CN217895149U - Quartz crucible and graphene manufacturing device - Google Patents

Quartz crucible and graphene manufacturing device Download PDF

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Publication number
CN217895149U
CN217895149U CN202221365262.4U CN202221365262U CN217895149U CN 217895149 U CN217895149 U CN 217895149U CN 202221365262 U CN202221365262 U CN 202221365262U CN 217895149 U CN217895149 U CN 217895149U
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quartz crucible
coating
graphene
side wall
radiation coating
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胡思茹
郭海峰
肖市明
梅婷婷
方平涛
王文斌
宋怡霏
杨康运
王宗丽
郑虹
祁琪
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Pingxiang University
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Pingxiang University
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Abstract

The utility model provides a quartz crucible and graphite alkene manufacturing installation belongs to high radiance coating technical field, and quartz crucible includes inside wall and lateral wall, and at least one of inside wall and lateral wall is provided with the radiation coating. At least one of the inner side wall and the outer side wall of the quartz crucible is provided with the radiation coating, so that a gradient temperature field can be formed in the quartz crucible when graphene is manufactured, carbon atoms are deposited layer by layer along with the gradient temperature field in the vaporization process, and graphene with high quality is formed.

Description

Quartz crucible and graphene manufacturing device
Technical Field
The utility model belongs to the technical field of the high radiance coating, concretely relates to quartz crucible and graphite alkene manufacturing installation.
Background
The graphene has an ultra-large specific surface area and ultra-strong adsorption and desorption capacity, is an ideal material for sewage treatment, has ultra-strong conductivity, and has a wide application prospect in the fields of new energy, electronic information and the like. The mainstream production method of graphene at present is a redox method, which is simple to operate and high in yield, but the product quality is low. The oxidation-reduction method uses strong acid such as sulfuric acid, nitric acid and the like, has great danger, needs to use a large amount of water for cleaning, generates a large amount of waste acid, and seriously pollutes the environment.
The university of rice in 2020 invented joule heat flash evaporation technology [ Nature,2020, 577. The Joule thermal flash evaporation technology is expected to realize green manufacturing of graphene. The method is essentially characterized in that amorphous carbon is vaporized at the temperature of more than 3000K, and then is deposited and crystallized to the surrounding low-temperature field to form graphene, so that the quality of the graphene is directly influenced by the temperature field in the quartz crucible, and the gradient temperature field is favorable for forming high-quality graphene. Therefore, in order to form the gradient temperature field in quartz crucible, improve the quality of discharge manufacturing graphite alkene, the utility model provides a quartz crucible and graphite alkene manufacturing installation.
SUMMERY OF THE UTILITY MODEL
The utility model discloses aim at solving one of the technical problem that exists among the prior art at least, provide a quartz crucible and graphite alkene manufacturing installation.
An aspect of the utility model provides a quartz crucible, quartz crucible includes inside wall and lateral wall, the inside wall with at least one in the lateral wall is provided with the radiation coating.
Optionally, the inner side wall and the outer side wall are both provided with the radiation coating.
Optionally, the radiation coating on the inner sidewall is in a dense film structure.
Optionally, the radiation coating on the outer sidewall is in a porous membrane structure.
Optionally, the thickness of the radiation coating ranges from 1 μm to 10 μm.
Optionally, the radiation coating is a high-emissivity ceramic slurry coating.
Optionally, the radiation coating includes a high-emissivity ceramic powder substrate and curing agent particles doped in the high-emissivity ceramic powder substrate.
Another aspect of the utility model provides a graphite alkene manufacturing installation, including capacitor bank and the foretell quartz crucible, the capacitor bank is used for placing amorphous carbon heating by discharge in the quartz crucible.
The utility model discloses a quartz crucible and graphite alkene manufacturing installation, quartz crucible include inside wall and lateral wall, and at least one in inside wall and the lateral wall is provided with the radiation coating. At least one of the inner side wall and the outer side wall of the quartz crucible is provided with the radiation coating, so that a gradient temperature field can be formed in the quartz crucible when graphene is manufactured, carbon atoms are deposited layer by layer along with the gradient temperature field in the vaporization process, and graphene with high quality is formed.
Drawings
