data diagram of a graphene product prepared by a catalyst-assisted microwave-excited metal discharge device.
Detailed Description
For convenience of illustration of the contents of the present invention, examples are listed below, and the contents of the present examples are not to be construed as specifically limiting the present invention. The applicant asserts that the present invention is illustrated by examples to illustrate the detailed process flow and technical details of the present invention, but not to limit the scope of the claims of the present invention, and does not imply that the present invention must be implemented by relying on the detailed process flow described above. It will be understood by those skilled in the art that modifications of certain details of the invention, equivalent substitutions of materials and additions of auxiliary components are within the scope and disclosure of the invention.
Example 1
Referring to fig. 1, a method and an apparatus introduction according to the technical solution of the present invention are described, and the apparatus specifically includes: the device comprises carbon source powder 1, powder stirring equipment 2, catalyst powder 3, a high-temperature resistant container 4, a conveyor belt 5, a metal wire array 5, a high-temperature resistant container cover 6, a microwave oven loose-leaf door 7, a microwave oven 8, a connecting column 9, a microwave oven control power supply 10, nitrogen equipment 11, an air valve 12, an air guide pipe 13, a quartz perspective window 14, a microwave radiation source 15, mixed powder after microwave treatment 16, powder screening equipment 17, graphene powder 18, powder packaging equipment 19 and a graphene product 20.
The specific operation method comprises the following steps:
step (1): the catalyst material 3 and the carbon source powder 1 were uniformly mixed through the powder stirring apparatus 2 at a mass ratio of 1.
Step (2): and (2) paving a layer of catalyst powder 3 with the thickness of about 1mm at the bottom of a high-temperature resistant container 4 to serve as a bottom auxiliary discharge material, and then uniformly and flatly paving the mixed powder of the catalyst and the carbon source in the step (1) on a bottom auxiliary material, wherein the thickness of the mixed powder is about 5-20 mm. The high temperature resistant container cover 6 is provided with a metal wire array 5, the container 4 is placed on the conveyor belt 4, the loose-leaf door 7 of the microwave oven is opened, and the container is conveyed into the microwave oven 8.
And (3): the nitrogen device 11 is started, the air valve 12 is opened, the oxygen concentration in the microwave oven 8 is enabled to be lower than 5%, then the microwave oven control power supply 10 is started, the microwave radiation source 15 radiates microwaves for about 1 second, then the microwaves excite electrons in the metal wire array 5 to actively move, tip discharge is caused, the catalyst material at the bottom absorbs the microwaves, the carbon source can be rapidly heated to be higher than 500 ℃, plasmas can be generated, and the plasmas generated by the metal wire array at the top are guided to act on the carbon source. And (3) the strong plasma flow causes the carbon chemical bonds in the carbon source to be broken, recombination arrangement is carried out, and the carbon source is converted into graphene.
And (4): and (3) closing the microwave control power supply 10, opening the microwave loose-leaf door 7, taking out the mixed powder 16 subjected to microwave treatment in the high-temperature resistant container 4, and separating the catalyst material 3 from the graphene powder 18 by using powder screening equipment 17 with 200-400 meshes. The separated graphene powder 18 is weighed, packed and packaged by a powder packaging device 19, and finally, a bagged or bottled graphene product 20 is obtained.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A method and a device for preparing graphene by catalyst-assisted microwave excitation metal discharge are characterized in that the method comprises the following steps: in an oxygen-free closed microwave radiation environment, a high-conductivity carbon quantum material absorbs microwaves to generate local high temperature and local plasma, the front end of a microwave-induced metal wire array can be enhanced to discharge rapidly, high-density and continuous electric explosion is generated, carbon atoms of a carbon-containing raw material are reduced and gasified in a high-temperature and high-activity plasma flow environment to be recombined into graphene, and the technology of converting a carbon source into the graphene by utilizing the high-temperature and high-activity plasma generated by microwave-induced metal is included in the principle of the method.
2. The method and the device for preparing graphene by using catalyst-assisted microwave-excited metal discharge according to claim 1, wherein the device comprises: the device comprises catalyst powder, carbon source powder, a powder stirring module, a high-temperature resistant container module, a microwave reaction module and a powder screening module;
the powder stirring module is used for uniformly mixing catalyst powder and carbon source powder to prepare a raw material; the high-temperature resistant container module comprises a cover containing a metal wire array, a high-temperature resistant container and a heat insulation layer, is used as a container for containing raw materials and is arranged in the microwave reaction module; the microwave reaction module comprises a special microwave oven and oxygen-free environment maintaining equipment, wherein the special microwave oven is used for exciting a metal wire and a catalyst to discharge to generate high-temperature and high-activity plasma, so that raw materials are converted into graphene powder under the action of high-temperature plasma flow; the anaerobic environment maintaining equipment is used for maintaining the interior of the special microwave oven in an anaerobic environment; the powder screening module is used for physically filtering out graphene with coarse grain size and graphene with micro grain size.
