CN105399089A - Graphene generation method, device and equipment based on arbitrary substrate - Google Patents

Graphene generation method, device and equipment based on arbitrary substrate Download PDF

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CN105399089A
CN105399089A CN201510933166.3A CN201510933166A CN105399089A CN 105399089 A CN105399089 A CN 105399089A CN 201510933166 A CN201510933166 A CN 201510933166A CN 105399089 A CN105399089 A CN 105399089A
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carbon
metal alloy
substrate
metal
alloy
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CN105399089B (en
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张淼
茆胜
慈立杰
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INSTITUTE OF NEW ENERGY SHENZHEN
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Abstract

The invention provides a graphene generation method based on arbitrary substrate, wherein the graphene generation method includes the steps: generating a carbon metal alloy from a metal and carbon; controlling a temperature to be higher than a melting point of the carbon metal alloy, and flow-coating the surface of the substrate with the liquid carbon metal alloy; and carrying out segregation at an interface of the carbon metal and the substrate, and conducting to remove the liquid carbon metal alloy, and generating a graphene thin film. Through the carbon metal alloy segregation way, the liquid carbon alloy material can be conveniently conducted to remove, so that the graphene thin film can be generated on arbitrary substrate, participation of etching, water and organic solvents are not required, and the limitation of the generated graphene on the substrate and the limitation of participation of other ingredients during graphene generation are reduced.

Description

Based on the Graphene generation method of any substrate, device and equipment
Technical field
The invention belongs to the rare field of graphite, particularly relate to based on the Graphene generation method of any substrate, device and equipment.
Background technology
Graphene separates from graphite material, the two dimensional crystal only having one deck atom Baidu be made up of carbon atom.Because its ductile strength is high, conduct electricity very well and feature that light transmission is good, such as, its breaking tenacity is also higher more than 200 times than steel, its conductivity is higher than the conductivity of silver, replaces silicon, will make the travelling speed hundreds of times soon of computer processor with Graphene, Graphene is almost transparent and compactness good in addition, can transparent electronic product raw material be used as, apply widely, and using value be very high.
In the making processes of Graphene, the method of current use comprises chemical gaseous phase deposition method, by the mixed gas of methane and hydrogen, reaction compartment is incorporated into by inlet manifold, mixed gas sorption on a substrate, there is the chemical reaction of migration and film forming, under certain humidity, generate Graphene.
The Graphene generation method of current use, can obtain Graphene, but needs the participation of etching reagent, water and organic solvent in process of production, and making substrate be limited to its surface needs smooth, or requires that the curvature on its surface is less.Therefore, need in prior art to use more batching to participate in, and the substrate generating Graphene is restricted.
Summary of the invention
The object of the present invention is to provide a kind of Graphene generation method based on any substrate, need to use more batching to participate in solve in prior art, and the problem that the substrate generating Graphene is restricted.
First aspect, embodiments provide a kind of Graphene generation method based on any substrate, described method comprises:
By metal and carbon Formed metal alloy;
The carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface by control temperature;
Carry out segregation at the interface of described carbon metal and substrate, lead away liquid carbon metal alloy, generate graphene film.
In conjunction with first aspect, may in implementation in the first of first aspect, described metal and carbon Formed metal alloy step to be comprised:
Described metal loaded container and is evacuated, heating described metal;
When described METAL HEATING PROCESS to the first temperature range, pass into the hydrogen of the first set rate and the carbon-source gas of the second set rate, control pressure in described container to predetermined pressure range;
The lasting duration meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets after predetermined time requires, Formed metal alloy.
In conjunction with the first possibility implementation of first aspect, in the second possibility implementation of first aspect, described first temperature range is 200 degrees Celsius to 1400 degrees Celsius, described first set rate 1-100SCCM, described second set rate is 1-5000SCCM, it is 1 minute to 5 hours that described predetermined time requires, described predetermined pressure range is the holder of 0.1m millitorr to 780.
In conjunction with the first possibility implementation of first aspect, in the third possibility implementation of first aspect, described carbon-source gas is carbon compound, or hydrocarbon polymer.
May implementation in conjunction with the first of first aspect, may in implementation at the 4th kind of first aspect, described container is pipe furnace, and described pipe furnace material comprises any one or multiple combination of following material: graphite, quartz, glass, metal.