FIG. 1 is a schematic view of a quartz crucible according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view of a quartz crucible according to an embodiment of the present invention.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1 and 2, an aspect of the present invention provides a quartz crucible 100, the quartz crucible 100 comprising an inner sidewall (not shown) and an outer sidewall (not shown), at least one of the inner sidewall and the outer sidewall being provided with a radiation coating. That is, the radiation coating may be provided on the inner side wall of the quartz crucible 100, or the radiation coating may be provided on the outer side wall of the quartz crucible 100.
When graphene is manufactured, amorphous conductive carbon powder is slightly compressed between two electrodes, the amorphous conductive carbon powder is placed in a quartz crucible 100, and a carbon source reaches a temperature of more than 3000 ℃ within 2 seconds through high-voltage discharge of a capacitor bank, so that amorphous carbon is converted into orderly stacked graphene. At 3000 ℃, carbon atoms are vaporized and deposited to a low-temperature field to quickly form graphene. The radiation coating arranged on the inner side wall or the outer side wall of the quartz crucible can reduce heat brought away by carbon atom vaporization, so that more heat can be radiated repeatedly in the reaction cavity, the heat efficiency is effectively improved by 10%, a gradient temperature field is formed in the reaction cavity, and carbon atoms are deposited layer by layer along with the gradient temperature field in the vaporization process to form high-quality graphene.
The utility model discloses quartz crucible is provided with the radiation coating through at least one in quartz crucible's inside wall and lateral wall, when making graphite alkene, can form the gradient temperature field in quartz crucible, makes the carbon atom deposit along with gradient temperature field successive layer at the in-process of vaporization, forms the higher graphite alkene of quality.
Further optimally, both the inner side wall and the outer side wall are provided with a radiation coating. As shown in fig. 1 and 2, that is, the quartz crucible 100 is provided on the inner sidewall with an inner sidewall radiation coating 111 and on the outer sidewall with an outer sidewall coating 112. That is, the quartz crucible 100 has a dual radiation coating structure.
In the above embodiment, due to the dual-radiation coating structure disposed on the quartz crucible 100, when graphene is manufactured, the heat resistance of the reaction chamber can be effectively improved, heat dissipation in the reaction chamber can be reduced, heat loss can be reduced, and the thermal efficiency can be significantly improved by 20% to 30%. And forming a gradient temperature field in the reaction cavity, and depositing carbon atoms layer by layer along with the gradient temperature field in the vaporization process to form high-quality graphene, wherein the Raman value 2D/G is 13-17.
Illustratively, the radiation coating on the inner sidewall is in a dense film structure. As shown in fig. 1 and 2, that is, the inner sidewall radiation coating 111 has a dense film structure. The dense membrane structure of the inner side wall can reduce the loss of heat, so that the heat generated by the rapid discharge of the capacitor can be concentrated in the reaction cavity.
Illustratively, the radiation coating on the outer sidewall is in a porous membrane structure. As shown in fig. 1, that is, the outer sidewall coating 112 has a porous membrane structure. The porous membrane structure has the characteristics of high temperature resistance and small heat conductivity, so that the heat dissipation of the reaction cavity is reduced.
Illustratively, the thickness of the radiation coating ranges from 1 μm to 10 μm.
Illustratively, the radiation coating is a high emissivity ceramic slurry coating. Further, the radiation coating comprises a high-emissivity ceramic powder substrate and curing agent particles doped in the high-emissivity ceramic powder substrate.
Another aspect of the utility model provides a graphite alkene manufacturing installation, including capacitor bank and the foretell quartz crucible, the capacitor bank is used for the amorphous carbon discharge heating of placing in quartz crucible. The specific structure of the quartz crucible has been described in detail above and will not be described in detail herein.
Specifically, amorphous conductive carbon powder is slightly compressed between two electrodes, placed in a quartz crucible 100, and a carbon source is brought to a temperature of 3000 ℃ or more within 2 seconds by high-voltage discharge of a capacitor bank, so that amorphous carbon is converted into orderly-stacked graphene. At 3000 ℃, carbon atoms are vaporized and deposited to a low-temperature field to quickly form graphene.
The forming process of the radiation coating of the quartz crucible of the utility model is as follows:
step 1, preparing a high-emissivity ceramic slurry coating.
Specifically, the mass ratio of the high-emissivity ceramic powder in the prepared high-emissivity ceramic slurry coating to the slurry is 30-50%, the added curing agent particles are one or more of sodium silicate, potassium silicate and silica sol, and the high-emissivity ceramic slurry coating is formed by ball milling for 1-3 hours. Wherein, the high-radiance ceramic raw material comprises 10-50% of copper-chromium black, 10-40% of titanium dioxide and 10-40% of zirconium dioxide.
