CN106835068B - Roll type graphene continuous growth equipment - Google Patents
Roll type graphene continuous growth equipment Download PDFInfo
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- CN106835068B CN106835068B CN201710186761.4A CN201710186761A CN106835068B CN 106835068 B CN106835068 B CN 106835068B CN 201710186761 A CN201710186761 A CN 201710186761A CN 106835068 B CN106835068 B CN 106835068B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/54—Apparatus specially adapted for continuous coating
- C23C16/545—Apparatus specially adapted for continuous coating for coating elongated substrates
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Abstract
The invention discloses rolled graphene continuous growth equipment capable of synchronously carrying out high-temperature annealing pretreatment and high-temperature growth on a graphene growth substrate. The rolled graphene continuous growth equipment comprises a discharging cooling cavity, a receiving cooling cavity, a first high-temperature process cavity, a second high-temperature process cavity and a transition cavity; the discharging cooling cavity and the receiving cooling cavity are both provided with vacuum pumps; two ends of the first high-temperature process cavity and two ends of the second high-temperature process cavity are both provided with a uniform-flow heat insulation device; the first high-temperature process cavity and the second high-temperature process cavity are both provided with heaters; discharging graphene growth substrates on the graphene growth substrate discharging roller sequentially pass through the discharging cooling zone guide roller, the first high-temperature process cavity, the transition cavity, the second high-temperature process cavity and the receiving cooling cavity guide roller and are finally rolled and received on the graphene substrate receiving roller. Adopt this formula of book graphite alkene continuous growth equipment can guarantee the final quality of graphite alkene film, improve production efficiency.
Description
Technical Field
The invention relates to graphene growing equipment, in particular to rolled graphene continuous growing equipment.
Background
It is well known that: graphene, although only one carbon atom thick, exhibits the most worldwide characteristics due to its own structural properties, such as thinnest, lightest, toughest, least resistivity, etc., and is called "black gold" in the material world, the king of new materials in the 21 st century.
Through extensive research in recent years, chemical vapor deposition is one of the most promising methods for large-scale preparation of graphene films. The CVD method for preparing the high-quality graphene film is to heat and decompose a carbon source into active carbon groups under the vacuum condition of about 1000 ℃, and then further decompose the active carbon groups on a transition metal substrate of Cu, Ni and the like to generate graphene. However, the method for rapidly and continuously preparing the large-area high-quality graphene film in a large scale has not made a great breakthrough, greatly limits the preparation efficiency and yield of the graphene, and hinders the rapid development of the graphene film industry.
The roll-to-roll growth of graphene is a dynamic growth process, and is essentially different from the sheet-type static growth. For the intermittent growth of high-quality graphene on a sheet, the graphene growth substrate is generally subjected to long-time high annealing near the melting point of the graphene growth substrate, so that the polycrystalline growth substrate is recrystallized, the domain area of the growth substrate is increased, and the preparation of a high-quality graphene film is facilitated. Although there are patents beginning to research the equipment and process for preparing graphene in roll-to-roll manner in recent years, it is difficult to realize the controllable preparation of high-quality graphene because only one high-temperature process chamber is provided and annealing and growth are performed simultaneously. For a high-temperature process chamber, if roll-to-roll high-temperature annealing is performed first, and then the annealing is performed again to perform roll-to-roll graphene growth, the graphene growth efficiency is seriously affected. In addition, the influence of high-temperature heat radiation on the sealing device and the problem of uniform distribution of gas in the process chamber are not considered in the previous patents.
