CN116281981B - Graphene preparation device and method - Google Patents
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- CN116281981B CN116281981B CN202310371420.XA CN202310371420A CN116281981B CN 116281981 B CN116281981 B CN 116281981B CN 202310371420 A CN202310371420 A CN 202310371420A CN 116281981 B CN116281981 B CN 116281981B
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 26
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- 239000002184 metal Substances 0.000 claims abstract description 87
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- 239000002904 solvent Substances 0.000 description 4
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- 229910052733 gallium Inorganic materials 0.000 description 1
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- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/186—Preparation by chemical vapour deposition [CVD]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The application discloses a graphene preparation device and a graphene preparation method, which belong to the technical field of nano material growth, and the method comprises the following steps: the device comprises a reaction container, a liquid level height measurement and control device, a feeding device, an air inlet device and a receiving device. According to the application, the carbon source gas is formed into bubbles by the air inlet device and is introduced into the molten metal catalyst, the liquid level of the molten metal catalyst is measured by the liquid level measurement and control device, and the feeding quantity of the feeding device is controlled according to the measurement result, so that the liquid level is always kept at the target liquid level, the path of the carbon source gas flowing through the molten metal catalyst can be regulated and controlled, the effective control of the growth of graphene is realized, and further, the graphene with different layers and thicknesses can be obtained according to the requirement; meanwhile, the operation is simple and feasible, and the method can be used for mass production.
Description
Technical Field
The application relates to the technical field of nano material growth, in particular to a graphene preparation device and method.
Background
Since 2004, graphene was found, attracting the favor of many researchers worldwide. Graphene has wide application prospects in the aspects of new energy batteries, composite materials, lithium batteries, flexible display screens, sensors and the like due to the unique structure and excellent heat conduction, electric conduction and other performances.
Researchers have developed a variety of methods for preparing graphene, and the production methods which are relatively mature in technology and can be mass-produced at present mainly include a redox method, a mechanical stripping method and a chemical vapor deposition method. Compared with other graphene preparation methods, the chemical vapor deposition method has the advantages of high yield, large growth area, controllable layer number and the like, and the performance of the method is closer to the intrinsic physical properties of graphene. However, the traditional chemical vapor deposition method has low yield and high cost, and simultaneously has the transfer problem. In 2009, a technology for preparing graphene by using a molten solvent is proposed, and in the process of preparing graphene by using a molten solvent, as a graphene sample is continuously generated, the molten solvent is entrained out, and the amount of the molten solvent in the interior is continuously reduced, so that the quality of the graphene is affected. However, there is currently a lack of means to effectively control graphene growth. Therefore, how to effectively control the growth of graphene is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
The application aims to provide a graphene preparation device and a graphene preparation method, so that graphene growth is effectively controlled.
To achieve the above object, the present application provides a graphene preparation apparatus, comprising: the device comprises a reaction container, a liquid level height measurement and control device, a feeding device, an air inlet device and a receiving device;
The reaction vessel is used for storing a molten metal catalyst;
The liquid level measuring and controlling device is used for measuring the liquid level of the molten metal catalyst in the reaction container; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
The liquid level height measurement and control device is connected with the feeding device and is used for controlling the feeding device to add the molten metal catalyst into the reaction container according to the to-be-supplemented amount so that the liquid level height reaches the target liquid level height;
the gas inlet device is used for introducing carbon source gas into the reaction container, so that the carbon source gas passes through the molten metal catalyst with the target liquid level height to generate graphene with a target layer number;
And the receiving device is used for collecting the graphene with the target layer number generated in the reaction container.
Optionally, a pressure sensing device is arranged at the bottom of the feeding device; the liquid level height measurement and control device is connected with the feeding device and is used for controlling the pressure sensing device to add the molten metal catalyst into the reaction container according to the to-be-supplemented amount so that the liquid level height reaches the target liquid level height.
Optionally, the controllable liquid level of the liquid level measuring and controlling device is 1mm-2m, and the controllable liquid level comprises values at two ends.