And 2, pretreating the quartz crucible 100.
Specifically, the quartz crucible 100 is soaked in an alkali solution for 1-3 hours, wherein the alkali is one or two of NaOH and KOH, and the concentration of the alkali solution is 2-5 wt%.
And 3, coating the high-radiation ceramic slurry coating on the pretreated quartz crucible 100 to form a compact inner wall and/or porous outer wall coating, drying, curing and then carrying out heat treatment to obtain the radiation coating structure on the quartz crucible wall.
Specifically, the coating thickness of the coating is 1-10 μm, the drying and curing temperature of the blank is 80-160 ℃, the heat treatment temperature is 500-1000 ℃, and the heat preservation time is 1-4 h.
The process of forming the radiation coating of the quartz crucible 100 in this embodiment is further illustrated by several specific examples.
Example 1
The embodiment provides a non-coating structure of a quartz crucible 100, which comprises the following specific processes: the quartz crucible 100 is put into an alkali solution for soaking for 1h to 3h, and the pretreated quartz crucible 100 is dried. Amorphous conductive carbon powder is slightly compressed between two electrodes, the amorphous conductive carbon powder is placed in a quartz crucible 100, and the carbon source reaches the temperature of more than 3000 ℃ within 2 seconds through high-voltage discharge of a capacitor bank, so that amorphous carbon can be converted into orderly-stacked graphene. At 3000 ℃, carbon atoms are vaporized and deposited to a low-temperature field to quickly form graphene, the Raman value 2D/G is 6-9, and the quality of the graphene is low.
Example 2
The present embodiment provides a quartz crucible 100 with a radiation coating on the outer sidewall, which comprises the following steps:
firstly, preparing a high-emissivity ceramic slurry coating, wherein the high-emissivity ceramic powder in the prepared slurry accounts for 30-50% of the mass of the slurry, the added curing agent particles are sodium silicate and potassium silicate, the mixture is ball-milled for 1-3h to form high-emissivity ceramic slurry, and then pore-forming agent is added to be dissolved in the slurry to form casting solution.
Meanwhile, the quartz crucible 100 is placed in an alkali solution for soaking for 1 h-3 h, and the pretreated quartz crucible is dried. Coating the prepared casting solution on the outer side wall of the pretreated quartz crucible 100, wherein the coating thickness is 1-10 mu m, the drying and curing temperature of the blank is 80-160 ℃, the heat treatment temperature is 500-1000 ℃, and the heat preservation time is 1-4 h. After drying and curing, heat treatment is carried out, and the quartz crucible 100 with the outer side wall in the porous membrane ceramic coating structure is obtained.
Then, amorphous conductive carbon powder is slightly compressed between two electrodes, the mixture is placed in a quartz crucible 100, and a carbon source reaches a temperature of more than 3000 ℃ within 2 seconds through high-voltage discharge of a capacitor bank, so that amorphous carbon is converted into orderly-stacked graphene. At 3000 ℃, carbon atoms are vaporized and deposited to a low-temperature field to quickly form graphene. The porous membrane has the characteristics of high temperature resistance and small heat conductivity, so that the heat dissipation of the reaction cavity is reduced. Meanwhile, the high-radiation ceramic coating technology can reduce the heat taken away by carbon atom vaporization, so that more heat is radiated repeatedly in the reaction cavity, the heat efficiency is effectively improved by 10%, a gradient temperature field is formed in the reaction cavity, and carbon atoms are deposited layer by layer along with the gradient temperature field in the vaporization process to form high-quality graphene.
Example 3
The present embodiment provides a quartz crucible 100 with a radiation coating on the inner sidewall, which comprises the following steps:
firstly, preparing a high-emissivity ceramic slurry coating, wherein the mass ratio of high-emissivity ceramic powder in the prepared slurry to the slurry is 30-50%, the added curing agent particles are sodium silicate and potassium silicate, and the high-emissivity ceramic slurry is formed by ball milling for 1-3 h.
Meanwhile, the quartz crucible 100 is placed into an alkali solution to be soaked for 1h to 3h, and the pretreated quartz crucible is dried. And then coating the prepared high-radiation ceramic coating on the inner side wall of the pretreated quartz crucible 100 by adopting a casting method, so that the inner side wall of the quartz crucible 100 forms a compact film ceramic coating structure. The coating thickness of the coating is 1-10 μm, the drying and curing temperature of the blank is 80-160 ℃, the heat treatment temperature is 500-1000 ℃, and the heat preservation time is 1-4 h. After drying and curing, heat treatment is carried out, and the compact film ceramic coating structure on the inner side wall of the quartz crucible 100 is obtained.
