CN112938947B - Preparation method of graphene with controllable layer number - Google Patents
Preparation method of graphene with controllable layer number Download PDFInfo
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- CN112938947B CN112938947B CN202110339764.3A CN202110339764A CN112938947B CN 112938947 B CN112938947 B CN 112938947B CN 202110339764 A CN202110339764 A CN 202110339764A CN 112938947 B CN112938947 B CN 112938947B
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/186—Preparation by chemical vapour deposition [CVD]
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The application relates to a preparation method of graphene with controllable layer number, which comprises the following steps: obtaining molten metal; regulating and controlling the temperature field of the molten metal; introducing a carbon-containing gas in the form of bubbles into the bottom of the molten metal; the advancing path of the bubbles in the molten metal is regulated, so that the number of layers of the precipitated graphene can be regulated, a means for effectively controlling the number of layers of the graphene can be provided for the prior art, and the method has an important application prospect.
Description
Technical Field
The application relates to the technical field of graphene preparation, in particular to a preparation method of graphene with controllable layer number.
Background
Graphene materials, which are representative of a family of two-dimensional materials, have unique zero-bandgap semimetal characteristics, high electron mobility, and excellent light transmission properties, as well as extremely high mechanical strength and thermal conductivity, so that they have been extensively studied by academia and industry for fifteen years since their successful preparation. Based on the excellent characteristics of the graphene material, the graphene material has or will be exposed to the corners in a conductive agent, a high-conductivity and high-thermal-conductivity composite material.
At present, few-layer graphene (1-10 layers) can be prepared in a large scale by a redox method, a chemical intercalation method, an electrochemical method, a mechanical exfoliation method or a chemical vapor deposition method, however, the graphene materials obtained by the schemes have the defects. For example, the use of the redox method has problems of many defects in products, high cost and high pollution; the chemical intercalation method, the electrochemical method and the mechanical exfoliation method have a problem of low yield.
By utilizing a chemical vapor deposition process, the high-quality single-layer graphene material can be prepared on the surfaces of different metal or alloy substrates by catalytically cracking carbon-containing gas, and the obtained graphene material has large transverse size, high crystallization quality and important application prospect. However, chemical vapor deposition processes face two problems: one is low yield and the other is lack of means to effectively control the number of layers.
Disclosure of Invention
The embodiment of the application provides a preparation method of graphene with controllable layer number, and the layer number of generated graphene can be controlled through regulating and controlling a temperature field of molten metal and a traveling path of bubbles in the molten metal.
The embodiment of the application provides a preparation method of graphene with controllable layer number, which comprises the following steps:
obtaining molten metal;
regulating and controlling the temperature field of the molten metal;
introducing a carbon-containing gas in the form of bubbles into the bottom of the molten metal;
and regulating and controlling the traveling path of the bubbles in the molten metal to regulate and control the number of layers of the precipitated graphene.
Optionally, obtaining molten metal comprises:
placing a catalytic metal material into a crucible;
and heating the crucible in an inert gas atmosphere until the metal material is in a molten state to obtain molten metal.
Optionally, the adjusting the temperature field of the molten metal includes:
creating a temperature gradient of the molten metal by a first heating element disposed at a bottom of the crucible and a second heating element disposed at a top of the crucible such that a bottom temperature of the molten metal is higher than a top temperature of the molten metal; the heating power of the first heating element is greater than the heating power of the second heating element.
Optionally, the temperature difference between the bottom temperature of the molten metal and the top temperature of the molten metal is in a range of 0 to 100 ℃.
Optionally, after the temperature field of the molten metal is adjusted and before the carbon-containing gas is introduced into the bottom of the molten metal in the form of bubbles, the method further includes:
a gas-liquid two-phase flow guiding device is arranged in the crucible;
regulating a travel path of a gas bubble in molten metal, comprising:
and introducing the bubbles from the bottom of the gas-liquid two-phase flow guiding device so as to guide the traveling path of the bubbles through the gas-liquid two-phase flow guiding device.
Optionally, the adjusting the travel path of the bubble in the molten metal includes:
the use of a stir bar disturbs the path of the gas bubbles rising straight through the molten metal.