Disclosure of Invention
The invention aims to solve the technical problem of providing rolled graphene continuous growth equipment which can separate and synchronously carry out high-temperature annealing pretreatment and high-temperature growth of a graphene growth substrate.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides rolled graphene continuous growth equipment which comprises a feeding cooling cavity, a receiving cooling cavity and a vacuum pump for vacuumizing the feeding cooling cavity and the receiving cooling cavity; the discharging cooling cavity is internally provided with a graphene growth substrate discharging roller and a discharging cooling zone guide roller, and the receiving cooling cavity is internally provided with a graphene growth substrate receiving roller and a receiving cooling cavity guide roller;
the roll type graphene continuous growth equipment further comprises a first high-temperature process cavity, a second high-temperature process cavity and a transition cavity; two ends of the first high-temperature process cavity and two ends of the second high-temperature process cavity are both provided with a uniform-flow heat insulation device; the first high-temperature process cavity and the second high-temperature process cavity are both provided with heaters;
one end of the first high-temperature process cavity is connected and communicated with the discharging cooling cavity, the other end of the first high-temperature process cavity is connected and communicated with the transition cavity, one end of the second high-temperature process cavity is connected and communicated with the transition cavity, and the other end of the second high-temperature process cavity is connected and communicated with the receiving cooling cavity; discharging graphene growth substrates on the graphene growth substrate discharging roller sequentially pass through the discharging cooling zone guide roller, the first high-temperature process cavity, the transition cavity, the second high-temperature process cavity and the receiving cooling cavity guide roller and are finally rolled and received on the graphene substrate receiving roller.
Furthermore, the first high-temperature process cavity is vertically arranged, the second high-temperature process cavity is transversely arranged, and a transition roller is arranged in the transition cavity.
Furthermore, a tension detection device for detecting the tension of the graphene growth substrate is arranged in the transition cavity.
Preferably, the receiving cooling cavity guide roller is a water-cooling guide roller.
Furthermore, both ends of the first high-temperature process cavity are respectively connected with the discharging cooling cavity and the transition cavity through multi-point air inlet sealing flanges, and both ends of the second high-temperature process cavity are respectively connected with the transition cavity and the receiving cooling cavity through multi-point air inlet sealing flanges.
Preferably, the multi-point air inlet sealing flange comprises an outer flange, an inner flange and a sealing rubber ring, the inner flange is provided with a boss end, the outer flange is provided with a groove matched with the inner flange, the sealing rubber ring is installed in the groove, the boss end of the inner flange is inserted into the groove of the outer flange and tightly props up the sealing rubber ring, and a ventilation channel communicated with the inner ring of the inner flange is arranged on the inner flange.
Preferably, the uniform-flow heat insulation device comprises at least two layers of heat insulation boards and a support column, and the support column is arranged between two adjacent layers of heat insulation boards; the heat insulation plates are provided with air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation plates are distributed in a staggered manner.
Furthermore, the central through hole on the heat insulation plate is a radial through groove.
Preferably, the discharging cooling cavity is provided with a vacuum pump, and the receiving cooling cavity is provided with a vacuum pump.
Preferably, the heater is a resistance heater.
The invention has the beneficial effects that: the roll type graphene continuous growth equipment is characterized in that two high-temperature process cavities are arranged between the discharging cooling cavity and the receiving cooling cavity, and the two high-temperature process cavities are separated by the transition cavity; therefore, the high-temperature annealing pretreatment and the high-temperature growth of the graphene growth substrate are respectively carried out in the two high-temperature process cavities and are synchronously carried out, the freedom of temperature setting in the substrate treatment process is solved, process gas in the substrate treatment process can be randomly selected, and the influence of a graphene growth carbon source on the substrate surface treatment process is eliminated. By means of the arrangement of the multiple cavities, all links in the graphene growth process are distributed into all cavities to be performed separately, and the influence of all links in the roll-to-roll growth process on each other is avoided, so that the final quality of a graphene film product is influenced; in addition, all processes can be performed synchronously through the arrangement of the multiple cavities, so that the preparation efficiency of the roll-to-roll graphene film can be improved.
