CN111439743A - Manufacturing method capable of continuously and stably producing large-area graphene - Google Patents
Manufacturing method capable of continuously and stably producing large-area graphene Download PDFInfo
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- CN111439743A CN111439743A CN202010083925.2A CN202010083925A CN111439743A CN 111439743 A CN111439743 A CN 111439743A CN 202010083925 A CN202010083925 A CN 202010083925A CN 111439743 A CN111439743 A CN 111439743A
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Abstract
The invention discloses a manufacturing method capable of continuously and stably producing large-area graphene, which comprises the following steps: providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area in the reaction furnace, and further comprising a transition temperature-changing area, wherein the transition temperature-changing area is positioned between the high-temperature area and the low-temperature area, the temperature difference between the high-temperature area and the low-temperature area is at least 30 ℃, the temperature difference between the transition temperature-changing area and the low-temperature area is at least 20 ℃, and a carbon source and alkali metal are placed into the high-temperature area to be mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature area to the low-temperature area through the transition temperature changing area to form a supersaturated solution, and a large-area graphene is precipitated and formed. The invention aims to provide a manufacturing method capable of continuously and stably producing large-area graphene and improving the quality of the graphene.
Description
Technical Field
The invention relates to a manufacturing method capable of continuously and stably producing large-area graphene.
Background
The graphene can be considered as a super material, and theoretically has many excellent properties, such as 1/300 with ultrahigh electron mobility, wherein the electron running speed is the light speed, the experimental measurement value is 1.5 × 105cm2/Vs, which is equivalent to about 100 times of the electron mobility of monocrystalline silicon, which is 2 times of the best material indium gradient recognized at present, the graphene has low resistance, high conductivity, 100 times of the conductivity of copper, good flexibility, high mechanical strength, 1TPa of Young modulus and 2600m2/g of specific surface area theory, and the excellent properties endow the graphene with wide application bases.
Common methods for preparing graphene are: mechanical micro-lift-off, redox, and Chemical Vapor Deposition (CVD). Among them, the simple and efficient method is a redox method. According to the method, graphene is prepared by oxidation and reduction. However, the chemical reduction method and other methods for preparing graphene have certain limitations, such as being not environment-friendly, high in energy consumption, not easy to separate products, and the like, and are not beneficial to the industrial development of graphene.
The invention of Chinese patent application No. 201710061799.9 discloses a method for continuously and stably producing large-area graphene, which comprises the steps of providing a reaction furnace containing a molten solvent, heating the solvent to form a high-temperature region and a low-temperature region having a temperature difference with the high-temperature region in the reaction furnace, wherein the temperature difference is at least 20 ℃, placing a carbon source into the high-temperature region to mix with the solvent to form an initial solution, and flowing the initial solution from the high-temperature region to the low-temperature region to form a supersaturated solution and precipitating the supersaturated solution on a surface of the supersaturated solution to form large-area graphene, wherein the number of layers of the large-area graphene is less than 20 and has a diameter of L a between 1 μm and 1000 μm, and the L a is a value obtained by Raman spectroscopy.
Disclosure of Invention
The invention aims to provide a manufacturing method capable of continuously and stably producing large-area graphene and improving the quality of the graphene.
In order to solve the technical problems, the invention adopts the following technical scheme:
a manufacturing method capable of continuously and stably producing large-area graphene comprises the following steps:
providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area with a temperature difference with the high-temperature area in the reaction furnace, and further comprising a transition temperature-changing area, wherein the transition temperature-changing area is positioned between the high-temperature area and the low-temperature area, the temperature difference between the high-temperature area and the low-temperature area is at least 30 ℃, the temperature difference between the transition temperature-changing area and the low-temperature area is at least 20 ℃, and a carbon source and alkali metal are placed into the high-temperature area to be mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature region to the low-temperature region through the transition temperature region to form a supersaturated solution, and the supersaturated solution is precipitated on one surface of the supersaturated solution to form large-area graphene.
Further, the reaction furnace has a spacer separating the high temperature zone, the transition temperature zone and the low temperature zone.
Further, the high temperature region has a temperature between 450 ℃ and 1400 ℃.
Further, the temperature difference is not higher than 80 ℃.
Furthermore, the carbon source is first deaerated by a deaerator and then supplied to the high temperature region by a feeding device.
Further, the solvent is selected from the group consisting of iron, cobalt, nickel, tantalum, palladium, platinum, lanthanum, cerium, europium and alloys thereof.
Further, the solvent is mixed with an activity-reducing inhibitor selected from the group consisting of gold, silver, copper, lead, zinc and alloys thereof.
Further, the alkali metal is at least one of lithium, sodium and potassium.
Further, the molar ratio of the carbon source to the alkali metal is 50-80: 1.
Compared with the prior art, the invention has the beneficial technical effects that:
according to the invention, by arranging the reasonable transition temperature changing area, the continuous stability in the production process of large-area graphene can be greatly improved, and meanwhile, the production quality of the graphene is improved by adding alkali metal.
Detailed Description
Example 1
A manufacturing method capable of continuously and stably producing large-area graphene comprises the following steps:
providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area with a temperature difference with the high-temperature area in the reaction furnace, and further comprising a transition temperature-changing area, wherein the transition temperature-changing area is positioned between the high-temperature area and the low-temperature area, the temperature difference between the temperature of the high-temperature area (the temperature is 400-1400 ℃) and the temperature of the transition temperature-changing area is 5 ℃, the temperature difference between the transition temperature-changing area and the low-temperature area is 30 ℃, and a carbon source and alkali metal sodium (the molar ratio of the carbon source to the alkali metal is 50: 1) are placed into the high-temperature area to be mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature region to the low-temperature region through the transition temperature region to form a supersaturated solution, and the supersaturated solution is precipitated on one surface of the supersaturated solution to form large-area graphene.
