CN209890731U - Chemical vapor deposition device for preparing two-dimensional thin film material - Google Patents
Chemical vapor deposition device for preparing two-dimensional thin film material Download PDFInfo
- Publication number
- CN209890731U CN209890731U CN201920315136.XU CN201920315136U CN209890731U CN 209890731 U CN209890731 U CN 209890731U CN 201920315136 U CN201920315136 U CN 201920315136U CN 209890731 U CN209890731 U CN 209890731U
- Authority
- CN
- China
- Prior art keywords
- main cavity
- vapor deposition
- chemical vapor
- preparing
- thin film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The utility model relates to a chemical vapor deposition device for preparing two-dimensional film materials. It includes: a gas source; the reaction cavity is provided with an air inlet and an object placing opening, and the object placing opening is provided with an opening and closing door; the reaction cavity is positioned in the main cavity; the interior of the main cavity body is provided with a heating device, the surface of the main cavity body is provided with an air inlet, and the air inlet is connected with an air inlet through an air pipe; the temperature measuring device comprises a temperature sensor and a temperature display device; the vacuumizing system is connected with the main cavity body; the vacuum measuring device is connected with the main cavity and comprises a measuring head inserted into the main cavity; further comprising: and the plasma enhancement device is arranged between the air source and the main cavity, the air source is connected with the activity enhancement inlet through a pipeline, and the activity enhancement outlet is connected with the air inlet through a flange. The utility model discloses a set up plasma reinforcing means to reaction gas plasmatization, increase reaction gas's activity for reaction gas reaction's temperature reduces, and reaction period is short, saves the cost.
Description
Technical Field
The utility model relates to a vapor deposition device technical field especially relates to a chemical vapor deposition device of preparation two-dimentional thin film material.
Background
Graphene is a thin film of monoatomic layers with carbon atoms arranged in a hexagonal structure. In the preparation of graphene, chemical preparation methods, especially chemical vapor deposition methods, are mostly adopted at present, and the most common methods are as follows: the graphene film is prepared by performing chemical vapor deposition by using gases such as methane or ethylene through catalytic cracking of a copper substrate. In the method, hydrocarbon gas is catalytically cracked into carbon atoms, hydrogen atoms and hydrocarbon active groups by a copper substrate at high temperature (> 1000 ℃), the hydrocarbon gas freely moves on the surface of the metal substrate and is self-assembled into graphene with a hexagonal structure, and the graphene film is obtained after the graphene film is self-assembled with time.
At present, most of traditional Chemical Vapor Deposition (CVD) methods for preparing graphene are quartz tube furnaces, namely thermal chemical vapor deposition (thermal CVD) methods, but thermal CVD methods generally have the problems of small size, temperature delay and short service life of quartz tubes of prepared thin film materials. In the prior art, a cold wall CVD device has been developed from thermal CVD, and for example, a device for preparing graphene thin film by using cold wall CVD with stainless steel wall is disclosed in the document with patent application No. 201610096667.5, which describes a solution to the problems of small size of thin film material, temperature delay and short life of quartz tube in thermal CVD. However, in using the device described in the literature, it was found that there are several places to be improved: the high-temperature condition (> 1000 ℃) of the cracking of hydrocarbon gas determines that the heating and cooling period of the graphene film prepared by the existing large-scale CVD is longer (> 30 h), and meanwhile, a matched vacuum pump and circulating water need to be operated all the time, so that the power consumption is increased, and the manufacturing cost is high.
Disclosure of Invention
An object of the utility model is to solve not enough among the prior art, provide a vapor deposition device that preparation cycle is short, save the cost.
A chemical vapor deposition apparatus for preparing a two-dimensional thin film material, comprising:
the gas source is used for providing hydrocarbon gas;
the reaction cavity is provided with an air inlet and an object placing opening, and the object placing opening is provided with an opening and closing door;
the reaction cavity is positioned in the main cavity; a heating device for heating the reaction cavity is arranged in the main cavity, and an air inlet is arranged on the surface of the main cavity and is connected with the air inlet through an air pipe;
the temperature measuring device comprises a temperature sensor arranged inside or on the surface of the reaction cavity and a temperature display device for displaying temperature;
the vacuumizing system is connected with the main cavity body and is used for reducing the air pressure in the main cavity body;
the vacuum measuring device is connected with the main cavity and comprises a measuring head inserted into the main cavity;
further comprising: the plasma enhancement device is arranged between the gas source and the main cavity and is provided with an activity enhancement inlet and an activity enhancement outlet, the gas source is connected with the activity enhancement inlet through a pipeline, and the activity enhancement outlet is connected with the gas inlet through a flange; the gas enters the reaction cavity in the main cavity through the plasma enhancement device.