Drawings
FIG. 1 is a schematic structural diagram of two high-temperature process chambers of rolled graphene continuous growth equipment in the embodiment of the invention, wherein one high-temperature process chamber is arranged horizontally, and the other high-temperature process chamber is arranged vertically;
FIG. 2 is a schematic structural diagram of a rolled graphene continuous growth apparatus in which two high-temperature process chambers are arranged laterally;
FIG. 3 is a schematic structural diagram of the vertical arrangement of two high temperature process chambers of the rolled graphene continuous growth apparatus in the embodiment of the present invention;
FIG. 4 is a schematic view of a flow equalization and thermal insulation device according to an embodiment of the present invention;
FIG. 5 is a schematic view of a multi-point inlet seal flange according to an embodiment of the present invention in a transverse configuration;
FIG. 6 is a schematic view of the multi-point inlet sealing flange of an embodiment of the present invention mounted vertically;
the following are marked in the figure: 1-a discharging cooling cavity, 2-a first high-temperature process cavity, 3-a second high-temperature process cavity, 4-a receiving cooling cavity, 41-a graphene-based receiving roller, 42-a receiving cooling cavity guide roller, 5-a transition cavity, 51-a tension detection device, 52-a transition roller, 6-a graphene growth substrate, 7-a vacuum pump, 8-a multi-point air inlet sealing flange, 81-an air channel, 82-an outer flange, 83-an inner flange, 84-a sealing rubber ring, 9-a uniform flow heat insulation device, 91-a heat insulation plate, 92-a support shaft, 93-a central through hole, 10-a heater, 11-a graphene growth substrate discharging roller and 12-a discharging cooling area guide roller.
Detailed Description
The invention is further illustrated with reference to the following figures and examples.
As shown in fig. 1 to 6, the rolled graphene continuous growth apparatus of the present invention includes a discharging cooling chamber 1, a receiving cooling chamber 4, and a vacuum pump 7 for evacuating the discharging cooling chamber 1 and the receiving cooling chamber 4; a graphene growth substrate discharging roller 11 and a discharging cooling zone guide roller 12 are arranged in the discharging cooling cavity 1, and a graphene growth substrate receiving roller 41 and a receiving cooling cavity guide roller 42 are arranged in the receiving cooling cavity 4;
the rolled graphene continuous growth equipment further comprises a first high-temperature process cavity 2, a second high-temperature process cavity 3 and a transition cavity 5; two ends of the first high-temperature process cavity 2 and two ends of the second high-temperature process cavity 3 are both provided with a uniform flow heat insulation device 9; the first high-temperature process cavity 2 and the second high-temperature process cavity 3 are both provided with heaters 10;
one end of the first high-temperature process cavity 2 is connected and communicated with the discharging cooling cavity 1, the other end of the first high-temperature process cavity is connected and communicated with the transition cavity 5, one end of the second high-temperature process cavity 3 is connected and communicated with the transition cavity 5, and the other end of the second high-temperature process cavity is connected and communicated with the receiving cooling cavity 4; the graphene growth substrate 6 is fed on the graphene growth substrate feeding roller 11 and finally wound onto the graphene bottom receiving roller 41 through the feeding cooling zone guide roller 12, the first high-temperature process chamber 2, the transition chamber 5, the second high-temperature process chamber 3 and the receiving cooling chamber guide roller 42 in sequence.
Specifically, the vacuum pump 7 for evacuating the discharging cooling cavity 1 and the receiving cooling cavity 4 mainly functions to evacuate the whole system, and particularly evacuates the discharging cooling cavity 1 and the receiving cooling cavity 4. The discharging cooling cavity 1 and the receiving cooling cavity 4 are vacuumized, and a vacuum pump 7 can be directly arranged between the discharging cooling cavity 1 and the receiving cooling cavity 4; the discharging cooling cavity 1 and the receiving cooling cavity 4 can be respectively provided with a vacuum pump 7 independently or share one vacuum pump 7; the vacuum pump 7 can also be arranged on the high-temperature process cavity or the transition cavity 5, and the multi-cavity process can be separately carried out by air inlet through the sealing flange between the first high-temperature process cavity 2 and the discharging cooling cavity 1 and the sealing flange between the second high-temperature process cavity 3 and the receiving cooling cavity 4.
Specifically, the graphene growth substrate 6 fed on the graphene growth substrate feeding roller 11 sequentially passes through the feeding cooling zone guide roller 12, the first high-temperature process chamber 2, the transition chamber 5, the second high-temperature process chamber 3 and the receiving cooling chamber guide roller 42 and is finally wound on the graphene substrate receiving roller 41, that is, the graphene growth substrate 6 fed on the graphene growth substrate feeding roller 11 is guided by the guide roller 12, then sequentially passes through the first high-temperature process chamber 2, the transition chamber 5 and the second high-temperature process chamber 3, and is not in contact with the inner walls of the respective chambers when passing through the first high-temperature process chamber 2, the transition chamber 5 and the second high-temperature process chamber 3, and finally is finally wound on the graphene substrate receiving roller 41 after being guided by the receiving cooling chamber guide roller 42.