Optionally, the graphene preparation device further includes: a gas recovery device;
the gas recovery device is used for collecting hydrogen generated after the carbon source gas passes through the molten metal catalyst with the target liquid level.
Optionally, the air inlet device is of a porous and breathable structure.
Optionally, the reaction vessel is an electromagnetic induction heating vessel.
Optionally, the liquid level height measurement and control device includes: a laser transmitter, a laser receiver and a control device;
The laser emitter is used for emitting laser to the liquid level of the molten metal catalyst in the reaction container;
The laser receiver is used for receiving the laser reflected by the liquid level of the molten metal catalyst;
The control device is used for determining the liquid level height of the molten metal catalyst according to the light path formed by the laser; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level height and the target liquid level height;
Correspondingly, the liquid level height measurement and control device is connected with the feeding device and comprises:
the control device is connected with the feeding device.
Optionally, the laser transmitter and the laser receiver are located opposite; the bottom of the laser emitter is provided with a first panel; the bottom of the laser receiver is provided with a second panel; the first panel and the second panel may be rotatable;
The first panel is used for adjusting the light path of the laser emitted by the laser emitter to the liquid level of the molten metal catalyst in the reaction container by rotating the first panel;
The second panel is used for enabling the laser receiver to receive the laser reflected by the liquid level of the molten metal catalyst by rotating the second panel.
Optionally, the rotation angle of the first panel is 0 ° -180 °, and includes values of both ends; the second panel has a rotation angle of 0 ° -180 °, and includes values of both ends.
In order to achieve the above object, the present application further provides a graphene preparation method, which is applied to the graphene preparation device, and includes:
Measuring the level of molten metal catalyst in the reaction vessel;
Determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
Adding a molten metal catalyst into the reaction vessel according to the to-be-replenished amount, so that the liquid level reaches the target liquid level;
and introducing carbon source gas into the reaction container, and enabling the carbon source gas to pass through the molten metal catalyst with the target liquid level height to generate graphene with the target layer number.
The application provides a graphene preparation device, which comprises: the device comprises a reaction container, a liquid level height measurement and control device, a feeding device, an air inlet device and a receiving device; the reaction vessel is used for storing a molten metal catalyst; the liquid level measuring and controlling device is used for measuring the liquid level of the molten metal catalyst in the reaction container; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level; the liquid level height measurement and control device is connected with the feeding device and is used for controlling the feeding device to add the molten metal catalyst into the reaction container according to the to-be-supplemented amount so that the liquid level height reaches the target liquid level height; the gas inlet device is used for introducing carbon source gas into the reaction container, so that the carbon source gas passes through the molten metal catalyst with the target liquid level height to generate graphene with a target layer number; and the receiving device is used for collecting the graphene with the target layer number generated in the reaction container.
Obviously, the application leads the carbon source gas into the molten metal catalyst through the bubble formed by the air inlet device, measures the liquid level of the molten metal catalyst through the liquid level height measuring and controlling device, and controls the feeding quantity of the feeding device according to the measuring result so as to keep the liquid level at the target liquid level all the time, thereby regulating and controlling the path of the carbon source gas flowing through the molten metal catalyst, realizing the effective control of the growth of the graphene, and further obtaining the grapheme with different layers and thicknesses according to the requirement; meanwhile, the operation is simple and feasible, and the method can be used for mass production. The application also provides a preparation method of the graphene, which has the beneficial effects.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present application, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
Fig. 1 is a structural diagram of a graphene preparation apparatus according to an embodiment of the present application;
Fig. 2 is a flowchart of a graphene preparation method provided in an embodiment of the present application.