In conjunction with first aspect, may in implementation at the 5th kind of first aspect, the carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface step and comprises by described control temperature:
Described carbon metal alloy is placed in the environment comprising air or nitrogen, and the temperature value of described environment is in the second temperature range, and described second temperature range is greater than the fusing point of described carbon metal alloy, is watered by described carbon metal alloy and is applied to described substrate surface;
Segregation is carried out at the described interface in institute's carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film step and comprises:
When described carbon metal alloy water the duration being applied to described substrate surface meet default time interval time, the carbon metal alloy of liquid state is led away, substrate leaves graphene film.
In conjunction with first aspect, in the 6th kind of possibility implementation of first aspect, described metal is the alloy of the alloy of gallium, gallium and indium, gallium and tin, or the alloy of gallium and zinc.
Second aspect, embodiments provide a kind of Graphene generating apparatus based on any substrate, described device comprises:
Carbon metal alloy generation unit, for by metal and carbon Formed metal alloy;
Flow coat unit, for the fusing point of control temperature higher than described carbon metal alloy, waters the carbon metal alloy of described liquid state and is applied to substrate surface;
Segregation unit, for carrying out segregation at the interface of described carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film.
In conjunction with second aspect, in the first possibility implementation of second aspect, described carbon metal alloy generation unit comprises:
Heating subelement, for described metal being loaded container and being evacuated, heats described metal;
Gas passes into subelement, for when described METAL HEATING PROCESS to the first temperature range, passes into the hydrogen of the first set rate and the carbon-source gas of the second set rate, controls pressure in described container to predetermined pressure range;
Alloy generates subelement, after the lasting duration for meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets predetermined time requirement, and Formed metal alloy.
The third aspect, embodiments provide a kind of Graphene based on any substrate and generate equipment, described equipment comprises: pipe furnace, first flow controller, second amount controller, heater block, pressure valve, pressure detecting part, temperature detection part and controller, wherein:
Described heater block is for heating described pipe furnace;
Described pressure valve is for regulating the pressure in pipe furnace;
Described temperature detection part is for detecting the temperature in pipe furnace;
Described pressure detecting part is for detecting the pressure in pipe furnace;
Described first flow controller and second amount controller are for controlling to enter the flow of hydrogen in pipe furnace and carbon-source gas;
Described controller is used for according to pressure detection section components.The detection data of temperature detection part, corresponding control pressure valve and heater block, by metal and carbon Formed metal alloy, and Correctional tube furnace temperature and pressure, the carbon metal alloy of described liquid state is watered and is applied to substrate surface; Make the interface of described carbon metal and substrate carry out segregation, lead away liquid carbon metal alloy, generate graphene film.
In the present invention, by by metal and carbon Formed metal alloy, and the temperature controlling carbon metal alloy is higher than its fusing point, the carbon metal alloy of liquid state is watered and is applied to substrate surface, by carrying out segregation at the interface of carbon metal and substrate, thus generation graphene film, the present invention is by the mode of carbon metal alloy segregation, can conveniently lead away liquid carbon alloy material, make it possible to generate graphene film in any substrate, and do not need etching yet, water, the participation of organic solvent, decrease and generate Graphene to the restriction of substrate, and restriction that other batching during Graphene generation participates in.
Accompanying drawing explanation
Fig. 1 is the realization flow figure of the Graphene generation method based on any substrate that first embodiment of the invention provides;
The graphene film generative process schematic diagram that Fig. 1 a provides for first embodiment of the invention;
Fig. 2 is the realization flow figure of the Graphene generation method based on any substrate that second embodiment of the invention provides;
Fig. 3 is the structural representation of the Graphene generating apparatus based on any substrate that third embodiment of the invention provides;
The structural representation of the generation of the Graphene based on any substrate equipment that Fig. 4 provides for fourth embodiment of the invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Based on the Graphene generation method of any substrate described in the embodiment of the present invention, when being intended to carry out Graphene generation in solution prior art, need to use more batching to participate in, and the problem that the substrate generating Graphene is restricted, when using chemical gaseous phase deposition method to generate Graphene in such as prior art, composition and reactant gases is introduced by inlet manifold, by composition adsorbs on substrate, by introducing etching reagent, the batching of water and other organic solvent, make reactant that the chemical reaction of migration and film forming occur, but need etching reagent, the batching of water and other organic solvent, the shape of substrate is restricted, it can only be such as the substrate of plane, or the curvature of substrate requires very little, when causing Graphene to generate, to the restriction of substrate.Below in conjunction with accompanying drawing, the present invention is specifically described.