In the production process:
firstly, installing a graphene growth substrate 6 on a graphene growth substrate discharging roller 11 of a discharging cooling cavity 1, and enabling one end of the graphene growth substrate 6 to sequentially pass through a discharging cooling zone guide roller 12, a first high-temperature process cavity 2, a transition cavity 5, a second high-temperature process cavity 3 and a material receiving cooling cavity guide roller 42 through discharging, and winding the graphene growth substrate onto a graphene bottom material receiving roller 41. And then the discharging cooling cavity 1 and the receiving cooling cavity 4 are vacuumized by a vacuum pump. Then, the first high-temperature process cavity 2 is heated by the heater 10 arranged on the first high-temperature process cavity 2, so that the temperature in the first high-temperature process cavity 2 reaches the temperature required by high-temperature annealing of graphene, and the second high-temperature process cavity 3 is heated by the heater 10 arranged on the second high-temperature process cavity 3, so that the temperature in the second high-temperature process cavity 3 reaches the temperature required by growth of graphene; and simultaneously filling corresponding process gas into the high-temperature process cavity. Then, the graphene growth substrate discharging roller 11 is started to discharge, and the graphene substrate receiving roller 41 is started to receive the graphene growth substrate 6. Therefore, the graphene growth substrate 6 is subjected to high-temperature annealing in the first high-temperature process cavity 2 and is grown in the second high-temperature process cavity 3, and continuous production of graphene is achieved.
In summary, the roll-type graphene continuous growth equipment provided by the invention is provided with two high-temperature process chambers between the discharging cooling chamber 1 and the receiving cooling chamber 4, and the two high-temperature process chambers are separated by the transition chamber 5; therefore, the high-temperature annealing pretreatment and the high-temperature growth of the graphene growth substrate are respectively carried out in the two high-temperature process cavities and are synchronously carried out, the freedom of temperature setting in the substrate treatment process is solved, process gas in the substrate treatment process can be randomly selected, and the influence of a graphene growth carbon source on the substrate surface treatment process is eliminated. By means of the arrangement of the multiple cavities, all links in the graphene growth process are distributed into all the cavities to be performed separately, and the influence of the links on the final quality of the graphene growth substrate due to the mutual influence in the roll-to-roll growth process is avoided; in addition, all processes can be performed synchronously through the arrangement of the multiple cavities, so that the preparation efficiency of the roll-to-roll graphene film can be improved.
The first high-temperature process chamber 2 and the second high-temperature process chamber 3 may adopt various arrangement modes, and in order to adapt to an installation environment, one arrangement mode is, as shown in fig. 1, the first high-temperature process chamber 2 is vertically arranged, the second high-temperature process chamber 3 is horizontally arranged, and a transition roller 52 is arranged in the transition chamber 5. Because the first high-temperature process cavity 2 is vertically arranged, and the second high-temperature process cavity 3 is transversely arranged, the transition roller 52 is arranged in the transition cavity 5, so that the graphene growth substrate 6 can be smoothly transited by the first high-temperature process cavity 2 through the transition cavity 5 and enters the second high-temperature process cavity 3, and the contact between the graphene growth substrate 6 and the inner wall of each cavity is avoided.
In order to detect the tension of the graphene growth substrate 6 in real time and obtain the tensile strength of the graphene growth substrate 6, as shown in fig. 2, a tension detection device 51 for detecting the tension of the graphene growth substrate 6 is further disposed in the transition cavity 5. Tension of the 6 base materials of graphene growth base can be monitored by the tension detection device 51, so that the discharging speed of the graphene growth base discharging roller 11 is adjusted according to the tension, the receiving speed of the graphene base receiving roller 41 is controlled, and product quality is guaranteed.
In order to increase the cooling rate of the substrate for growing graphene, in the invention, the receiving cooling cavity guide roller 42 is a water-cooling guide roller. Therefore, the temperature of the substrate for growing the graphene can be quickly reduced to room temperature, and the reduction of the quality of the graphite film caused by thermal expansion and cooling in the rolling process is avoided.
The discharging cooling cavity 1, the first high-temperature process cavity 2, the second high-temperature process cavity 3, the receiving cooling cavity 4 and the transition cavity 5 can be connected through various modes, such as welding or connection by adopting a common flange. In order to facilitate the installation and maintenance of equipment and simultaneously facilitate the introduction of process gas into the process chamber, preferably, both ends of the first high-temperature process chamber 2 are respectively connected with the discharge cooling chamber 1 and the transition chamber 5 through the multipoint gas inlet sealing flange 8, and both ends of the second high-temperature process chamber 3 are respectively connected with the transition chamber 5 and the material receiving cooling chamber 4 through the multipoint gas inlet sealing flange 8.
The multi-point air inlet sealing flange 8 can be in various forms, and in order to simplify the structure, reduce the manufacturing cost and facilitate the installation, one of the preferable modes is as follows: as shown in fig. 5 and 6, the multi-point air inlet sealing flange 8 includes an outer flange 82, an inner flange 83 and a sealing rubber ring 84, the inner flange 83 has a boss end, the outer flange 82 is provided with a groove matched with the inner flange 83, the sealing rubber ring 84 is installed in the groove, the boss end of the inner flange 83 is inserted into the groove of the outer flange 82 and tightly supports the sealing rubber ring 84, and the inner flange 83 is provided with a vent passage 81 communicated with an inner ring of the inner flange 83.
The uniform flow heat insulation device 9 can adopt a single uniform flow heat insulation board, and in order to improve the heat insulation effect and enable the gas to be uniformly distributed in the high-temperature process chamber, preferably, as shown in fig. 4, the uniform flow heat insulation device 9 comprises at least two layers of heat insulation boards 91 and a support column 92, and the support column 92 is arranged between two adjacent layers of heat insulation boards 91; the heat insulation board 91 is provided with a central through hole and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards 91 are distributed in a staggered manner. Specifically, the thermal insulation plate can be made of different materials such as quartz, ceramics, molybdenum, stainless steel, copper and the like, and the quartz thermal insulation plate is preferred in the invention.
By adopting the structure, the uniform-flow heat insulation device 9 can effectively prevent partial heat radiation from influencing the vacuum sealing rubber ring; on the other hand, the process gas can be uniformly dispersed in the process chamber, so that the surfaces of the graphene growth substrates are all in a uniform environment, and the purpose of uniformly preparing the graphene sample is achieved.
Blowing cooling chamber 1 and receipts material cooling chamber 4 all need carry out the evacuation and handle, blowing cooling chamber 1 can use a vacuum pump 7 jointly with receipts material cooling chamber 4 and carry out the evacuation, adopt this kind of setting to be not convenient for to blowing cooling chamber 1 and receive the independent control of material cooling chamber 4 internal pressure, for the ease of blowing cooling chamber 1 and the independent control of receiving material cooling chamber 4 internal pressure, preferred, blowing cooling chamber 1 is provided with a vacuum pump 7, it is provided with a vacuum pump 7 to receive material cooling chamber 4.
The heater 10 may be implemented in various manners, such as resistance heating, infrared heating, electromagnetic field heating, etc., and it is preferable that the heater 10 of the present invention is implemented as a resistance heater in order to control the heating temperature of the heater 10.
Example one
As shown in fig. 1, 4, 5 and 6, the rolled graphene continuous growth apparatus includes a discharging cooling chamber 1 and a receiving cooling chamber 4; a graphene growth substrate discharging roller 11 and a discharging cooling zone guide roller 12 are arranged in the discharging cooling cavity 1, and a graphene growth substrate receiving roller 41 and a receiving cooling cavity guide roller 42 are arranged in the receiving cooling cavity 4; the discharging cooling cavity 1 is provided with a vacuum pump 7, and the receiving cooling cavity 4 is provided with a vacuum pump 7.
The rolled graphene continuous growth equipment further comprises a first high-temperature process cavity 2, a second high-temperature process cavity 3 and a transition cavity 5; two ends of the first high-temperature process cavity 2 and two ends of the second high-temperature process cavity 3 are both provided with a uniform flow heat insulation device 9; the first high-temperature process cavity 2 and the second high-temperature process cavity 3 are both provided with heaters 10; the heater 10 employs a resistance heater.
One end of the first high-temperature process cavity 2 is connected and communicated with the discharging cooling cavity 1 through a multi-point air inlet sealing flange 8, the other end of the first high-temperature process cavity is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, one end of the second high-temperature process cavity 3 is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, and the other end of the second high-temperature process cavity is connected and communicated with the material receiving cooling cavity 4 through the multi-point air inlet sealing flange 8; the graphene growth substrate 6 is fed on the graphene growth substrate feeding roller 11 and finally wound onto the graphene bottom receiving roller 41 through the feeding cooling zone guide roller 12, the first high-temperature process chamber 2, the transition chamber 5, the second high-temperature process chamber 3 and the receiving cooling chamber guide roller 42 in sequence.
As shown in fig. 1, the first high temperature process chamber 2 is vertically arranged, the second high temperature process chamber 3 is horizontally arranged, and a transition roller 52 is arranged in the transition chamber 5.
The multi-point air inlet sealing flange 8 comprises an outer flange 82, an inner flange 83 and a sealing rubber ring 84, wherein the inner flange 83 is provided with a boss end, the outer flange 82 is provided with a groove matched with the inner flange 83, the sealing rubber ring 84 is installed in the groove, the boss end of the inner flange 83 is inserted into the groove of the outer flange 82 and tightly supports the sealing rubber ring 84, and a ventilation channel 81 for communicating the inner ring of the inner flange 83 is arranged on the inner flange 83. The receiving cooling cavity guide roller 42 adopts a water-cooling guide roller.
The uniform flow heat insulation device 9 comprises at least two layers of heat insulation boards 91 and a support column 92, wherein the support column 92 is arranged between two adjacent layers of heat insulation boards 91; the heat insulation board 91 is provided with a central through hole 93 and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards 91 are distributed in a staggered manner.
Example two
As shown in fig. 2, 4, 5 and 6, the rolled graphene continuous growth apparatus includes a discharging cooling chamber 1 and a receiving cooling chamber 4; a graphene growth substrate discharging roller 11 and a discharging cooling zone guide roller 12 are arranged in the discharging cooling cavity 1, and a graphene growth substrate receiving roller 41 and a receiving cooling cavity guide roller 42 are arranged in the receiving cooling cavity 4; the discharging cooling cavity 1 is provided with a vacuum pump 7, and the receiving cooling cavity 4 is provided with a vacuum pump 7.
The rolled graphene continuous growth equipment further comprises a first high-temperature process cavity 2, a second high-temperature process cavity 3 and a transition cavity 5; two ends of the first high-temperature process cavity 2 and two ends of the second high-temperature process cavity 3 are both provided with a uniform flow heat insulation device 9; the first high-temperature process cavity 2 and the second high-temperature process cavity 3 are both provided with heaters 10; the heater 10 employs a resistance heater.
One end of the first high-temperature process cavity 2 is connected and communicated with the discharging cooling cavity 1 through a multi-point air inlet sealing flange 8, the other end of the first high-temperature process cavity is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, one end of the second high-temperature process cavity 3 is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, and the other end of the second high-temperature process cavity is connected and communicated with the material receiving cooling cavity 4 through the multi-point air inlet sealing flange 8; the graphene growth substrate 6 is fed on the graphene growth substrate feeding roller 11 and finally wound onto the graphene bottom receiving roller 41 through the feeding cooling zone guide roller 12, the first high-temperature process chamber 2, the transition chamber 5, the second high-temperature process chamber 3 and the receiving cooling chamber guide roller 42 in sequence.
As shown in fig. 2, the discharging cooling cavity 1, the first high-temperature process cavity 2, the second high-temperature process cavity 3, the receiving cooling cavity 4 and the transition cavity 5 are all transversely arranged; and a tension detection device 51 for detecting the tension of the graphene growth substrate 6 is arranged in the transition cavity 5. The installation is convenient through transverse arrangement, and the tension condition that can detect the graphite alkene through set up tension detection device in the transition chamber controls product quality.
The multi-point air inlet sealing flange 8 comprises an outer flange 82, an inner flange 83 and a sealing rubber ring 84, wherein the inner flange 83 is provided with a boss end, the outer flange 82 is provided with a groove matched with the inner flange 83, the sealing rubber ring 84 is installed in the groove, the boss end of the inner flange 83 is inserted into the groove of the outer flange 82 and tightly supports the sealing rubber ring 84, and a ventilation channel 81 for communicating the inner ring of the inner flange 83 is arranged on the inner flange 83. The receiving cooling cavity guide roller 42 adopts a water-cooling guide roller.
The uniform flow heat insulation device 9 comprises at least two layers of heat insulation boards 91 and a support column 92, wherein the support column 92 is arranged between two adjacent layers of heat insulation boards 91; the heat insulation board 91 is provided with a central through hole 93 and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards 91 are distributed in a staggered manner.
EXAMPLE III
As shown in fig. 3, 4, 5 and 6, the rolled graphene continuous growth apparatus includes a discharging cooling chamber 1 and a receiving cooling chamber 4; a graphene growth substrate discharging roller 11 and a discharging cooling zone guide roller 12 are arranged in the discharging cooling cavity 1, and a graphene growth substrate receiving roller 41 and a receiving cooling cavity guide roller 42 are arranged in the receiving cooling cavity 4; the discharging cooling cavity 1 is provided with a vacuum pump 7, and the receiving cooling cavity 4 is provided with a vacuum pump 7.
The rolled graphene continuous growth equipment further comprises a first high-temperature process cavity 2, a second high-temperature process cavity 3 and a transition cavity 5; two ends of the first high-temperature process cavity 2 and two ends of the second high-temperature process cavity 3 are both provided with a uniform flow heat insulation device 9; the first high-temperature process cavity 2 and the second high-temperature process cavity 3 are both provided with heaters 10; the heater 10 employs a resistance heater.
One end of the first high-temperature process cavity 2 is connected and communicated with the discharging cooling cavity 1 through a multi-point air inlet sealing flange 8, the other end of the first high-temperature process cavity is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, one end of the second high-temperature process cavity 3 is connected and communicated with the transition cavity 5 through the multi-point air inlet sealing flange 8, and the other end of the second high-temperature process cavity is connected and communicated with the material receiving cooling cavity 4 through the multi-point air inlet sealing flange 8; the graphene growth substrate 6 is fed on the graphene growth substrate feeding roller 11 and finally wound onto the graphene bottom receiving roller 41 through the feeding cooling zone guide roller 12, the first high-temperature process chamber 2, the transition chamber 5, the second high-temperature process chamber 3 and the receiving cooling chamber guide roller 42 in sequence.
As shown in fig. 3, the first high temperature process chamber 2 is vertically arranged, the second high temperature process chamber 3 is vertically arranged, and a transition roller 52 is arranged in the transition chamber 5. Through with two high temperature process chamber vertical layout, can reduce the influence of action of gravity to graphite alkene product.
The multi-point air inlet sealing flange 8 comprises an outer flange 82, an inner flange 83 and a sealing rubber ring 84, wherein the inner flange 83 is provided with a boss end, the outer flange 82 is provided with a groove matched with the inner flange 83, the sealing rubber ring 84 is installed in the groove, the boss end of the inner flange 83 is inserted into the groove of the outer flange 82 and tightly supports the sealing rubber ring 84, and a ventilation channel 81 for communicating the inner ring of the inner flange 83 is arranged on the inner flange 83. The receiving cooling cavity guide roller 42 adopts a water-cooling guide roller.
The uniform flow heat insulation device 9 comprises at least two layers of heat insulation boards 91 and a support column 92, wherein the support column 92 is arranged between two adjacent layers of heat insulation boards 91; the heat insulation board 91 is provided with a central through hole 93 and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards 91 are distributed in a staggered manner.
Claims (7)
1. The roll type graphene continuous growth equipment comprises a feeding cooling cavity (1), a receiving cooling cavity (4) and a vacuum pump (7) for vacuumizing the feeding cooling cavity (1) and the receiving cooling cavity (4); a graphene growth substrate discharging roller (11) and a discharging cooling zone guide roller (12) are arranged in the discharging cooling cavity (1), and a graphene substrate receiving roller (41) and a receiving cooling cavity guide roller (42) are arranged in the receiving cooling cavity (4);
the method is characterized in that: the device also comprises a first high-temperature process cavity (2), a second high-temperature process cavity (3) and a transition cavity (5); two ends of the first high-temperature process cavity (2) and two ends of the second high-temperature process cavity (3) are respectively provided with a uniform-flow heat insulation device (9); the first high-temperature process cavity (2) and the second high-temperature process cavity (3) are both provided with heaters (10);
one end of the first high-temperature process cavity (2) is connected and communicated with the discharging cooling cavity (1), the other end of the first high-temperature process cavity is connected and communicated with the transition cavity (5), one end of the second high-temperature process cavity (3) is connected and communicated with the transition cavity (5), and the other end of the second high-temperature process cavity is connected and communicated with the receiving cooling cavity (4); the graphene growth substrate (6) is fed on the graphene growth substrate feeding roller (11) and is finally wound on a graphene substrate receiving roller (41) through a feeding cooling zone guide roller (12), a first high-temperature process cavity (2), a transition cavity (5), a second high-temperature process cavity (3) and a receiving cooling cavity guide roller (42) in sequence;
the two ends of the first high-temperature process cavity (2) are respectively connected with the discharging cooling cavity (1) and the transition cavity (5) through multi-point air inlet sealing flanges (8), and the two ends of the second high-temperature process cavity (3) are respectively connected with the transition cavity (5) and the receiving cooling cavity (4) through the multi-point air inlet sealing flanges (8).
2. The rolled graphene continuous growth apparatus according to claim 1, wherein: the first high-temperature process cavity (2) is vertically arranged, the second high-temperature process cavity (3) is transversely arranged, and a transition roller (52) is arranged in the transition cavity (5).
3. The rolled graphene continuous growth apparatus according to claim 1, wherein: and a tension detection device (51) for detecting the tension of the graphene growth substrate (6) is arranged in the transition cavity (5).
4. The rolled graphene continuous growth apparatus according to claim 1, wherein: the receiving cooling cavity guide roller (42) adopts a water-cooling guide roller.
5. The rolled graphene continuous growth apparatus according to claim 1, wherein: the uniform-flow heat insulation device (9) comprises at least two layers of heat insulation boards (91) and a supporting column (92), wherein the supporting column (92) is arranged between two adjacent layers of heat insulation boards (91); the heat insulation board (91) is provided with a central through hole (93) and air holes which are uniformly distributed, and the air holes on the two adjacent layers of heat insulation boards (91) are distributed in a staggered manner.
6. The rolled graphene continuous growth apparatus according to claim 1, wherein: the discharging cooling cavity (1) is provided with a vacuum pump (7), and the receiving cooling cavity (4) is provided with a vacuum pump (7).
7. The rolled graphene continuous growth apparatus according to claim 1, wherein: the heater (10) adopts a resistance heater.
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| CN107858666A (en) * | 2017-12-13 | 2018-03-30 | 北京创昱科技有限公司 | A kind of integrated chamber of vacuum coating |
| CN110254026A (en) * | 2019-07-23 | 2019-09-20 | 中车工业研究院有限公司 | Using the device of pressure roller worked copper base-graphite alkene |
| CN111072020A (en) * | 2020-01-14 | 2020-04-28 | 烯旺新材料科技股份有限公司 | Efficient graphene roll-to-roll continuous growth equipment and preparation method |
| US20230105104A1 (en) * | 2020-01-17 | 2023-04-06 | Lg Electronics Inc. | Chemical vapor deposition apparatus |
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| CN102492937A (en) * | 2011-12-29 | 2012-06-13 | 中国科学院半导体研究所 | Inlet spray head used for reaction chamber of metal chemical vapor deposition equipment |
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| CN105624640A (en) * | 2016-01-31 | 2016-06-01 | 安徽贝意克设备技术有限公司 | Roll-to-roll continuous grapheme film growth device and technique |
| CN105803522B (en) * | 2016-03-30 | 2018-02-13 | 北京大学 | A kind of continuous method for preparing large single crystal graphene |
| CN105908149B (en) * | 2016-06-30 | 2018-12-14 | 青岛赛瑞达电子科技有限公司 | The roll-to-roll continuous growth apparatus of graphene film |
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