3. The method and apparatus for preparing graphene by catalyst-assisted microwave-excited metal discharge according to claim 2, wherein the catalyst powder may be a carbonaceous material with high conductivity and high microwave absorption efficiency, such as vermicular graphite, graphene, etc., or a metal/metal oxide nanoparticle powder, and the mass ratio is not limited to 1;
the carbon source powder can be carbon materials such as bamboo charcoal, graphite, charcoal, activated carbon and the like, and can also be biomass materials such as straws and the like;
the powder stirring module can be a sand mill, a ball mill, a pulverizer and the like, and the stirring mode can be dry grinding or wet grinding.
4. The method and the device for preparing graphene by catalyst-assisted microwave-excited metal discharge according to claim 2, wherein the metal wire array, in which the diameter of the metal wire is less than 2mm, is a high-temperature-resistant tungsten wire, or other metal or alloy materials with the characteristics of high temperature resistance, low electron emission power, high microwave absorption rate, or a mixture of metal and wave-absorbing materials;
the metal wire array is vertically arranged on the cover like a wood pile, and then one surface of the metal wire array faces downwards to cover the mixed powder at a distance of about 1-3mm from the mixed powder;
the wire array is not limited to the shape of a wire, and may be in various shapes such as a metal mesh, a mesoporous metal plate, and a foam metal plate.
5. The method and apparatus for preparing graphene by catalyst-assisted microwave-excited metal discharge according to claim 2, wherein the high temperature resistant container is a crucible made of high temperature resistant materials such as corundum crucible, corundum-mullite crucible, fused silica crucible, ceramic crucible, and aluminum silicate crucible.
6. The method and the device for preparing graphene by using the catalyst-assisted microwave-excited metal discharge as claimed in claim 2, wherein the oxygen-free environment maintaining device can be a nitrogen supplementing device or other inert gas supplementing devices, and a gas atmosphere with low oxygen concentration is provided in a microwave-dedicated furnace; or vacuum pumping equipment, and provides a low-pressure environment in a microwave special oven; the oxygen-free environment maintaining equipment comprises an oxygen concentration monitor, and gas circulation is started when the oxygen concentration is higher than 0.1%.
7. The method and the device for preparing graphene by catalyst-assisted microwave-excited metal discharge according to claim 2, wherein the special microwave oven can be an industrial microwave oven with a microwave power of ten thousand watts, or a household microwave oven with a microwave power of kilowatts; the microwave special oven can be provided with a plurality of microwave tubes, and the directions of the microwaves emitted by the plurality of microwave tubes have a common intersection point.
8. The invention provides a method and a device for preparing graphene by catalyst-assisted microwave-excited metal discharge, which are provided by the invention according to claim 1, and are characterized in that the specific method comprises the following steps:
(1) Uniformly mixing a catalyst material and a carbon source through a powder stirring module according to the mass ratio of 1;
(2) Laying a layer of catalyst material with the thickness of about 1mm at the bottom of the high-temperature resistant container to serve as a bottom layer auxiliary discharge material, and then uniformly and flatly laying mixed powder of the catalyst and the carbon source in the step (1) on a bottom layer auxiliary material, wherein the thickness of the mixed powder is about 5-20 mm; covering a cover with a metal wire array, and putting the container into special microwave equipment in an oxygen-free environment;
(3) Starting oxygen-free environment maintaining equipment to enable the oxygen concentration in the microwave special furnace to be lower than 5%, then starting a power supply of the microwave special furnace, exciting electrons in the metal wire array to actively move after the microwaves are radiated for about 1 second to cause point discharge, absorbing the microwaves by a catalyst material at the bottom, rapidly heating a carbon source to above 500 ℃, generating plasma, and guiding the plasma generated by the top metal wire array to act on the carbon source; the strong plasma flow causes the breakage of carbon chemical bonds in the carbon source, and recombination arrangement is carried out to form graphene;
(4) Turning off a microwave power supply, taking out the powder after the discharge reaction in the high-temperature resistant container, and separating the powder in the crucible by using a micron-sized fine sieve; the powder with fine particle size reaches the preparation standard, and then is discharged and bagged; collecting powder with coarse grain size for the mixing operation in the step (1).
9. The method and the device for preparing graphene by using catalyst-assisted microwave-excited metal discharge as claimed in claim 1, wherein the specific device in the embodiment comprises: carbon source powder, powder stirring equipment, catalyst powder, a high-temperature-resistant container, aluminum silicate heat-insulating cotton, a conveyor belt, a metal wire array, a high-temperature-resistant container cover, a microwave oven loose-leaf door, a microwave oven, a connecting column, a microwave oven control power supply, nitrogen equipment, an air valve, an air duct, a quartz perspective window, a microwave radiation source, microwave-treated mixed powder, powder screening and filtering equipment, graphene powder, powder packaging equipment and a graphene product.
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