Embodiment one:
Fig. 1 shows the realization flow of the Graphene generation method based on any substrate that first embodiment of the invention provides, and details are as follows:
In step S101, by metal and carbon Formed metal alloy.
Concrete, the metal alloy of carbon described in the embodiment of the present invention, refers to the alloy material comprising carbon and metallic element, as one of the present invention preferred embodiment in, described metallic substance can be the alloy of gallium, gallium and indium, the alloy of gallium and tin, or the alloy of gallium and zinc.
In the method for described metal and carbon Formed metal alloy, the material of carbon can be comprised, it can be such as carbon-source gas, or also can comprise the material of carbon and the metal mode Formed metal alloy by heating and pressurizing for other, such as can carry out chemical vapour deposition by chemical Vapor deposition process to molten metal, doping carbon element in liquid metal.Especially by the method for chemical Vapor deposition process Formed metal alloy, will be described further in embodiment two.
In step s 102, the carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface by control temperature.
In embodiments of the present invention, before described carbon metal alloy is carried out flow coat, need the temperature controlling carbon metal alloy place environment to be greater than the fusing point of described carbon metal alloy, thus make carbon metal alloy for liquid.
Concrete, as one of the present invention preferred embodiment in, the carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface step and comprises by described control temperature:
Described carbon metal alloy is placed in the environment comprising air or nitrogen, and the temperature value of described environment is in the second temperature range, and described second temperature range is greater than the fusing point of described carbon metal alloy, is watered by described carbon metal alloy and is applied to described substrate surface.
The described environment comprising air or nitrogen can be under the physical environment that weather is warmmer, and such as temperature can be greater than 30 degree etc.When the alloy that the metal in described carbon metal alloy is gallium and indium, the alloy of gallium and tin, or during the alloy of gallium and zinc, described second temperature range can be preferably 30 degrees Celsius to 35 degrees Celsius, it can be such as 31 degrees Celsius, 32 degrees Celsius, 33 degrees Celsius, 34 degrees Celsius etc.This is because: the fusing point of gallium is 29.8 degrees Celsius.When the molar fraction of indium, tin, zinc is less than 15%, the fusing point of the alloy of gallium and indium, gallium and the alloy of tin and the alloy of gallium and zinc can be lower, therefore, the second temperature range is set to 30 degrees Celsius to 35 degrees Celsius can to meet carbon metal alloy is liquid requirement.
As shown in Figure 1a, in the temperature range that temperature is 30 degrees Celsius to 35 degrees Celsius, pressure can be under standard atmospheric pressure, by carbon metal alloy liquid flow coat on the surface of the substrate, substrate 110 surface is as shown in Figure 1a plane, can certainly be on-plane surface, because the carbon metal alloy 106 of liquid state can according to liquid fluidity, on the on-plane surface of substrate, such as generate contact surface on irregular surfaces, and in described rule or irregular contact surface, resolve generation graphene film 202.
In step s 103, carry out segregation at the interface of described carbon metal and substrate, lead away liquid carbon metal alloy, generate graphene film.
As in the preferred a kind of embodiment of the present invention, segregation is carried out at the described interface in institute's carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film step and comprises:
When described carbon metal alloy water the duration being applied to described substrate surface meet default time interval time, the carbon metal alloy of liquid state is led away, substrate leaves graphene film.
Described default time interval, can be 1 minute to 5 hours, such as can select 10 minutes, 20 minutes, half an hour, 1 hour, 2 hours, 3 hours, 4 hours etc.The selection of described default time interval, can select flexibly according to the resolution speed of the carbon metal alloy of liquid state, such as very fast in carbon metal alloy speed of cooling, such as be reduced to 30 degrees Celsius by 34 degrees Celsius, the graphene film generated is resolved very fast on the surface of substrate and carbon metal alloy liquid, thus can select the short period accordingly, after the short period, described carbon metal alloy liquid be led away.Accordingly, if the resolution speed of graphene film is comparatively slow, when such as temperature declines less, resolve and need the longer time, then select longer steady time accordingly, to resolve generation graphene film.