Optionally, the method further comprises:
graphene overflowing from the molten metal with the inert gas stream is collected by a collection device.
Optionally, the metal material is one or more of nickel, cobalt, iron, platinum, copper, aluminum, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc, silver, indium and palladium.
Optionally, the carbon-containing gas is one or more of methane, ethylene, acetylene, carbon monoxide, ethanol, ethane, propylene, propane, butane, butadiene, pentane, pentene, benzene, and toluene.
Optionally, the inert gas is nitrogen, helium, argon or carbon dioxide.
The preparation method of the graphene with the controllable number of layers provided by the embodiment of the application has the following beneficial effects:
by obtaining molten metal; regulating and controlling the temperature field of the molten metal; introducing a carbon-containing gas in the form of bubbles into the bottom of the molten metal; the advancing path of the bubbles in the molten metal is regulated, so that the number of precipitated layers of the graphene can be regulated, a means for effectively controlling the number of layers of the graphene can be provided for the prior art, and the method has an important application prospect.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic flow chart of a method for preparing graphene with controllable layer number according to an embodiment of the present disclosure;
FIG. 2 is a schematic illustration of a catalytic reaction process provided in an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or server that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The performance of graphene is closely related to the number of layers, and graphene with different layers has different physical, chemical and mechanical properties. Therefore, it is an urgent need to solve the problem of providing a method for preparing graphene with controllable layer number.
At present, the chemical vapor deposition of graphene on the surface of metal has two main growth mechanisms, namely surface chemical reaction and dissolution and precipitation. Both growth mechanisms occur depending on the amount of carbon dissolved by the metal. For metals with low dissolved carbon content, the surface chemistry is the predominant reaction, such as copper. In a high-temperature environment, after the carbon-containing gas is catalytically cracked on the surface of the metal, carbon atoms are deposited on the surface of the metal, and the carbon atoms are diffused and gathered on the surface of the metal, so that the graphene is nucleated and further grows up. When the metal surface is completely covered by the single-layer graphene, the graphene isolates the metal from the gas environment, the catalytic reaction does not occur any more, and the reaction stops. Such metal-grown graphene is thus predominantly single-layer graphene. For metals with high dissolved carbon content, the dissolution and precipitation of carbon atoms is the main reaction, such as nickel. In a high-temperature environment, the surface of the metal catalyzes the cracking of carbon-containing gas, and carbon is diffused and infiltrated into the metal after being deposited on the surface of the metal. During the cooling process of the metal, the carbon solubility of the metal decreases with temperature, and a large number of carbon atoms are precipitated to form thick-layer graphene. Therefore, no matter the metal with low carbon content or the metal with high carbon content is dissolved, the prior art lacks a means for effectively controlling the number of graphene layers.
In view of the defects in the prior art, the embodiment of the application provides a preparation method of graphene with controllable layer number. A specific example of a method for preparing graphene with controllable layer number according to the present application is described below, fig. 1 is a schematic flow chart of a method for preparing graphene with controllable layer number according to the present application, and the present specification provides the method operation steps according to the example or the flow chart, but more or fewer operation steps can be included based on conventional or non-inventive labor. The order of steps recited in the embodiments is merely one manner of performing the steps in a multitude of sequences, and does not represent a unique order of performance. Specifically, as shown in fig. 1, the method may include:
s101: obtaining molten metal;
s103: regulating and controlling the temperature field of the molten metal;
s105: introducing a carbon-containing gas in the form of bubbles into the bottom of the molten metal;
s107: and regulating and controlling the traveling path of the bubbles in the molten metal to regulate and control the number of layers of the precipitated graphene.
In the embodiment of the application, molten metal is used, the temperature field of the molten metal is regulated, carbon-containing gas advances in the molten metal in a bubble mode, the advancing path of the bubbles is controlled, the temperature ranges of the bubble paths are different, the supersaturated precipitation of carbon in the metal is caused by the temperature difference formed by the relatively high temperature of the metal carried by the bubbles and the relatively low temperature of the metal, the precipitation amount of the carbon is related to the temperature difference, and therefore the number of layers of the graphene powder is controlled.