In fig. 1, the reference numerals are as follows:
1-a reaction vessel; 2-level of molten metal catalyst; 3-an air intake device; 41-a laser emitter; 42-a first panel; 43-laser receiver; 44-a second panel; 45-control means; 5-a feeding device; and 6, a material receiving device.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Referring to fig. 1, fig. 1 is a block diagram of a graphene preparation apparatus according to an embodiment of the present disclosure, where the apparatus may include: the device comprises a reaction vessel 1, a liquid level height measurement and control device, a feeding device 5, an air inlet device 3 and a receiving device 6;
a reaction vessel 1 for storing a molten metal catalyst;
the liquid level height measurement and control device is used for measuring the liquid level 2 height of the molten metal catalyst in the reaction vessel 1; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
the liquid level measurement and control device is connected with the feeding device 5 and is used for controlling the feeding device 5 to add the molten metal catalyst into the reaction vessel 1 according to the amount to be supplemented so that the liquid level reaches the target liquid level;
The gas inlet device 3 is used for introducing carbon source gas into the reaction container 1, so that the carbon source gas passes through the molten metal catalyst with the target liquid level to generate graphene with the target layer number;
and the material receiving device 6 is used for collecting the graphene with the target layer number generated in the reaction container 1.
The embodiment is not limited to a specific structure of the liquid level height measurement and control device, as long as the liquid level height measurement and control device can have a liquid level height measurement and control function, for example, the liquid level height measurement and control device can include: a laser transmitter 41, a laser receiver 43 and a control device 45; a laser emitter 41 for emitting laser light to the liquid surface 2 of the molten metal catalyst in the reaction vessel 1; a laser receiver 43 for receiving laser light reflected by the liquid surface 2 of the molten metal catalyst; a control device 45 for determining the level 2 of the molten metal catalyst based on the optical path formed by the laser; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level; correspondingly, the liquid level height measurement and control device is connected with the feeding device 5 and comprises: the control device 45 is connected to the feeding device 5. The embodiment does not limit the specific controllable liquid level of the liquid level measuring and controlling device, and determines the specific controllable liquid level of the liquid level measuring and controlling device according to practical situations, for example, the controllable liquid level of the liquid level measuring and controlling device can be 1mm-2m and comprises values at two ends.
The specific structures of the laser transmitter 41 and the laser receiver 43 are not limited in this embodiment, as long as the laser receiver 43 is ensured to be able to receive the laser light emitted by the laser transmitter 41, for example, the laser transmitter 41 and the laser receiver 43 may be located opposite to each other; the bottom of the laser transmitter 41 is provided with a first panel 42; the bottom of the laser receiver 43 is provided with a second panel 44; the first panel 42 and the second panel 44 may rotate; a first panel 42 for adjusting an optical path of the laser light emitted from the laser emitter 41 to the liquid level 2 of the molten metal catalyst in the reaction vessel 1 by rotating the first panel 42; and a second panel 44 for causing the laser receiver 43 to receive the laser light reflected by the liquid surface 2 of the molten metal catalyst by rotating the second panel 44. It should be noted that the first panel 42 and the second panel 44 may receive the laser beam. When the signal from the laser receiver 43 is received by the laser receiver 43 by rotating the panel by a suitable angle, the control device 45 can automatically calculate the level of the liquid. The present embodiment is not limited to a specific rotation angle of the first panel 42 and the second panel 44, as long as the first panel 42 and the second panel 44 are guaranteed to be rotatable, for example, the rotation angle of the first panel 42 is 0 ° -180 °, and includes values of both ends; the second panel 44 rotates through an angle of 0 deg. -180 deg., and includes values at both ends.
The present embodiment is not limited to the specific structure of the feeding device 5 as long as it is ensured that the molten metal catalyst can be added to the reaction vessel 1 according to the amount to be replenished, and for example, a pressure sensing device may be provided at the bottom of the feeding device 5; the liquid level measuring and controlling device is connected with the feeding device 5 and is used for controlling the pressure sensing device to add the molten metal catalyst into the reaction vessel 1 according to the amount to be supplemented, so that the liquid level reaches the target liquid level. The control device 45 is connected to the feeding device 5, and a pressure sensing device is disposed at the bottom of the feeding device 5, so as to automatically control the feeding amount according to the requirement.
The carbon source gas is bubbled through the gas inlet device 3, and is introduced into the molten metal catalyst as bubbles are formed. The carbon source stream is cracked through the molten metal catalyst to form graphene. The present embodiment is not limited to the specific structure of the gas inlet means 3 as long as the carbon source gas can be surely introduced into the reaction vessel 1, and for example, the gas inlet means 3 may be of a porous gas permeable structure. The specific composition of the carbon source gas is not limited to this embodiment, and may be determined according to practical situations, for example, the carbon source gas may include a carbon source and a carrier gas. The present embodiment is not limited to a specific kind and amount of the carbon source, and for example, the carbon source may be one or more of methane, ethane, ethylene, acetylene, carbon monoxide, carbon dioxide, ethanol, propylene, propane, butane, butadiene, pentane, pentene, benzene, or toluene; at least one of ammonia gas and borane can be selectively doped. The present embodiment is not limited to a specific kind of carrier gas, and for example, the carrier gas may be hydrogen, nitrogen, argon or helium.
Further, since the graphene is generated by cracking a carbon source in the reaction process and hydrogen is generated at the same time, in order to recover and recycle the reacted gas, the embodiment may further include: a gas recovery device; and a gas recovery device for collecting hydrogen gas generated after the carbon source gas passes through the molten metal catalyst having the target liquid level.
The present embodiment is not limited to the specific kind of the reaction vessel 1 as long as the reaction vessel 1 is ensured to be resistant to high temperature, and for example, the reaction vessel 1 may be an electromagnetic induction heating vessel. The embodiment is not limited to the specific reaction pressure in the reaction vessel 1, and the specific reaction pressure in the reaction vessel 1 may be determined according to the actual situation, for example, the reaction pressure in the reaction vessel 1 is-0.5 MPa to 0.5MPa, and includes values of both ends. The present embodiment is not limited to a specific kind of the molten metal catalyst, and for example, the molten metal catalyst may be a mixture of one or more metals of iron, cobalt, nickel, copper, chromium, gold, silver, platinum, zinc, aluminum, chromium, manganese, titanium, tin, magnesium, gallium, indium, or palladium.
Based on the embodiment, the carbon source gas is formed into bubbles by the air inlet device and is introduced into the molten metal catalyst, the liquid level of the molten metal catalyst is measured by the liquid level height measurement and control device, and the feeding amount of the feeding device is controlled according to the measurement result, so that the liquid level is always kept at the target liquid level, the path of the carbon source gas flowing through the molten metal catalyst can be regulated and controlled, the growth of graphene is effectively controlled, and graphenes with different layers and thicknesses can be obtained according to requirements; meanwhile, the operation is simple and feasible, and the method can be used for mass production.
Referring to fig. 2, fig. 2 is a flowchart of a graphene preparation method according to an embodiment of the present application. The application also provides a graphene preparation method, which is applied to the graphene preparation device, and the method can comprise the following steps:
S101: measuring the level of molten metal catalyst in the reaction vessel;
S102: determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
s103: adding a molten metal catalyst into the reaction vessel according to the amount to be replenished, so that the liquid level reaches the target liquid level;
S104: and introducing carbon source gas into the reaction container, and enabling the carbon source gas to pass through the molten metal catalyst with the target liquid level height to generate graphene with the target layer number.
Based on the embodiment, the carbon source gas is formed into bubbles by the air inlet device and is introduced into the molten metal catalyst, the liquid level of the molten metal catalyst is measured by the liquid level height measurement and control device, and the feeding amount of the feeding device is controlled according to the measurement result, so that the liquid level is always kept at the target liquid level, the path of the carbon source gas flowing through the molten metal catalyst can be regulated and controlled, the growth of graphene is effectively controlled, and graphenes with different layers and thicknesses can be obtained according to requirements; meanwhile, the operation is simple and feasible, and the method can be used for mass production.
Referring to fig. 1, fig. 1 is a block diagram of a graphene preparation apparatus according to an embodiment of the present application, including a reaction vessel 1, a liquid level 2 of a molten metal catalyst, an air inlet device 3, a laser emitter 41, a first panel 42, a laser receiver 43, a second panel 44, a control device 45, a feeding device 5, and a receiving device 6. The laser transmitter 41 and the laser receiver 43 are opposite in position, the first panel 42 is connected to the laser transmitter 41 bottom, the second panel 44 is connected to the laser receiver 43 bottom, and the adjustment of the laser light path is performed by rotating the first panel 42 and the second panel 44. After the signal from the laser receiver 43 is received by the laser receiver 43 through the first and second panels 42, 44 rotated by a suitable angle, the control device 45 can automatically calculate the level 2 of the molten metal catalyst. The control device 45 is connected with the feeding device 5, and a pressure sensing device is arranged at the bottom of the feeding device 5, so that the feeding amount can be automatically controlled according to the requirement. The graphene produced by the reaction is collected by the collecting device 6.
The comparative example is a process of preparing graphene by a conventional graphene preparation apparatus, and specifically includes:
Step 1, placing 30L of metal catalyst (corresponding to the liquid level of 15 cm) in a reaction container, heating and melting, wherein the volume of the reaction container is 100L;
step 2, continuously introducing a carbon source and a carrier gas into a molten metal catalyst in a reaction container, wherein the flow ratio of the natural gas to the carrier gas is 1:100;
And 3, collecting the graphene sample 1 through a collecting device, and collecting the graphene sample 2 after reacting for 12 hours.
The results show that the number of graphene samples is 1-3, and after 12 hours of reaction, the liquid level of the molten metal catalyst is reduced, and the number of graphene layers is thickened to 4-7.
Embodiment 1 is a process for preparing graphene by the graphene preparation device of the present application, specifically including:
step 1, placing 20L of metal catalyst (corresponding to the liquid level of 10 cm) in a reaction vessel 1, heating and melting, wherein the volume of the reaction vessel 1 is 100L;
step 2, setting the feeding height of the laser liquid level height measurement and control device to be 15cm, namely, setting the feeding height of the feeding device 5 to be 5cm except the initial liquid level height;
Continuously introducing a carbon source and a carrier gas into the molten metal catalyst in the reaction container 1, wherein the flow ratio of the natural gas to the carrier gas is 1:100;
and 4, collecting the graphene sample 1 through a collecting device, and collecting the graphene sample 2 after reacting for 12 hours.
The result shows that the number of the graphene sample 1 is 1-3, after 12 hours of reaction, the liquid level 2 of the molten metal catalyst is regulated by the laser liquid level height measurement and control device and is always maintained at a stable height, and the number of the graphene layers is still 1-3.
Embodiment 2 is a process for preparing graphene by the graphene preparation device of the present application, specifically including:
Step 1, placing 10L of metal catalyst (corresponding to the liquid level of 5 cm) in a reaction vessel 1, heating and melting, wherein the volume of the reaction vessel 1 is 100L;
step 2, setting the feeding height of the laser liquid level height measurement and control device to be 10cm, namely, setting the feeding height of the feeding device 5 to be 5cm except the initial liquid level height;
Continuously introducing a carbon source and a carrier gas into the molten metal catalyst in the reaction container 1, wherein the flow ratio of the natural gas to the carrier gas is 1:100;
And 4, collecting a graphene sample 1 through a collecting device, and collecting a graphene sample 2 after reacting for 12 hours.
The result shows that the number of the graphene sample 1 is 4-7, after 12 hours of reaction, the liquid level 2 of the molten metal catalyst is regulated by the laser liquid level height measurement and control device and is always maintained at a stable height, and the number of the graphene layers is still 4-7.
The parameters of the three embodiments and the number of layers of the graphene sample are shown in table 1, and compared with the three embodiments, the laser liquid level height measurement and control device can ensure that the liquid level of the molten metal catalyst is kept at a fixed height, so that the number of layers of the prepared graphene can be kept within the required range of layers.
Table 1 parameters and number of graphene sample layers for three examples
The principles and embodiments of the present application are described herein with reference to specific examples, where each example is a progressive relationship, and each example is mainly described by differences from other examples, and identical and similar parts of each example are mutually referred to. For the methods disclosed in the examples, reference may be made to the corresponding device section description. The above description of the embodiments is only for aiding in the understanding of the method of the present application and its core ideas. It will be apparent to those skilled in the art that various changes and modifications can be made to the present application without departing from the principles of the application, and such changes and modifications fall within the scope of the appended claims.
It should also be noted that in this specification, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises an element.
Claims (10)
1. The utility model provides a graphite alkene preparation facilities which characterized in that includes: the device comprises a reaction container, a liquid level height measurement and control device, a feeding device, an air inlet device and a receiving device;
The reaction vessel is used for storing a molten metal catalyst;
The liquid level measuring and controlling device is used for measuring the liquid level of the molten metal catalyst in the reaction container; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
The liquid level height measurement and control device is connected with the feeding device and is used for controlling the feeding device to add the molten metal catalyst into the reaction container according to the to-be-supplemented amount so that the liquid level height reaches the target liquid level height;
the gas inlet device is used for introducing carbon source gas into the reaction container, so that the carbon source gas passes through the molten metal catalyst with the target liquid level height to generate graphene with a target layer number;
And the receiving device is used for collecting the graphene with the target layer number generated in the reaction container.
2. The graphene preparation device according to claim 1, wherein a pressure sensing device is arranged at the bottom of the feeding device; the liquid level height measurement and control device is connected with the feeding device and is used for controlling the pressure sensing device to add the molten metal catalyst into the reaction container according to the to-be-supplemented amount so that the liquid level height reaches the target liquid level height.
3. The graphene preparation device according to claim 1, wherein the controllable liquid level of the liquid level measurement and control device is 1mm-2m and includes values at both ends.
4. The graphene preparation device according to claim 1, further comprising: a gas recovery device;
the gas recovery device is used for collecting hydrogen generated after the carbon source gas passes through the molten metal catalyst with the target liquid level.
5. The graphene preparation device according to claim 1, wherein the air inlet means is a porous and breathable structure.
6. The graphene preparation apparatus according to claim 1, wherein the reaction vessel is an electromagnetic induction heating vessel.
7. The graphene preparation device according to any one of claims 1 to 6, wherein the liquid level height measurement and control device comprises: a laser transmitter, a laser receiver and a control device;
The laser emitter is used for emitting laser to the liquid level of the molten metal catalyst in the reaction container;
The laser receiver is used for receiving the laser reflected by the liquid level of the molten metal catalyst;
The control device is used for determining the liquid level height of the molten metal catalyst according to the light path formed by the laser; determining the amount of the molten metal catalyst to be replenished according to the measured liquid level height and the target liquid level height;
Correspondingly, the liquid level height measurement and control device is connected with the feeding device and comprises:
the control device is connected with the feeding device.
8. The graphene preparation device of claim 7, wherein the laser emitter and the laser receiver are positioned opposite; the bottom of the laser emitter is provided with a first panel; the bottom of the laser receiver is provided with a second panel; the first panel and the second panel may be rotatable;
The first panel is used for adjusting the light path of the laser emitted by the laser emitter to the liquid level of the molten metal catalyst in the reaction container by rotating the first panel;
The second panel is used for enabling the laser receiver to receive the laser reflected by the liquid level of the molten metal catalyst by rotating the second panel.
9. The graphene preparation device according to claim 8, wherein the rotation angle of the first panel is 0 ° -180 °, and includes values of both ends; the second panel has a rotation angle of 0 ° -180 °, and includes values of both ends.
10. A graphene preparation method applied to the graphene preparation apparatus according to any one of claims 1 to 9, comprising:
Measuring the level of molten metal catalyst in the reaction vessel;
Determining the amount of the molten metal catalyst to be replenished according to the measured liquid level and the target liquid level;
Adding a molten metal catalyst into the reaction vessel according to the to-be-replenished amount, so that the liquid level reaches the target liquid level;
and introducing carbon source gas into the reaction container, and enabling the carbon source gas to pass through the molten metal catalyst with the target liquid level height to generate graphene with the target layer number.
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