Described carbon metal alloy liquid is led away, can, according to the gravity of carbon metal alloy own, carbon metal alloy be flowed away, or can also pass through other adsorption tool, such as adopts the mode of pressure adsorption, is led away by described carbon metal alloy liquid.Thus stay in substrate at Graphene.
The present invention passes through by metal and carbon Formed metal alloy, and the temperature controlling carbon metal alloy is higher than its fusing point, the carbon metal alloy of liquid state is watered and is applied to substrate surface, by carrying out segregation at the interface of carbon metal and substrate, thus generation graphene film, the present invention is by the mode of carbon metal alloy segregation, can conveniently lead away liquid carbon alloy material, make it possible to generate graphene film in any substrate, and do not need etching yet, water, the participation of organic solvent, decrease and generate Graphene to the restriction of substrate, and restriction that other batching during Graphene generation participates in.
Embodiment two:
Fig. 2 shows the realization flow of the Graphene generation method based on any substrate that second embodiment of the invention provides, and details are as follows:
In step s 201, described metal loaded container and is evacuated, heating described metal.
Concrete, the metal alloy of carbon described in the embodiment of the present invention, can select the method for chemical vapour deposition to generate.In the present embodiment, step S201-S203 specifically will schematically illustrate introduction to the method.Be understandable that, by the method Formed metal alloy of chemical vapour deposition just wherein a kind of comparatively preferential embodiment, can not the method as the restriction of the application's Formed metal alloy.
Wherein, described container can be pipe furnace 101, and the Graphene based on any substrate as shown in Figure 4 generates equipment 100, and the diameter of pipe furnace is a, and the length of pipe furnace is 5-8 times of diameter.The diameter of such as pipe furnace can be 8 centimetres, and so the length of pipe furnace can be then 40 centimetres to 60 centimetres.Described pipe furnace material comprises any one or multiple combination of following material: graphite, quartz, glass, metal.Be understandable that, when described pipe furnace material is metal, need the metallic substance selecting higher melt, to make the requirement adapting in process of production heat.
Cylindrical cavity is provided with in described pipe furnace, the surface of described cylindrical cavity is provided with heater block 102, substrate 110 and temperature detection part is provided with in described cylindrical cavity, described temperature detection part can be temperature sensor, by will detect Temperature Feedback to controller, control described heater block by controller and carry out heating or reducing temperature, described substrate surface can be regular planar, or also can non-regulation planar, for watering the carbon metal alloy 106 of coating liquid.
Described container is evacuated, its object is to reduce when other impurity or gas generate carbon metal alloy and cause impurity effect.
In step S202, when described METAL HEATING PROCESS to the first temperature range, pass into the hydrogen of the first set rate and the carbon-source gas of the second set rate, control pressure in described container to predetermined pressure range.
Heating of metal to the first temperature range, for the gallium described in the embodiment of the present invention, the alloy of gallium and indium, the alloy of gallium and tin, or the alloy of gallium and zinc, described first temperature range can be 200 degrees Celsius to 1400 degrees Celsius, can be such as 300 degrees Celsius, 500 degrees Celsius, 700 degrees Celsius, 900 degrees Celsius, 1200 degrees Celsius etc.
Described pressure-controlling, can be controlled by described pressure detecting part 107 and pressure valve, when pressure detecting part detection 107 is undesirable to current pressure, is adjusted accordingly by pressure valve 108.
Described predetermined pressure range, can for being the holder of 0.1m millitorr to 780, and wherein, 1 holds in the palm (Torr)=133.322 handkerchief (Pa).Arbitrary pressure range can be selected wherein, such as 1 holder, 10 holders, 50 holders, 100 holders, 500 holders etc.
Passing into of described hydrogen and carbon-source gas, as shown in Figure 4, its uninterrupted passed into can be controlled by first flow controller 103A and second amount controller 103B, such as, in the embodiment of the present invention, first flow controller 103A is for controlling the flow leading to hydrogen 104, and second amount controller 103B controls the flow of carbon-source gas 105.In preferred implementation method, described first set rate 1-100SCCM, described second set rate is 1-5000SCCM.Wherein SCMM represents standard state ml/min.
