CN209974884U - Continuous growth equipment for graphene metal composite powder - Google Patents
Continuous growth equipment for graphene metal composite powder Download PDFInfo
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- CN209974884U CN209974884U CN201822232542.8U CN201822232542U CN209974884U CN 209974884 U CN209974884 U CN 209974884U CN 201822232542 U CN201822232542 U CN 201822232542U CN 209974884 U CN209974884 U CN 209974884U
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Abstract
The utility model discloses a compound powder continuous growth equipment of graphite alkene metal, including consecutive sample chamber, CVD tube furnace and cooling chamber, still include vacuum unit, gas supply system and heating device, vacuum unit and gas supply system are equallyd divide and are do not connected with sample chamber, CVD tube furnace and cooling chamber, heating device is connected with CVD tube furnace, intercommunication mouth department between CVD tube furnace and the sample chamber is equipped with first vacuum flapper valve, and intercommunication mouth department between CVD tube furnace and the cooling chamber is equipped with second vacuum flapper valve. The utility model discloses a continuous growth equipment of graphite alkene metal composite powder improves production efficiency, enlarges production scale, reduces the energy consumption.
Description
Technical Field
The utility model relates to a low voltage apparatus technical field, concretely relates to compound powder continuous growth equipment of graphite alkene metal.
Background
Graphene is a sheet-shaped structural material formed by carbon atoms in sp2 hybridized orbitals, is a hexagonal two-dimensional film-shaped carbon nano material in a honeycomb lattice structure, and is a two-dimensional material with the thickness of only one carbon atom in a single-layer graphene. Due to the special chemical structure of graphene, graphene has important application prospects in the aspects of materials science, micro-nano processing, energy, detection, biomedicine and drug delivery, shows excellent characteristics of electricity, optics, heat, mechanics and the like, is considered to be a novel material with revolutionary significance, and has attracted extensive attention in application and development in various fields.
The preparation method of graphene powder is various, and Chemical Vapor Deposition (CVD) has been highly approved for preparing high-quality graphene. CVD refers to a process of introducing a gaseous reactant containing elements constituting a graphene film, vapor of a liquid or solid reactant, and other gases required for reaction into a reaction chamber, and forming a film on a bottom surface through a chemical reaction under a certain condition.
At present, graphene film growth CVD equipment is relatively mature, and particularly relates to a roll-to-roll continuous growth furnace for growing large-size graphene films and a static CVD growth furnace for scientific research and small-scale experiments. Most of the substrates are large-size materials such as flat plates, thin films, porous macroscopic bodies and the like, and for micro-size substrates such as powder and the like, no special CVD continuous growth equipment exists at present, and the substrates are grown in a single furnace by adopting general-purpose CVD equipment. The general process flow is as follows: sample pretreatment, sample loading, vacuumizing, protective gas introduction, heating, process gas introduction, heat preservation, protective gas introduction, cooling to room temperature and sampling. The process has low efficiency and high energy consumption, the prepared powder has poor quality uniformity, and the continuous growth of the graphene metal composite powder with high efficiency and large batch is difficult to realize.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's defect, provide a graphite alkene metal composite powder continuous growth equipment that can improve production efficiency, enlarge production scale, low energy consumption.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides a continuous growth equipment of graphite alkene metal composite powder, includes sampling chamber 1, CVD tubular furnace 2 and cooling chamber 3 that link to each other in proper order, still includes vacuum unit 11, gas supply system 8 and heating device 4, vacuum unit 11 and gas supply system 8 are equallyd divide and are connected with sampling chamber 1, CVD tubular furnace 2 and cooling chamber 3 respectively, heating device 4 is connected with CVD tubular furnace 2, the intercommunication mouth department between CVD tubular furnace 2 and the sampling chamber 1 is equipped with first vacuum flapper valve 6, and the intercommunication mouth department between CVD tubular furnace 2 and the cooling chamber 3 is equipped with second vacuum flapper valve 15.
Preferably, the device also comprises a radio frequency power supply 9 and a radio frequency plasma generator 5 which are matched, wherein the radio frequency plasma generator 5 is connected with the CVD tube furnace 2.
Preferably, a first vacuum magnetic sample transmission rod 7 for transmitting samples between the sample inlet chamber 1 and the CVD tube furnace 2 is arranged in the sample inlet chamber, and a second vacuum magnetic sample transmission rod 16 for transmitting samples between the CVD tube furnace 2 and the temperature reduction chamber 3 is arranged in the sample inlet chamber and the CVD tube furnace.
Preferably, two cooling devices 14 are arranged on the outer wall of the CVD tube furnace 2 at both ends of the CVD tube furnace 2, and the two cooling devices 14 are respectively connected with the first vacuum flapper valve 6 and the second vacuum flapper valve 15.
Preferably, the CVD tube furnace 2 is correspondingly connected with the multi-path gas supply system 8 through a plurality of temperature-resistant gas inlet pipelines 13, and the temperature-resistant gas inlet pipelines 13 penetrate through the side wall of the CVD tube furnace 2 and are communicated with the interior of the CVD tube furnace 2.
Preferably, the heating device 4 is installed on the outer wall of the CVD tube furnace 2, and the heating device 4 is provided with a plurality of avoidance holes for avoiding a plurality of temperature-resistant gas inlet pipes 13.
Preferably, each temperature-resistant air inlet pipeline 13 is provided with a flow controller at the connection part with the air supply system 8.
Preferably, two heat insulation devices 12 are arranged on the inner wall of the CVD tube furnace 2 and positioned at two ends of the CVD tube furnace 2, and the heat insulation devices 12 are aligned with the communication ports at two ends of the CVD tube furnace 2.
Preferably, the CVD tube furnace 2 is provided with an exhaust port 17 at each end.
Preferably, the plurality of quartz or metal temperature-resistant inlet pipes 13 are regularly arranged.
The utility model discloses a compound powder continuous growth equipment of graphite alkene metal, sampling chamber, CVD tube furnace and cooling room all have independent air supply system and vacuum unit, have solved the continuous growth problem of compound powder of graphite alkene metal, improve production efficiency, the enlarging production scale, low energy consumption. The method is particularly suitable for the continuous growth of graphene adopting micro-size such as powder as a substrate.
Drawings
Fig. 1 is a perspective view of the continuous growth apparatus for graphene-metal composite powder according to the present invention;
fig. 2 is a cross-sectional view of a continuous chamber of the continuous graphene metal composite powder growing apparatus of the present invention;
FIG. 3 is a top cross-sectional view of the CVD tube furnace of the present invention.
Detailed Description
The following describes a specific embodiment of the graphene metal composite powder continuous growth apparatus according to the present invention with reference to the embodiments shown in fig. 1 to 3. The utility model discloses a continuous growth equipment of graphite alkene metal composite powder is not limited to the description of following embodiment.
As shown in fig. 1-2, the utility model discloses a continuous growth equipment of compound powder of graphite alkene metal, including sampling room 1, CVD tubular furnace 2, cooling chamber 3, heating device 4, switch board 10 and set up vacuum unit 11 and the air supply system 8 in switch board 10, sampling room 1, CVD tubular furnace 2 and cooling chamber 3 link to each other in proper order and constitute continuous chamber, vacuum unit 11 and air supply system 8 are equallyd divide and are connected with sampling room 1, CVD tubular furnace 2 and cooling chamber 3 respectively, heating device 4 is connected with CVD tubular furnace 2, the intercommunication mouth department between CVD tubular furnace 2 and the sampling room 1 is equipped with first vacuum flapper valve 6, and the intercommunication mouth department between CVD tubular furnace 2 and the cooling chamber 3 is equipped with second vacuum flapper valve 15. The sample chamber 1 is a first cavity for an external sample to enter the device, the external sample refers to graphene metal composite powder loaded on a tray, and the external sample can be manually or automatically placed into the sample chamber 1. The utility model discloses a compound powder continuous growth equipment of graphite alkene metal, sampling chamber, CVD tube furnace and cooling room all have independent air supply system and vacuum unit, have solved the continuous growth problem of compound powder of graphite alkene metal, improve production efficiency, the scale of enlarging production, low energy consumption, the specially adapted adopts the small-size graphite alkene continuous growth as the substrate such as powder.
As shown in figure 1, the utility model discloses a continuous growth equipment of graphite alkene metal composite powder still includes the radio frequency power supply 9 and the radio frequency plasma generator 5 of looks adaptation, radio frequency power supply 9 sets up in switch board 10, radio frequency plasma generator 5 is connected with CVD tubular furnace 2. The radio frequency plasma generator 5 can generate uniform equivalent glow in the CVD tubular furnace 2, accelerate the decomposition of a carbon source and the growth of graphene, effectively reduce the growth temperature of the graphene and reduce the structural damage to a substrate material.
As shown in fig. 1-2, a first vacuum magnetic sample transmission rod 7 is arranged in the sample chamber 1 and the CVD tube furnace 2, so that vacuum transmission of a sample from the sample chamber 1 to the CVD tube furnace 2 can be realized; and second vacuum magnetic sample transmission rods 16 are arranged in the CVD tube furnace 2 and the temperature reduction chamber 3, so that the vacuum transmission of samples from the CVD tube furnace 2 to the temperature reduction chamber 3 can be realized. The vacuum magnetic sample transfer rod is driven by electric power. In an object stage loaded with a powdery sample, such as a quartz boat, a first vacuum magnetic sample transmission rod 7 can be connected with the tail end of the object stage in a buckling manner, and the object stage loaded with the sample is pushed to a CVD tube furnace 2 from a sample inlet chamber 1 under the drive of electric power; the second vacuum magnetic sample transmission rod 16 can be connected with the head end of the objective table in a buckling mode, the objective table is pulled under the driving of electric power, the first vacuum magnetic sample transmission rod 7 is tripped with the tail end of the objective table, and then the objective table is pulled to the cooling chamber 3.
The first vacuum baffle valve 6 has two main functions, when the first vacuum baffle valve 6 is closed, the sample chamber 1 can be kept in a vacuum state or a gas protection state through the independent vacuum unit 11 and the gas supply system 8, when the first vacuum baffle valve 6 is opened, the gas pressure of the sample chamber 1 is equivalent to that of the cavity of the CVD tube furnace 2, and a sample can be introduced into the CVD tube furnace 2 from the sample chamber 1 with the help of the first vacuum magnetic transmission rod 7.
As shown in fig. 1-2, two cooling devices 14 are provided on the outer wall of the CVD tube furnace 2 at both ends of the CVD tube furnace 2, and the two cooling devices 14 are connected to the first vacuum flapper valve 6 and the second vacuum flapper valve 15, respectively. The cooling device 14 can adopt a water-cooling flange or an oil-cooling flange and is externally connected with a circulating system to take away a large amount of heat diffused to the two ends of the CVD tube furnace 2 when the rapid heating device 4 is heated, so that the vacuum baffle valve can work normally. Two heat insulation devices 12 positioned at two ends of the CVD tubular furnace 2 are arranged on the inner wall of the CVD tubular furnace 2, and the heat insulation devices 12 are aligned with the communication ports at two ends of the CVD tubular furnace 2. The heat insulation device 12 reflects the irradiation heat generated by the heating device 4 to the middle part of the CVD tube furnace 2 through the reflecting plate, so that the irradiation heat received by the vacuum gate valves at the two ends of the CVD tube furnace 2 can be effectively reduced. Two ends of the CVD tube furnace 2 are respectively provided with an exhaust port 17 for exhausting protective gas such as inert carrier gas introduced by the gas supply system 8. The exhaust port 17 may be provided with a manual valve or an automatic valve.
As shown in fig. 3, the CVD tube furnace 2 is correspondingly connected to the multi-channel gas supply system 8 through a plurality of temperature-resistant gas inlet pipes 13, and the temperature-resistant gas inlet pipes 13 penetrate through the side wall of the CVD tube furnace 2 and communicate with the inside of the CVD tube furnace 2. The special gas enters different areas of the CVD tubular furnace 2 from different temperature-resistant gas inlet pipelines simultaneously, so that the atmosphere distribution in the cavity is more uniform, and the quality of the graphene metal composite powder is improved. Meanwhile, the temperature-resistant air inlet pipeline 13 is arranged at the middle position of the front surface of the heating device 4, which requires that a channel with the same size is reserved at the corresponding position of the middle of the front surface of the heating device 4. In addition, each temperature-resistant air inlet pipeline 13 is provided with a flow controller at the connection part with the air supply system 8, so as to control the air flow in each pipeline. The plurality of temperature-resistant air inlet pipes 13 are regularly arranged. Specifically, the number of the temperature-resistant air inlet pipes 13 is three, and the three temperature-resistant air inlet pipes 13 are arranged in a straight line. The position of the temperature-resistant air inlet pipeline 13 is influenced by the heating device 4 and is in a high-temperature state during the use of the equipment, so the temperature-resistant air inlet pipeline 13 can be made of quartz or high-temperature alloy.
In addition, heating device 4 installs on the outer wall of CVD tube furnace 2, and heating device 4 is equipped with a plurality of holes of dodging that are used for dodging a plurality of temperature resistant admission lines 13, and temperature resistant admission line 13 runs through heating device 4 through dodging the hole.
The utility model discloses a graphite alkene metal composite powder continuous growth equipment's use divide into two kinds of states:
in the first state: the external graphene metal composite powder enters the equipment through the sampling chamber 1, after the sealing flange is closed, the vacuum unit 11 is opened by the sampling chamber 1 and the CVD tubular furnace 2, so that the sampling chamber 1 and the CVD tubular furnace 2 reach a vacuum state, then the vacuum unit 11 is closed, and the gas supply system 8 is opened to introduce inert carrier gas, hydrogen, carbon source gas and the like required by graphene growth. When the pressure of the sample chamber 1 is equal to the pressure of the CVD tube furnace 2, the first vacuum flapper valve 6 is opened, the sample is transferred from the sample chamber 1 to the CVD tube furnace 2 by the first vacuum magnetic transfer rod 7, and the first vacuum flapper valve 6 is closed.
Setting the temperature and the heating speed required by operation through the heating device 4, setting the gas components and the flow through the gas supply system 8, setting the radio frequency power and the operation time through the radio frequency power supply 9, and starting the production process; starting the heating device 4, introducing gas required for growing graphene when the temperature in the CVD tubular furnace 2 rises to about 650 ℃ of the required growth temperature, starting the radio frequency plasma generator 5, and adjusting the glow area to be optimized; after the growth stage is finished, the vacuum unit 11 connected with the cooling chamber 3 is opened to enable the cooling chamber 3 to reach a vacuum state, then the vacuum unit 11 is closed, and the gas supply system 8 is opened to introduce inert carrier gas and other protective gases. Under the same pressure, the second vacuum flapper valve 15 between the temperature-reducing chamber 3 and the CVD tube furnace 2 is opened, the sample is transferred from the CVD tube furnace 2 to the temperature-reducing chamber 3 by the second vacuum magnetic transfer rod 16, and the second vacuum flapper valve 15 is closed. The sample is cooled in the cooling chamber 3, and after the sample is cooled to room temperature, the flange at the cooling device 14 is opened to take the sample out of the apparatus.
After the graphene metal composite powder is conveyed from the CVD tubular furnace 2 to the temperature reduction chamber 3, a new group of graphene metal composite powder enters the sampling chamber 1 to start to grow for a new round, and thus continuous preparation of the graphene metal composite powder is realized in cycles.
In the second state: the operation and process in the loadlock chamber 1 and the temperature decrease chamber 3 are the same as in the first state, except that the process in the CVD tube furnace 2 is different. The method comprises the following specific steps: after the graphene metal composite powder enters the CVD tubular furnace 2, the temperature and the heating speed required by operation are set through the control system of the heating device 4, the gas components and the flow are set through the control system of the gas supply system 8, the heating device 4 is started, and when the temperature in the CVD tubular furnace 2 rises to about 1000 ℃ of the required growth temperature, the gas required by graphene growth is introduced for graphene growth, so that the radio frequency plasma generator 5 is not required to be started.
It should be noted that the heating device 4, the control cabinet 10, the vacuum unit 11, the gas supply system 8, the radio frequency power supply 9, the vacuum flapper valve, and the vacuum magnetic sample transmission rod of the present invention are realizable by the prior art. Moreover, the starting or the closing of the device can be automatically controlled by arranging a controller, so that the full automation is realized, which can be realized by the prior art.
The foregoing is a more detailed description of the present invention, taken in conjunction with the specific preferred embodiments thereof, and it is not intended that the invention be limited to the specific embodiments shown and described. To the utility model belongs to the technical field of ordinary technical personnel, do not deviate from the utility model discloses under the prerequisite of design, can also make a plurality of simple deductions or replacement, all should regard as belonging to the utility model discloses a protection scope.
Claims (10)
1. The utility model provides a continuous growth equipment of graphite alkene metal composite powder which characterized in that: the device comprises a sample inlet chamber (1), a CVD (chemical vapor deposition) tube furnace (2) and a cooling chamber (3) which are sequentially connected, and further comprises a vacuum unit (11), an air supply system (8) and a heating device (4), wherein the vacuum unit (11) and the air supply system (8) are respectively connected with the sample inlet chamber (1), the CVD tube furnace (2) and the cooling chamber (3), the heating device (4) is connected with the CVD tube furnace (2), a communication port between the CVD tube furnace (2) and the sample inlet chamber (1) is provided with a first vacuum valve baffle (6), and a communication port between the CVD tube furnace (2) and the cooling chamber (3) is provided with a second vacuum baffle (15).
2. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: the plasma tube type CVD furnace further comprises a radio frequency power supply (9) and a radio frequency plasma generator (5) which are matched, wherein the radio frequency plasma generator (5) is connected with the CVD tube type furnace (2).
3. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: the sample feeding chamber (1) and the CVD tubular furnace (2) are internally provided with a first vacuum magnetic sample transmission rod (7) for transmitting samples between the sample feeding chamber and the CVD tubular furnace, and the CVD tubular furnace (2) and the cooling chamber (3) are internally provided with a second vacuum magnetic sample transmission rod (16) for transmitting samples between the sample feeding chamber and the CVD tubular furnace.
4. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: two cooling devices (14) positioned at two ends of the CVD tubular furnace (2) are arranged on the outer wall of the CVD tubular furnace (2), and the two cooling devices (14) are respectively connected with the first vacuum baffle valve (6) and the second vacuum baffle valve (15).
5. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: CVD tubular furnace (2) correspond through a plurality of temperature resistant admission pipes (13) and are connected with multichannel air supply system (8), temperature resistant admission pipe (13) run through the lateral wall of CVD tubular furnace (2) and communicate with the inside of CVD tubular furnace (2).
6. The graphene metal composite powder continuous growth device according to claim 5, characterized in that: heating device (4) are installed on the outer wall of CVD tubular furnace (2), and heating device (4) are equipped with a plurality of holes of dodging that are used for dodging a plurality of temperature resistant admission lines (13).
7. The graphene metal composite powder continuous growth device according to claim 5, characterized in that: each temperature-resistant air inlet pipeline (13) is provided with a flow controller at the joint with the air supply system (8).
8. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: two heat insulation devices (12) which are positioned at two ends of the CVD tubular furnace (2) are arranged on the inner wall of the CVD tubular furnace (2), and the heat insulation devices (12) are aligned with communication ports at two ends of the CVD tubular furnace (2).
9. The graphene metal composite powder continuous growth device according to claim 1, characterized in that: two ends of the CVD tube furnace (2) are respectively provided with an exhaust port (17).
10. The graphene metal composite powder continuous growth device according to claim 5, characterized in that: the temperature-resistant air inlet pipelines (13) are made of quartz or metal, and the temperature-resistant air inlet pipelines (13) are regularly arranged.
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| CN201822232542.8U CN209974884U (en) | 2018-12-28 | 2018-12-28 | Continuous growth equipment for graphene metal composite powder |
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| CN201822232542.8U CN209974884U (en) | 2018-12-28 | 2018-12-28 | Continuous growth equipment for graphene metal composite powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113340897A (en) * | 2021-06-15 | 2021-09-03 | 云南大学 | In-situ photoelectric testing device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113340897A (en) * | 2021-06-15 | 2021-09-03 | 云南大学 | In-situ photoelectric testing device |
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