Further, the pipeline is connected with a gas flow control valve for controlling the gas flow.
Preferably, the air pipe is also connected with a switch valve. The switch valve directly controls whether the air source is ventilated or not.
Further, a sample holder for placing a substrate is arranged in the reaction cavity.
Further, the temperature display means comprises a temperature meter or a display.
Further, the plasma enhancement device comprises a radio frequency power supply device, a microwave device, a glow discharge device, an electron cyclotron resonance device or an inductive coupling device plasma source.
Further, a valve is arranged between the main cavity and the vacuum-pumping system.
Further, the vacuum pumping system comprises a mechanical pump and a molecular pump.
The utility model discloses the beneficial effect who gains does: the utility model discloses a set up plasma reinforcing means to reaction gas plasmatization, increase reaction gas's activity for the required temperature of reaction gas reaction reduces, and the cycle of preparation film is short, saves the cost.
Drawings
Fig. 1 is a schematic diagram of a structural principle of the present embodiment.
FIG. 2: is a schematic diagram of the air inlet mode of the existing large-scale CVD in the utility model.
Reference numerals:
1-vacuum pumping system; 2-a valve; 3-a heating device; 4-opening and closing the door; 5-vacuum measuring device; 6-temperature measuring device; 7-main cavity; 8-sample holder; 9-reaction chamber; 10-trachea; 11-flange; 12-plasma-enhanced device; 13-on-off valve; 14-a flow control valve; 15-gas source; 16-the conduit.
Detailed Description
Example (b): see fig. 1. A chemical vapor deposition apparatus for preparing a two-dimensional thin film material, comprising:
a gas source 15 for providing hydrocarbon gas;
the reaction cavity 9 is provided with an air inlet and an object placing opening, and the object placing opening is provided with an opening and closing door 4;
the main cavity 7, the reaction cavity 9 is positioned in the main cavity 7; the interior of the main cavity 7 is provided with a heating device 3 for heating the reaction cavity 9, the surface of the main cavity is provided with an air inlet, and the air inlet is connected with an air inlet through an air pipe 10;
the temperature measuring device 6 comprises a temperature sensor arranged inside or on the surface of the reaction cavity 9 and a temperature display device for displaying temperature; can be a thermocouple, etc.;
the vacuum pumping system 1 is connected with the main cavity 7 and is used for reducing the air pressure in the main cavity 7;
a vacuum measuring device 5, connected to the main cavity 7, comprising a measuring head inserted in the main cavity 7; may be a vacuum gauge.
Further comprising: the plasma enhancement device 12 is arranged between the gas source 15 and the main cavity 7, the plasma enhancement device 12 is provided with an activity enhancement inlet and an activity enhancement outlet, the gas source 15 is connected with the activity enhancement inlet through a pipeline 16, and the activity enhancement outlet is connected with the gas inlet through a flange 11; the gas enters the reaction chamber 9 in the main chamber 7 through the plasma-enhanced device 12.
According to the technical scheme, the hydrocarbon gas is heated and enters the plasma enhancement device, the activity of the hydrocarbon gas is increased, and then the hydrocarbon gas enters the reaction cavity 9 to be heated, and the reaction gas starts to be cracked into carbon atoms, hydrogen atoms and hydrocarbon active groups at a relatively low temperature, such as about 700 ℃ due to the increased activity of the reaction gas, the carbon atoms, the hydrogen atoms and the hydrocarbon active groups freely move on the surface of the metal substrate and are self-assembled into graphene with a hexagonal structure, and the graphene film is obtained as the time is prolonged. Referring to fig. 2, gas enters a plasma enhancement device area a from a gas source through a gas guide tube, the plasmatized gas enters a large CVD cavity B and directly enters a heating cavity C through a pipeline, and the reaction gas is pumped out from the other end of the heating cavity C by a vacuum pump after the reaction.