Described carbon-source gas is carbon compound, or hydrocarbon polymer, can be such as methane, ethene etc.
In step S203, the lasting duration meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets after predetermined time requires, Formed metal alloy.
When described METAL HEATING PROCESS is to predetermined scope and after leading to hydrogen and carbon-source gas simultaneously, when maintaining condition in this temperature range, namely pass into hydrogen and carbon-source gas according to predetermined flow, the lasting time gets final product Formed metal alloy after reaching predetermined time requirement simultaneously.After the present invention obtains carbon metal alloy, need bomb furnace to carry out cooling process, described in add waterfall or cooling method comprises rapid thermal process and flash anneal process etc.
Described predetermined time requirement can be 0.1 minute to 5 hours, according to leading to hydrogen, the uninterrupted of carbon-source gas, the size of temperature and adjusting flexibly.The hydrogen such as passed into, the amount of carbon-source gas is more, temperature is higher, then described predetermined time requires to reduce accordingly.
In step S204, the carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface by control temperature.
In step S205, carry out segregation at the interface of described carbon metal and substrate, lead away liquid carbon metal alloy, generate graphene film.
Step S204 is substantially identical with the embodiment of the present invention one with step S205, does not repeat at this.
The embodiment of the present invention, on the basis of embodiment one, is described the generative process of wherein a kind of carbon metal alloy further, is carried out the control of formation condition by bomb furnace, realizes more easily making the generation of Graphene.
Embodiment three:
Fig. 3 shows the structural representation of the Graphene generating apparatus based on any substrate that third embodiment of the invention provides, and details are as follows:
Based on the Graphene generating apparatus of any substrate described in the embodiment of the present invention, comprising:
Carbon metal alloy generation unit 301, for by metal and carbon Formed metal alloy;
Flow coat unit 302, for the fusing point of control temperature higher than described carbon metal alloy, waters the carbon metal alloy of described liquid state and is applied to substrate surface;
Segregation unit 303, for carrying out segregation at the interface of described carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film.
Preferably, described carbon metal alloy generation unit comprises:
Heating subelement, for described metal being loaded container and being evacuated, heats described metal;
Gas passes into subelement, for when described METAL HEATING PROCESS to the first temperature range, passes into the hydrogen of the first set rate and the carbon-source gas of the second set rate, controls pressure in described container to predetermined pressure range;
Alloy generates subelement, after the lasting duration for meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets predetermined time requirement, and Formed metal alloy.
Preferably, described first temperature range is 200 degrees Celsius to 1400 degrees Celsius, described first set rate 1-100SCCM, and described second set rate is 1-5000SCCM, it is 1 minute to 5 hours that described predetermined time requires, described predetermined pressure range is the holder of 0.1m millitorr to 780.
Preferably, described carbon-source gas is carbon compound, or hydrocarbon polymer.
Preferably, described container is pipe furnace, and described pipe furnace material comprises any one or multiple combination of following material: graphite, quartz, glass, metal.
Preferably, described metal is the alloy of the alloy of gallium, gallium and indium, gallium and tin, or the alloy of gallium and zinc.
Based on the Graphene generating apparatus of any substrate described in the embodiment of the present invention, corresponding with the Graphene generation method based on any substrate described in embodiment one and two, do not repeat at this.
Embodiment four:
The Graphene based on any substrate that Fig. 4 shows fourth embodiment of the invention to be provided generates equipment, and details are as follows:
Generate equipment based on the Graphene of any substrate described in the embodiment of the present invention, comprising:
Pipe furnace 101, first flow controller 103A, second amount controller 103B, heater block 102, pressure valve 108, pressure detecting part 107, temperature detection part and controller, wherein:
Described heater block 102 is for heating described pipe furnace;
Described pressure valve 108 is for regulating the pressure in pipe furnace;
Described temperature detection part is for detecting the temperature in pipe furnace;
Described pressure detecting part 107 is for detecting the pressure in pipe furnace;
Described first flow controller 103A and second amount controller 103B is for controlling to enter the flow of hydrogen 104 in pipe furnace and carbon-source gas 105;
Described controller is used for according to pressure detection section components.The detection data of temperature detection part, corresponding control pressure valve and heater block, by metal and carbon Formed metal alloy, and Correctional tube furnace temperature and pressure, the carbon metal alloy of described liquid state is watered and is applied to substrate surface; Make the interface of described carbon metal and substrate carry out segregation, lead away liquid carbon metal alloy, generate graphene film.
By generating the generation method of equipment based on the Graphene of any substrate in the existing introduction of embodiment two in the embodiment of the present invention, do not repeat at this.
In several embodiment provided by the present invention, should be understood that, disclosed apparatus and method, can realize by another way.Such as, device embodiment described above is only schematic, such as, the division of described unit, be only a kind of logic function to divide, actual can have other dividing mode when realizing, such as multiple unit or assembly can in conjunction with or another system can be integrated into, or some features can be ignored, or do not perform.Another point, shown or discussed coupling each other or direct-coupling or communication connection can be by some interfaces, and the indirect coupling of device or unit or communication connection can be electrical, machinery or other form.
The described unit illustrated as separating component or can may not be and physically separates, and the parts as unit display can be or may not be physical location, namely can be positioned at a place, or also can be distributed on multiple NE.Some or all of unit wherein can be selected according to the actual needs to realize the object of the present embodiment scheme.
In addition, each functional unit in each embodiment of the present invention can be integrated in a processing unit, also can be that the independent physics of unit exists, also can two or more unit in a unit integrated.Above-mentioned integrated unit both can adopt the form of hardware to realize, and the form of SFU software functional unit also can be adopted to realize.
If described integrated unit using the form of SFU software functional unit realize and as independently production marketing or use time, can be stored in a computer read/write memory medium.Based on such understanding, the part that technical scheme of the present invention contributes to prior art in essence in other words or all or part of of this technical scheme can embody with the form of software product, this computer software product is stored in a storage media, comprising some instructions in order to make a computer equipment (can be Personal Computer, server, or the network equipment etc.) perform all or part of of method described in each embodiment of the present invention.And aforesaid storage media comprises: USB flash disk, portable hard drive, read-only storage (ROM, Read-OnlyMemory), random access memory (RAM, RandomAccessMemory), magnetic disc or CD etc. various can be program code stored medium.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. one kind based on the Graphene generation method of any substrate, and it is characterized in that, described method comprises:
By metal and carbon Formed metal alloy;
The carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface by control temperature;
Carry out segregation at the interface of described carbon metal and substrate, lead away liquid carbon metal alloy, generate graphene film.
2. method according to claim 1, is characterized in that, describedly metal and carbon Formed metal alloy step is comprised:
Described metal loaded container and is evacuated, heating described metal;
When described METAL HEATING PROCESS to the first temperature range, pass into the hydrogen of the first set rate and the carbon-source gas of the second set rate, control pressure in described container to predetermined pressure range;
The lasting duration meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets after predetermined time requires, Formed metal alloy.
3. method according to claim 2, it is characterized in that, described first temperature range is 200 degrees Celsius to 1400 degrees Celsius, described first set rate 1-100SCCM, described second set rate is 1-5000SCCM, it is 1 minute to 5 hours that described predetermined time requires, described predetermined pressure range is the holder of 0.1m millitorr to 780.
4. method according to claim 2, it is characterized in that, described carbon-source gas is carbon compound, or hydrocarbon polymer.
5. method according to claim 2, it is characterized in that, described container is pipe furnace, and described pipe furnace material comprises any one or multiple combination of following material: graphite, quartz, glass, metal.
6. method according to claim 1, is characterized in that, the carbon metal alloy of described liquid state, higher than the fusing point of described carbon metal alloy, waters and is applied to substrate surface step and comprises by described control temperature:
Described carbon metal alloy is placed in the environment comprising air or nitrogen, and the temperature value of described environment is in the second temperature range, and described second temperature range is greater than the fusing point of described carbon metal alloy, is watered by described carbon metal alloy and is applied to described substrate surface;
Segregation is carried out at the described interface in institute's carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film step and comprises:
When described carbon metal alloy water the duration being applied to described substrate surface meet default time interval time, the carbon metal alloy of liquid state is led away, substrate leaves graphene film.
7. method according to claim 1, it is characterized in that, described metal is the alloy of the alloy of gallium, gallium and indium, gallium and tin, or the alloy of gallium and zinc.
8. based on a Graphene generating apparatus for any substrate, it is characterized in that, described device comprises:
Carbon metal alloy generation unit, for by metal and carbon Formed metal alloy;
Flow coat unit, for the fusing point of control temperature higher than described carbon metal alloy, waters the carbon metal alloy of described liquid state and is applied to substrate surface;
Segregation unit, for carrying out segregation at the interface of described carbon metal and substrate, leads away liquid carbon metal alloy, generates graphene film.
9. device according to claim 8, it is characterized in that, described carbon metal alloy generation unit comprises:
Heating subelement, for described metal being loaded container and being evacuated, heats described metal;
Gas passes into subelement, for when described METAL HEATING PROCESS to the first temperature range, passes into the hydrogen of the first set rate and the carbon-source gas of the second set rate, controls pressure in described container to predetermined pressure range;
Alloy generates subelement, after the lasting duration for meeting the first temperature range when the temperature of described METAL HEATING PROCESS meets predetermined time requirement, and Formed metal alloy.
10. the Graphene based on any substrate generates an equipment, and it is characterized in that, described equipment comprises: pipe furnace, first flow controller, second amount controller, heater block, pressure valve, pressure detecting part, temperature detection part and controller, wherein:
Described heater block is for heating described pipe furnace;
Described pressure valve is for regulating the pressure in pipe furnace;
Described temperature detection part is for detecting the temperature in pipe furnace;
Described pressure detecting part is for detecting the pressure in pipe furnace;
Described first flow controller and second amount controller are for controlling to enter the flow of hydrogen in pipe furnace and carbon-source gas;
Described controller is used for according to pressure detection section components.The detection data of temperature detection part, corresponding control pressure valve and heater block, by metal and carbon Formed metal alloy, and Correctional tube furnace temperature and pressure, the carbon metal alloy of described liquid state is watered and is applied to substrate surface; Make the interface of described carbon metal and substrate carry out segregation, lead away liquid carbon metal alloy, generate graphene film.
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CN107364846A (en) * 2017-09-06 2017-11-21 蚌埠玻璃工业设计研究院 A kind of device in substrate surface growth graphene film
CN107381553A (en) * 2017-09-06 2017-11-24 蚌埠玻璃工业设计研究院 A kind of method in substrate surface growth graphene film
CN111825082A (en) * 2020-07-17 2020-10-27 绍兴小竹新能源有限公司 Preparation method of graphene
CN112551509A (en) * 2019-09-25 2021-03-26 中国科学院金属研究所 Method for preparing nano porous carbon or nano spherical carbon

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583359A (en) * 2012-04-01 2012-07-18 中国科学院上海微***与信息技术研究所 Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition
CN102627275A (en) * 2012-04-28 2012-08-08 郑州大学 Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process
CN103663434A (en) * 2012-09-12 2014-03-26 铼钻科技股份有限公司 Method and device for mass production of graphene

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102583359A (en) * 2012-04-01 2012-07-18 中国科学院上海微***与信息技术研究所 Method for preparing graphene by adopting liquid catalyst aided chemical vapor deposition
CN102627275A (en) * 2012-04-28 2012-08-08 郑州大学 Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process
CN103663434A (en) * 2012-09-12 2014-03-26 铼钻科技股份有限公司 Method and device for mass production of graphene

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LIFANG TAN ET AL.: "Design of catalytic substrates for uniform graphene films:from solid-metal to liquid-metal", 《NANOSCALE》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107364846A (en) * 2017-09-06 2017-11-21 蚌埠玻璃工业设计研究院 A kind of device in substrate surface growth graphene film
CN107381553A (en) * 2017-09-06 2017-11-24 蚌埠玻璃工业设计研究院 A kind of method in substrate surface growth graphene film
CN112551509A (en) * 2019-09-25 2021-03-26 中国科学院金属研究所 Method for preparing nano porous carbon or nano spherical carbon
CN111825082A (en) * 2020-07-17 2020-10-27 绍兴小竹新能源有限公司 Preparation method of graphene

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