In an alternative embodiment, the carbon-containing gas is a mixture of one or more of methane, ethylene, acetylene, carbon monoxide, ethanol, ethane, propylene, propane, butane, butadiene, pentane, pentene, benzene, and toluene.
In an alternative embodiment, step S101, obtaining molten metal comprises:
s1011: placing a catalytic metal material into a crucible;
s1012: and heating the crucible in an inert gas atmosphere until the metal material is in a molten state to obtain molten metal.
Specifically, the metal material is one or a mixture of more of nickel, cobalt, iron, platinum, copper, aluminum, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc, silver, indium and palladium; the inert gas is nitrogen, helium, argon or carbon dioxide.
In an alternative embodiment, the step S103 of regulating the temperature field of the molten metal includes:
creating a temperature gradient of the molten metal by means of a first heating element disposed at the bottom of the crucible and a second heating element disposed at the top of the crucible, such that the bottom temperature of the molten metal is higher than the top temperature of the molten metal; the heating power of the first heating element is greater than the heating power of the second heating element. In the regulation and control process of the temperature field, the convection action possibly exists to enable the high-temperature metal at the bottom to rise, but the actual convection speed is relatively slow, and the method belongs to the controllable range.
Specifically, the temperature difference between the bottom temperature of the molten metal and the top temperature of the molten metal is 0-100 ℃ through heating elements with different powers.
In the embodiment of the application, in step S105, a carbon-containing gas is introduced into the bottom of the molten metal in the form of bubbles, the bubbles of the carbon-containing gas rise from the bottom to the top of the molten metal, and are cracked in the rising process, one carbon atom of the cracked product is dissolved into the molten metal, the carbon concentration in the metal gradually rises along with the passage of time, the metal is nearly saturated, and the carbon atom is separated out from the metal, so that graphene is obtained; the evolution path of carbon atoms is: carbon in the carbon-containing gas → carbon atoms on the bubble interface → carbon atoms dissolved inside the metal → carbon in graphene.
In the embodiment of the present application, considering that if the bubbles rise straight in the molten metal, the rising path is short, and the rising time is fast, resulting in a small amount of precipitated carbon, the traveling path of the bubbles in the molten metal is controlled by step S107, the rising path thereof is extended, and the rising time thereof is delayed; when the bubbles move in molten metal with different temperature gradients, a small amount of metal is carried by the bubbles to move together, and when the metal carried by the bubbles enters a low-temperature area at the top from a high-temperature area at the bottom, the metal carried by the bubbles is supersaturated with carbon and is separated out due to the temperature difference effect, so that graphene is obtained; the precipitation amount of carbon can be controlled by controlling the bubble advancing path and the temperature difference of different temperature zones of the molten metal, so that graphene with different layers can be obtained.
In an alternative embodiment, the step S107 of regulating the traveling path of the bubbles in the molten metal includes:
the use of a stir bar disturbs the straight-rising path of the bubbles in the molten metal.
In another alternative embodiment, after the step S103 of regulating the temperature field of the molten metal and before the step S105 of introducing the carbon-containing gas into the bottom of the molten metal in the form of bubbles, the method further includes:
s104: a gas-liquid two-phase flow guiding device is arranged in the crucible;
correspondingly, in step S105, the controlling the traveling path of the bubbles in the molten metal includes:
and introducing the bubbles from the bottom of the gas-liquid two-phase flow guiding device so as to guide the traveling path of the bubbles through the gas-liquid two-phase flow guiding device.
Specifically, the gas-liquid two-phase flow guiding device is designed into a spiral pipeline form, bubbles are guided to ascend in a spiral path through the spiral pipeline, and compared with a straight ascending path, the spiral ascending path is long, the ascending time is large, and the precipitation amount is large.
It should be noted that the method for regulating the travel path of the bubbles in the molten metal in the present application is not limited to the method using the stirring rod and the gas-liquid two-phase flow guiding device in the above-mentioned alternative embodiment, and in other embodiments, the regulation of the travel path of the bubbles in the molten metal may be realized by adjusting the angle of injecting the carbon-containing gas into the molten metal, and the method related to changing the travel path of the bubbles in the molten metal is within the scope of the present application.
In an alternative embodiment, the method of making further comprises:
s109: graphene overflowing from the molten metal with the inert gas and reaction product gas streams is collected by a collection device.
In the embodiment of the present application, the separated graphene leaves the molten metal along with the inert gas and the reaction product gas (e.g., hydrogen) flow, the gas is separated, and the graphene is continuously collected by the collecting device.
Specific examples 1 to 4 are provided below, in the examples 1 to 4, preparation of graphene is performed by using molten metal copper as a catalytic metal and using a mixed gas of methane and argon as a carbon-containing gas under four different temperature field distributions, respectively, as shown in fig. 2, fig. 2 is a schematic diagram of a catalytic reaction process provided in the example of the present application, and different controls are performed on the temperature field of the molten metal on the left side and the right side in fig. 2, respectively, to show differences.
Example 1:
adding copper powder into a graphite crucible with the depth of 40 cm, heating the crucible in an inert gas atmosphere, and heating until the copper is molten to obtain molten metal copper; controlling the temperature gradient in the crucible to ensure that the bottom temperature of the crucible is 1300 ℃ and the top temperature of the crucible is 1250 ℃; introducing methane and argon mixed gas (the flow rate is 150sccm/10SLM), wherein when bubbles move to the surface of the molten metal copper, the bubbles are broken, the generated graphene leaves the molten metal along with the gas flow, the gas is separated, and the graphene is continuously collected by a collecting device;
example 2:
adding copper powder into a graphite crucible with the depth of 40 cm, heating the crucible in an inert gas atmosphere, and heating until the copper is molten to obtain molten metal copper; controlling the temperature gradient in the crucible to ensure that the temperature at the bottom of the crucible is 1300 ℃ and the temperature at the top of the crucible is 1270 ℃; introducing methane and argon mixed gas (the flow rate is 150sccm/10SLM), wherein when bubbles move to the surface of the molten metal copper, the bubbles are broken, the generated graphene leaves the molten metal along with the gas flow, the gas is separated, and the graphene is continuously collected by a collecting device;
example 3:
adding copper powder into a graphite crucible with the depth of 40 cm, heating the crucible in an inert gas atmosphere, and heating until the copper is molten to obtain molten metal copper; controlling the temperature gradient in the crucible to ensure that the bottom temperature of the crucible is 1300 ℃ and the top temperature of the crucible is 1290 ℃; introducing methane and argon mixed gas (the flow rate is 150sccm/10SLM), wherein when bubbles move to the surface of the molten metal copper, the bubbles are broken, the generated graphene leaves the molten metal along with the gas flow, the gas is separated, and the graphene is continuously collected by a collecting device;
example 4:
placing the graphite spiral pipeline in a graphite crucible with the depth of 40 cm, adding copper powder into the graphite crucible, heating the crucible in an inert gas atmosphere, heating until the copper is molten to obtain molten metal copper, and immersing the whole spiral pipeline into the molten metal copper; controlling the temperature gradient in the crucible to ensure that the bottom temperature of the crucible is 1300 ℃ and the top temperature of the crucible is 1290 ℃; introducing a methane and argon mixed gas (the flow rate is 150sccm/10SLM) at the bottom of the spiral pipeline, leading bubbles to advance spirally under the guidance of the spiral pipeline, breaking the bubbles when the bubbles advance to the surface of molten metal copper, separating the gas, and continuously collecting the gas by a collecting device to obtain graphene, wherein the bubbles are separated from the molten metal along with the gas flow;
sampling the graphene prepared in the embodiments 1 to 4, and measuring the number of graphene layers by using a transmission electron microscope; not less than 5 samples per example, not less than 10 random sample points per sample, and the number of graphene layers measured for each example is shown in the following table:
| serial number | Average number of layers |
| Example 1 | 12.3 |
| Example 2 | 8.6 |
| Example 3 | 2.1 |
| Example 4 | 3.5 |
Therefore, the graphene with different layers can be obtained under different temperature gradients and different advancing routes by regulating and controlling the temperature field of the molten metal and the advancing route of the bubbles; in addition, according to the embodiments 1 to 3, the smaller the temperature difference between the bottom and the top of the molten metal is, the smaller the number of layers is; as can be seen from examples 3 and 4, the longer the bubble travel path, the more the number of layers, and thus the preparation of a specific number of layers of graphene can be achieved according to actual needs.
In summary, according to the preparation method of graphene with controllable layer number provided by the embodiment of the application, carbon-containing gas can be continuously introduced from the bottom of molten metal, and the layer number of the generated graphene can be controlled by regulating and controlling the temperature field of the molten metal and the advancing path of bubbles in the molten metal, so that the preparation method has an important application prospect in practical process application.
It should be noted that: the sequence of the embodiments of the present application is only for description, and does not represent the advantages and disadvantages of the embodiments. And specific embodiments thereof have been described above. Other embodiments are within the scope of the following claims. In some cases, the actions or steps recited in the claims may be performed in a different order than in the embodiments and still achieve desirable results. In addition, the processes depicted in the accompanying figures do not necessarily require the particular order shown, or sequential order, to achieve desirable results. In some embodiments, multitasking and parallel processing may also be possible or may be advantageous.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (3)
1. A preparation method of graphene with controllable layer number is characterized by comprising the following steps:
placing a catalytic metal material into the crucible; the metal material is one or a mixture of more of nickel, cobalt, iron, platinum, copper, aluminum, chromium, gold, manganese, titanium, tin, magnesium, gallium, zinc, silver, indium and palladium;
heating the crucible in an inert gas atmosphere until the metal material is in a molten state to obtain molten metal;
regulating and controlling the temperature field of the molten metal; the regulating the temperature field of the molten metal comprises: creating a temperature gradient of the molten metal by a first heating element disposed at a bottom of the crucible and a second heating element disposed at a top of the crucible such that a bottom temperature of the molten metal is higher than a top temperature of the molten metal; the heating power of the first heating element is larger than that of the second heating element; the temperature difference between the bottom temperature of the molten metal and the top temperature of the molten metal is 10-100 ℃;
introducing a carbon-containing gas in the form of bubbles into the bottom of the molten metal; the carbon-containing gas is one or more mixed gas of methane, ethylene, acetylene, carbon monoxide, ethanol, ethane, propylene, propane, butane, butadiene, pentane, pentene, benzene and toluene;
regulating and controlling the traveling path of the bubbles in the molten metal to regulate and control the number of layers of the precipitated graphene; the regulating the traveling path of the bubbles in the molten metal comprises: introducing the bubbles from the bottom of a gas-liquid two-phase flow guide device in the form of a spiral pipe arranged inside the crucible to guide the traveling path of the bubbles through the gas-liquid two-phase flow guide device, or disturbing the straight-rising path of the bubbles in the molten metal using a stirring rod.
2. The method of claim 1, further comprising:
graphene overflowing from the molten metal with the inert gas and reaction product gas streams is collected by a collection device.
3. The method of claim 1, wherein the inert gas is nitrogen, helium, argon, or carbon dioxide.
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| CN114832729B (en) * | 2022-03-29 | 2023-05-09 | 清华大学 | Device and method for simultaneously producing carbon nano tube and graphene |
| CN115432697B (en) * | 2022-08-15 | 2023-09-19 | 江阴镓力材料科技有限公司 | Preparation method of graphene |
| CN115784214B (en) * | 2023-02-08 | 2023-04-25 | 厦门凯纳石墨烯技术股份有限公司 | Reaction device for graphene growth and graphene preparation method |
| CN116177537A (en) * | 2023-04-28 | 2023-05-30 | 厦门凯纳石墨烯技术股份有限公司 | High-quality graphene powder growth and synchronous hydrogen production method and device |
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Application publication date: 20210611 Assignee: Shanghai Hetian New Material Technology Co.,Ltd. Assignor: Yu Qingkai Contract record no.: X2021990000578 Denomination of invention: A preparation method of graphene with controllable layers License type: Common License Record date: 20210918 |
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