The preparation method comprises the following steps:
s1, taking copper foil with proper size, and cleaning and pretreating the copper foil;
s2, placing the copper foil in the reaction cavity 9;
s3, the vacuum-pumping system 1 is opened until the vacuum pressure is reduced to 1 x 10-5mbar below;
s4, opening the gas source 15, introducing ethylene gas, and performing gas washing for 20 min;
s5, the air source 15 is closed, and the vacuum pressure is reduced to 1X 10 again-5 Below mbar, the heating device 3 is switched on and the sample is heated to 650 ℃;
s6, opening the plasma enhancement device 12 and the gas source 15 to make the ethylene gas become plasma and grow graphene;
and S7, turning off heating, turning off ethylene, cooling to room temperature (about 12 hours), and taking out to obtain the graphene film.
The technical scheme has the advantages of low reaction temperature, short period and cost saving. The vacuum pumping system 1 and the heating device 3 in the technical scheme can be both the prior art.
Further, a gas flow control valve 14 for controlling the flow of gas is connected to the pipe 16.
When the hydrocarbon gas passes through the plasma enhancement device 12 and reacts in the reaction cavity 9, the flow rate of the hydrocarbon gas needs to be matched with the power of the plasma enhancement device 12, the heating power and other factors; the provision of the gas flow control valve 14 facilitates control of the flow rate of the hydrocarbon gas.
Preferably, the air tube 10 is further connected with a switching valve 13. The switch valve 13 directly controls whether the air source 15 is ventilated or not.
Further, a sample holder 8 for placing a substrate is arranged in the reaction chamber 9.
The substrate is generally made of copper foil or the like, and a sample holder 8 is provided in the reaction chamber 9 for the convenience of placing or fixing the copper foil.
Further, the temperature display means comprises a temperature meter or a display.
When the temperature display device is used in a laboratory, more common instruments are used, so that the temperature display device generally adopts temperature instruments, and is convenient to install and fix.
Further, the plasma enhancement device 12 includes a radio frequency power supply device, a microwave device, a glow discharge device, an electron cyclotron resonance device, or an inductive coupling device plasma source.
The plasma enhancement device 12 in the technical scheme mainly adopts a radio frequency power supply device for turning gas into plasma and increasing activity.
Further, a valve 2 is arranged between the main cavity 7 and the vacuum pumping system 1.
This valve 2 is used for controlling being connected between the main cavity body 7 and the vacuum pumping system 1, before vacuum pumping system 1 closes, needs in time to close this valve 2, avoids vacuum pumping system 1 to close the back, and the air current backward flow influences the inside vacuum of the main cavity body 7.
Further, the vacuum pumping system 1 includes a mechanical pump and a molecular pump.
The mechanical pump is used as a backing pump, and is started when working, the air pressure in the main cavity 7 is reduced to about 1mbar, and then the molecular pump works. The backing pump may also be a roots pump.
The utility model discloses the effect that gains:
1. the plasma enhancement device is added on the existing equipment to realize the purposes of reducing the preparation temperature from 1000 ℃ to 600-800 ℃, and reducing the power consumption of the equipment because the higher the temperature is, the more time is consumed for heating and maintaining the temperature at the high temperature, so that the heating and cooling period can be further shortened (< 20 h);
2. an internal gas path pipeline between the plasma device and the heating cavity is designed, so that gas is directly communicated into the reaction cavity, the gas utilization rate is improved, and the cost is saved;
3. the two ends of the opening and closing cover of the heating cavity are improved, the two ends are not sealed, the opening end of the object placing port is provided with the air outlet, the other end of the object placing port is sealed, the original gas is improved into one end in and one end out, the gas utilization rate is improved, and the cost is saved.