Then, amorphous conductive carbon powder is slightly compressed between two electrodes, the mixture is placed in a quartz crucible 100, and the carbon source reaches a temperature of more than 3000 ℃ within 2 seconds through high-voltage discharge of a capacitor bank, so that the amorphous carbon can be converted into orderly stacked graphene. At 3000 ℃, carbon atoms are vaporized and deposited to a low-temperature field to quickly form graphene. The structure of the dense film on the inner wall can reduce the loss of heat, so that the heat generated by the rapid discharge of the capacitor can be concentrated in the reaction cavity. Meanwhile, the high-radiation ceramic coating technology can reduce the heat taken away by carbon atoms through vaporization, so that more heat is radiated repeatedly in the reaction cavity, the heat efficiency is effectively improved by 10%, a gradient temperature field is formed in the reaction cavity, the carbon atoms are deposited layer by layer along with the gradient temperature field in the vaporization process, graphene with high quality is formed, and the Raman value 2D/G is 11-14.
Example 4
The embodiment provides a quartz crucible with radiation coatings on the inner side wall and the outer side wall, and the specific process is as follows: firstly, preparing a high-emissivity ceramic slurry coating, wherein the mass ratio of high-emissivity ceramic powder in the prepared slurry to the slurry is 30-50%, the added curing agent particles are sodium silicate and potassium silicate, and the high-emissivity ceramic slurry is formed by ball milling for 1-3 h.
Meanwhile, the quartz crucible 100 is placed into an alkali solution to be soaked for 1h to 3h, and the pretreated quartz crucible is dried. And coating the prepared high-radiation ceramic coating on the inner side wall and the outer side wall of the pretreated quartz crucible to form a compact film structure on the inner side wall and a porous film structure on the outer side wall. The coating thickness of the coating is 1-10 μm, the drying and curing temperature of the blank is 80-160 ℃, the heat treatment temperature is 500-1000 ℃, and the heat preservation time is 1-4 h. After drying and curing, heat treatment is carried out, and the double-radiation ceramic coating structure on the wall of the quartz crucible 100 is obtained.
Then, amorphous conductive carbon powder is slightly compressed between two electrodes, the amorphous conductive carbon powder is placed in a quartz crucible 100, and the carbon source reaches the temperature of more than 3000 ℃ within 2 seconds through high-voltage discharge of a capacitor bank, so that amorphous carbon can be converted into orderly-stacked graphene. At 3000 ℃, carbon atoms are vaporized and are deposited in a low-temperature field to quickly form graphene, and the added double-radiation ceramic coating can effectively improve the heat resistance of the reaction cavity, reduce the heat dissipation in the reaction cavity, reduce the heat loss and obviously improve the thermal efficiency by 20-30%. And forming a gradient temperature field in the reaction cavity, and depositing carbon atoms layer by layer along with the gradient temperature field in the vaporization process to form high-quality graphene, wherein the Raman value 2D/G is 13-17.
Furthermore, the present invention emphasizes again pointing out: the process flow adopted by the utility model belongs to the prior art, only one example is illustrated in the specific embodiment, the process flow of the embodiment can not be limited to the specific process flow of the application, and all the process flows of the formula, the additive, the coating, the heat treatment and the like adopted in the field can be applied to the application.
It is to be understood that the above embodiments are merely exemplary embodiments that have been employed to illustrate the principles of the present invention, and that the present invention is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.

Claims (6)

1. The quartz crucible is used for manufacturing graphene and is characterized by comprising an inner side wall and an outer side wall, wherein at least one of the inner side wall and the outer side wall is provided with a radiation coating, and the radiation coating adopts a high-emissivity ceramic slurry coating.
2. The quartz crucible of claim 1, wherein the inner sidewall and the outer sidewall are each provided with the radiant coating.
3. The quartz crucible of claim 2, wherein the radiation coating on the inner sidewall is in a dense film structure.
4. The quartz crucible of claim 2, wherein the radiation coating on the outer sidewall is in a porous membrane configuration.
5. The quartz crucible of any of claims 1 to 4, wherein the radiation coating has a thickness in the range of 1 μm to 10 μm.
6. A graphene manufacturing apparatus, characterized by comprising a capacitor bank for discharge heating of amorphous carbon placed in the quartz crucible and the quartz crucible of any one of claims 1 to 5.
CN202221365262.4U 2022-06-02 2022-06-02 Quartz crucible and graphene manufacturing device Active CN217895149U (en)

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Application Number Priority Date Filing Date Title
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Publication Number Publication Date
CN217895149U true CN217895149U (en) 2022-11-25

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