In this embodiment: the carbon source is first deaerated by a deaerating device to remove an oxygen component contained therein, and then is supplied to the high temperature region through a feeding device. The solvent is selected from the group consisting of iron, cobalt, nickel, tantalum, palladium, platinum, lanthanum, cerium, europium and alloys thereof. The solvent is mixed with an activity-reducing inhibitor selected from the group consisting of gold, silver, copper, lead, zinc and alloys thereof.
Example 2
A manufacturing method capable of continuously and stably producing large-area graphene comprises the following steps:
providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area with a temperature difference with the high-temperature area in the reaction furnace, and further comprising a transition temperature-changing area, wherein the transition temperature-changing area is positioned between the high-temperature area and the low-temperature area, the temperature difference between the temperature of the high-temperature area (the temperature is 400-1400 ℃) and the temperature of the transition temperature-changing area is 8 ℃, the temperature difference between the transition temperature-changing area and the low-temperature area is 40 ℃, and a carbon source and alkali metal lithium (the molar ratio of the carbon source to the alkali metal lithium is 80: 1) are placed into the high-temperature area to be mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature region to the low-temperature region through the transition temperature region to form a supersaturated solution, and the supersaturated solution is precipitated on one surface of the supersaturated solution to form large-area graphene.
In this embodiment: the carbon source is first deaerated by a deaerating device to remove an oxygen component contained therein, and then is supplied to the high temperature region through a feeding device. The solvent is selected from the group consisting of iron, cobalt, nickel, tantalum, palladium, platinum, lanthanum, cerium, europium and alloys thereof. The solvent is mixed with an activity-reducing inhibitor selected from the group consisting of gold, silver, copper, lead, zinc and alloys thereof.
Comparative example 1
A manufacturing method capable of continuously and stably producing large-area graphene comprises the following steps:
providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area with a temperature difference with the high-temperature area in the reaction furnace, wherein the temperature difference between the high-temperature area (the temperature is 400-1400 ℃) and the low-temperature area is 20-40 ℃, and placing a carbon source into the high-temperature area to be mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature region to the low-temperature region through the transition temperature region to form a supersaturated solution, and the supersaturated solution is precipitated on one surface of the supersaturated solution to form large-area graphene.
In this embodiment: the carbon source is first deaerated by a deaerating device to remove an oxygen component contained therein, and then is supplied to the high temperature region through a feeding device. The solvent is selected from the group consisting of iron, cobalt, nickel, tantalum, palladium, platinum, lanthanum, cerium, europium and alloys thereof. The solvent is mixed with an activity-reducing inhibitor selected from the group consisting of gold, silver, copper, lead, zinc and alloys thereof.
Compared with the comparative example, the examples 1 and 2 not only can more effectively realize the continuous and stable production of large-area graphene, but also the quality of the produced graphene is obviously superior to that of the comparative example. The electrical property and the mechanical property are detected by the comparison example, and the performance is more excellent particularly on the electrical property.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. A manufacturing method capable of continuously and stably producing large-area graphene comprises the following steps:
providing a reaction furnace, wherein the reaction furnace contains a molten solvent; heating the solvent to enable the solvent to form a high-temperature area and a low-temperature area with a temperature difference with the high-temperature area in the reaction furnace, wherein the temperature difference between the high-temperature area and the low-temperature area is at least 30 ℃, the temperature difference between the high-temperature area and the low-temperature area is at least 20 ℃, and a carbon source and alkali metal are placed into the high-temperature area and mixed with the solvent to form an initial solution; the initial solution flows from the high-temperature region to the low-temperature region through the transition temperature region to form a supersaturated solution, and the supersaturated solution is precipitated on one surface of the supersaturated solution to form large-area graphene.
2. The method as claimed in claim 1, wherein the reaction furnace has a spacer for spacing the high temperature region, the transition temperature region and the low temperature region.
3. The method of claim 1, wherein the high temperature region has a temperature of 450 ℃ to 1400 ℃.
4. The method according to claim 1, wherein the temperature difference is not higher than 80 ℃.
5. The method of claim 1, wherein the carbon source is removed an oxygen component by an oxygen removal device and then fed to the high temperature region through a feeding device.
6. The method of claim 1, wherein the solvent is selected from the group consisting of Fe, Co, Ni, Ta, Pd, Pt, La, Ce, Eu and their alloys.
7. The method of claim 1, wherein the solvent is mixed with an activity-reducing inhibitor selected from the group consisting of gold, silver, copper, lead, zinc, and alloys thereof.
8. The method according to claim 1, wherein the alkali metal is at least one of lithium, sodium, and potassium.
9. The method according to claim 1 or 8, wherein the molar ratio of the carbon source to the alkali metal is 50-80: 1.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106946241A (en) * | 2017-01-26 | 2017-07-14 | 北京清烯科技有限公司 | The manufacture method of large-area graphene |
| CN107119316A (en) * | 2017-04-13 | 2017-09-01 | 孙旭阳 | A kind of temperature-varying zone liquid bed Direct precipitation grows the preparation method of graphene |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106946241A (en) * | 2017-01-26 | 2017-07-14 | 北京清烯科技有限公司 | The manufacture method of large-area graphene |
| CN107119316A (en) * | 2017-04-13 | 2017-09-01 | 孙旭阳 | A kind of temperature-varying zone liquid bed Direct precipitation grows the preparation method of graphene |
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