It is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A chemical vapor deposition apparatus for preparing a two-dimensional thin film material, comprising:
the gas source is used for providing hydrocarbon gas;
the reaction cavity is provided with an air inlet and an object placing opening, and the object placing opening is provided with an opening and closing door;
the reaction cavity is positioned in the main cavity; a heating device for heating the reaction cavity is arranged in the main cavity, and an air inlet is arranged on the surface of the main cavity and is connected with the air inlet through an air pipe;
the temperature measuring device comprises a temperature sensor arranged inside or on the surface of the reaction cavity and a temperature display device for displaying temperature;
the vacuumizing system is connected with the main cavity body and is used for reducing the air pressure in the main cavity body;
the vacuum measuring device is connected with the main cavity and comprises a measuring head inserted into the main cavity;
the method is characterized in that: further comprising: the plasma enhancement device is arranged between the gas source and the main cavity and is provided with an activity enhancement inlet and an activity enhancement outlet, the gas source is connected with the activity enhancement inlet through a pipeline, and the activity enhancement outlet is connected with the gas inlet through a flange; the gas enters the reaction cavity in the main cavity through the plasma enhancement device.
2. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: the pipeline is connected with a gas flow control valve for controlling the gas flow.
3. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: the air pipe is also connected with a switch valve.
4. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: and a sample rack for placing a substrate is arranged in the reaction cavity.
5. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: the temperature display means comprises a temperature meter or display.
6. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: the plasma enhancement device comprises a radio frequency power supply device, a microwave device, a glow discharge device, an electron cyclotron resonance device or an inductive coupling device plasma source.
7. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: a valve is arranged between the main cavity and the vacuum pumping system.
8. The chemical vapor deposition apparatus for preparing two-dimensional thin film material according to claim 1, wherein: the vacuum pumping system comprises a mechanical pump and a molecular pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920315136.XU CN209890731U (en) | 2019-03-13 | 2019-03-13 | Chemical vapor deposition device for preparing two-dimensional thin film material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920315136.XU CN209890731U (en) | 2019-03-13 | 2019-03-13 | Chemical vapor deposition device for preparing two-dimensional thin film material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209890731U true CN209890731U (en) | 2020-01-03 |
Family
ID=68997307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920315136.XU Active CN209890731U (en) | 2019-03-13 | 2019-03-13 | Chemical vapor deposition device for preparing two-dimensional thin film material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN209890731U (en) |
-
2019
- 2019-03-13 CN CN201920315136.XU patent/CN209890731U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102849733B (en) | Low-temperature direct preparation method of graphene under double-temperature-zone control, and double-temperature-zone tube furnace | |
| CN100500934C (en) | Method and device for plating diamond like film on inner-outer wall of quartz round tube | |
| CN103569998B (en) | Carbon nanotube preparing apparatus and method | |
| CN102534569A (en) | Atmospheric pressure glow plasma enhanced atom layer deposition device | |
| CN105752968A (en) | Reel-to-reel continuous graphene film growth equipment | |
| CN109112492B (en) | Device suitable for coating film on inner surface of multiple narrow thin pipelines | |
| CN105734524B (en) | Metallo-Organic Chemical Vapor precipitation equipment and the method for using the device | |
| CN209890731U (en) | Chemical vapor deposition device for preparing two-dimensional thin film material | |
| KR20100037071A (en) | Heating element cvd apparatus | |
| CN107099782A (en) | A kind of chemical vapor deposition unit for preparing the thin-film materials such as graphene, hexagonal boron nitride | |
| CN105439126A (en) | Simple preparation method of millimeter level monocrystalline graphene | |
| CN204874732U (en) | Cool off volume to volume plasma reinforcing CVD stove of growing in succession fast | |
| CN106555175A (en) | A kind of high-density plasma reinforced chemical vapor deposition apparatus | |
| CN217438292U (en) | LPCVD furnace structure | |
| CN211689227U (en) | Graphene deposition equipment | |
| CN209974884U (en) | Continuous growth equipment for graphene metal composite powder | |
| CN110408911B (en) | Controllable preparation device and method for large-area thin film | |
| CN203639552U (en) | Microwave excited plasma enhanced chemical vapor deposition device | |
| CN103628047A (en) | Device for preparing SiNx dielectric film by chemical vapor deposition | |
| CN204752846U (en) | Growth carbon nanotube's plasma vapour deposition system | |
| RU2704691C1 (en) | Chemical vapor deposition system for graphene growth | |
| CN106517163A (en) | Cold wall furnace for preparation of graphene through CVD method and continuous production method | |
| CN107021480B (en) | A kind of reactor preparing diamond for deposition | |
| CN208776835U (en) | A kind of industrialization chemical vapor deposition unit | |
| CN204898064U (en) | Gaseous extrinsic cycle type heater CVD diamond film growing device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |