CN214244667U

CN214244667U - Preparation chamber and large-scale preparation equipment for CVD (chemical vapor deposition) deposited graphene

Info

Publication number: CN214244667U
Application number: CN202120243855.2U
Authority: CN
Inventors: 孙华
Original assignee: Individual
Current assignee: Individual
Priority date: 2021-01-28
Filing date: 2021-01-28
Publication date: 2021-09-21
Anticipated expiration: 2031-01-28

Abstract

The utility model belongs to the technical field of graphite alkene preparation equipment technique and specifically relates to a scale preparation equipment of preparation cavity and CVD deposit graphite alkene is related to. The preparation chamber is a closed chamber and comprises a main chamber and an auxiliary chamber, the outlet end of the main chamber is communicated with the inlet end of the auxiliary chamber, part of the bottom surface of the preparation chamber is downwards sunken to form a liquid airtight pool, and the outlet end of the main chamber and the inlet end of the auxiliary chamber are both positioned below the liquid level of the liquid airtight pool; an elastic airtight component is arranged at the outlet end of the auxiliary chamber. The preparation chamber can be sealed in a first way by the liquid-tight cell and in a second way by the elastic gas-tight component. Carry out the effect of secondary seal through the airtight subassembly of elasticity, prevent when preparation cavity evacuation, because of the first sealed inefficacy that the liquid level of deionized water and etching liquid changes and leads to.

Description

Preparation chamber and large-scale preparation equipment for CVD (chemical vapor deposition) deposited graphene

Technical Field

The utility model belongs to the technical field of graphite alkene preparation equipment technique and specifically relates to a scale preparation equipment of preparation cavity and CVD deposit graphite alkene is related to.

Background

Graphene, namely 'single-layer graphite flake', is a new member in a carbon crystal family, has a unique single-atomic-layer two-dimensional crystal structure, and integrates multiple excellent characteristics. Such as ultrahigh carrier mobility, electrical conductivity, thermal conductivity, light transmittance, high strength, and the like.

The current preparation method of graphene comprises the following steps:

1. the solid phase method is divided into a mechanical stripping method and an epitaxial growth method;

2. the liquid phase method is classified into a redox method, an ultrasonic dispersion method, an organic synthesis method, a solvothermal method, and the like.

3. The gas phase method can be classified into a chemical vapor deposition plasma enhanced method, a flame method, an arc discharge method, and the like.

Through combing all the preparation methods of the graphene and comparing and analyzing the preparation methods of each graphene, the fact that only a chemical vapor deposition method is most suitable for preparing a high-quality graphene product is found, but the chemical vapor deposition method has the following technical problems in the practical preparation of the graphene:

1: carbon source gas such as methane, acetylene and liquid such as ethanol must be prepared in a vacuum oxygen-free environment, otherwise, when the concentration of the carbon source gas reaches 5 to 15 percent, the carbon source gas is mixed with oxygen in the air and then is exploded.

2: the mechanism for generating graphene in a laboratory is relatively fixed, so that the area for preparing graphene is too small, and large-scale and large-batch generation cannot be achieved.

3: the intermittent preparation causes large energy consumption and very high cost for processing and generating the graphene.

SUMMERY OF THE UTILITY MODEL

A first object of the utility model is to provide a preparation cavity, because of preparing the cavity in sealed problem, problem that can not the large-scale production.

The utility model provides a preparation chamber, the preparation chamber is airtight chamber, the preparation chamber includes main chamber and auxiliary chamber, the exit end of main chamber and the entrance point of auxiliary chamber communicate, part of the bottom surface of the preparation chamber is sunken downwards to form a liquid airtight pool, and the exit end of main chamber and the entrance point of auxiliary chamber are both located below the liquid level of liquid airtight pool;

an elastic airtight component is arranged at the outlet end of the auxiliary chamber.

Preferably, the liquid airtight pool comprises an etching tank and a cleaning tank which are sleeved with each other;

the cleaning tank is a structure formed by sinking the bottom surface of the preparation chamber part downwards;

a partition board is arranged in the preparation chamber and divides the preparation chamber into a main chamber and an auxiliary chamber;

one side of the clapboard and the side wall of the cleaning tank form an outlet end of the main chamber, and the other side of the clapboard and the side wall of the cleaning tank form an inlet end of the auxiliary chamber;

the lower end of the baffle is inserted in the etching groove, and the lower end of the baffle is positioned below the liquid level of the etching groove.

Preferably, deionized water is arranged in the cleaning tank;

and the inner surface of the etching groove and the lower end of the partition plate are provided with anticorrosive layers.

Preferably, an ultrasonic generator is arranged in the etching groove.

Preferably, the outlet end of the auxiliary chamber is hermetically connected with the elastic airtight piece;

the elastic airtight piece is provided with a channel for the conveyor belt assembly to pass through, and the conveyor belt assembly is arranged on the conveyor belt assembly;

the elastomeric seal assembly further includes a clamping portion that applies pressure to the elastomeric seal to control the spacing between the channel and the conveyor belt assembly.

Preferably, the elastic air-tight piece comprises a first base plate, a second base plate, a third base plate and a fourth base plate which are arranged in sequence from top to bottom;

conveyor belt component channels are arranged between the second base plate and the third base plate and between the third base plate and the fourth base plate.

Preferably, the clamping part comprises a pull rod and a tow rod bracket;

the second base plate, the third base plate and the fourth base plate are all inserted with a towing rod bracket;

the pull rod is fixed at the outlet end of the auxiliary chamber, a plurality of adjusting assemblies are arranged on the pull rod, and each tow rod support corresponds to one adjusting assembly;

the adjusting component comprises a pair of nuts and a spring arranged between the two nuts, and when the adjusting component is matched with the backing plate, the backing plate is sleeved on the pull rod and clamped between the spring and the nuts.

Preferably, the clamping portion further comprises a fastening bolt, and the first pad is disposed at an outlet end of the sub-chamber through the fastening bolt.

Preferably, the outlet end of the sub-chamber has an embossing structure on the side facing the elastomeric airtight member.

A scale-up preparation apparatus for CVD deposited graphene, comprising the preparation chamber as described above.

The beneficial effects are that:

the preparation chamber can be sealed in a first way by the liquid-tight cell and in a second way by the elastic gas-tight component. Carry out the effect of secondary seal through the airtight subassembly of elasticity, prevent when preparation cavity evacuation, because of the first sealed inefficacy that the liquid level of deionized water and etching liquid changes and leads to.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the technical solutions in the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

Fig. 1 is a schematic diagram of an internal structure of a large-scale CVD graphene deposition apparatus according to an embodiment of the present invention;

fig. 2 is a top view of a large-scale apparatus for CVD deposition of graphene according to an embodiment of the present invention;

FIG. 3 is a schematic structural view of a reaction chamber according to an embodiment of the present invention;

FIG. 4 is a cross-sectional view of a reaction chamber according to an embodiment of the present invention;

FIG. 5 is a schematic view of a reaction chamber and a heating element support according to an embodiment of the present invention;

fig. 6 is a schematic structural diagram of a discharge cord according to an embodiment of the present invention;

fig. 7 is a schematic structural view of a heating element holder according to an embodiment of the present invention;

fig. 8 is a schematic structural view of a liquid sealed tank according to an embodiment of the present invention;

fig. 9 is a schematic structural view of an elastic airtight member according to an embodiment of the present invention;

figure 10 is a cross-sectional view of an elastomeric air seal according to an embodiment of the present invention;

FIG. 11 is a schematic view of a structure of a tie plate and a support bracket of a towing bar according to an embodiment of the present invention;

fig. 12 is a top view of a first shim plate according to an embodiment of the present invention;

fig. 13 is a top view of a second shim plate according to an embodiment of the present invention;

fig. 14 is a side view of a second shim plate according to an embodiment of the present invention;

fig. 15 is a top view of a third shim plate according to an embodiment of the present invention;

fig. 16 is a side view of a third shim plate according to an embodiment of the present invention;

fig. 17 is a top view of a fourth shim plate according to an embodiment of the present invention;

fig. 18 is a side view of a fourth shim plate according to an embodiment of the present invention;

fig. 19 is a schematic structural view of a conveyor belt assembly and a preparation chamber according to an embodiment of the present invention.

Description of reference numerals:

1: preparing a chamber; 2: a reaction chamber; 3: a cooling chamber; 4: a liquid airtight tank; 5: a conveyor belt assembly; 6: a thermal insulation material; 7: a crimping apparatus; 8: an elastomeric air seal;

11: a main chamber; 12: a secondary chamber; 13: a partition plate;

21: a groove structure; 22: discharging the filament; 23: an outer side hanging hole; 24: an inner side hanging hole; 25: a terminal post hole; 26: an air inlet; 27: a heating element support;

221: a top frame; 222: a main boom; 223: a secondary boom; 224: bur;

31: a cold discharge pipe; 32: a liquid nitrogen inlet; 33: a liquid nitrogen outlet;

41: a cleaning tank; 42: etching a groove; 43: an ultrasonic generator; 44: an ultrasonic host;

81: a first backing plate; 82: a second backing plate; 83: a third base plate; 84: a fourth base plate; 85: a conveyor belt assembly channel; 86: a pull rod; 87: a tow bar support; 88: a nut; 89: a spring; 90: and (5) tightening the bolts.

Detailed Description

The technical solution of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise" and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and to simplify the description, but do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", may explicitly or implicitly include one or more of the described features. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise. Furthermore, the terms "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases to those skilled in the art.

As shown in figure 1, the preparation chamber is a closed chamber and comprises a main chamber and a secondary chamber, wherein the outlet end of the main chamber is communicated with the inlet end of the secondary chamber, part of the bottom surface of the preparation chamber is downwards sunken to form a liquid airtight pool, and the outlet end of the main chamber and the inlet end of the secondary chamber are both positioned below the liquid level of the liquid airtight pool.

In this embodiment, a first seal can be formed to the preparation chamber by the de-liquefying airtight cell, and a second seal can be formed to the preparation chamber by the elastic airtight assembly. Carry out the effect of secondary seal through the airtight subassembly of elasticity, prevent when preparation cavity evacuation, because of the first sealed inefficacy that the liquid level of deionized water and etching liquid changes and leads to.

The specific composition structure of the liquid airtight pool 4 and the elastic airtight assembly is as follows:

liquid airtight pool 4

Referring to FIG. 8, the liquid airtight tank 4 includes a cleaning tank 41 and an etching tank 42 which are fitted to each other.

The cleaning tank 41 is a structure formed by partially recessing the bottom surface of the preparation chamber downward.

A partition 13 is provided in the preparation chamber 1, and the partition 13 divides the preparation chamber into a main chamber 11 and a sub-chamber 12.

One side of the partition 13 and the side wall of the wash bowl 41 constitute an outlet end of the main chamber 11, and the other side thereof and the side wall of the wash bowl 41 constitute an inlet end of the sub-chamber 12.

The lower end of the partition plate 13 is inserted into the etching groove 42, and the lower end of the partition plate 13 is positioned below the liquid level of the etching groove 42.

The preparation chamber 1 is divided into a main chamber 11 and a sub-chamber 12 by a partition 13, and the lower end of the partition is inserted into the etching groove 42. When the cleaning tank 41 and the etching tank 42 are filled with liquid, the liquid in the cleaning tank 41 and the etching tank 42 forms a liquid seal structure at the main chamber 11 and the sub-chamber 12. The main chamber 11 and the sub-chamber 12 form relatively independent spaces, and particularly the main chamber 11 can form a closed space, so that a closed space is provided for the production of graphene.

The reason why the liquid seal tank 4 adds the etching tank 42 to the cleaning tank 41 is that:

the conveyor belt assembly 5 is an annular structure, and graphene products are arranged on the upper conveyor belt of the conveyor belt assembly 5 and need to enter the etching groove 42 to be stripped. Graphene products on the lower conveyor belt of the conveyor belt assembly 5 are completely peeled off, and need to enter preparation equipment for producing graphene again, and a cleaning tank 41 is needed for cleaning the conveyor belt before entering graphene production. Therefore, the etching tank 42 and the cleaning tank 41 are required, one for peeling off the graphene and the other for cleaning the conveyor belt.

In particular, the method comprises the following steps of,

an etchant (low concentration acid) is provided in the etching tank 42, deionized water is provided in the cleaning tank 41, and the inner surface of the etching tank 42 and the lower end of the partition 13 are provided with an anticorrosive layer.

The etchant in the etching groove 42 can etch and strip the adhered graphene grown on the substrate of the conveyor belt, so that the graphene can be rolled off the substrate by the subsequent process. The rolling-off of the graphene is realized by a rolling device 7. The preparation equipment of graphite alkene is mainly protected in this application, and the book of graphite alkene is not the key protection content in this application, so, curling equipment 7 does not just describe in detail.

An ultrasonic generator 43 is arranged in the etching groove 42, and the etching agent can vibrate through the ultrasonic generator 43, so that the graphene etching and stripping efficiency is improved. The ultrasonic generator 43 is also connected with an ultrasonic host 44.

Pure deionized water is arranged in the cleaning tank 41, and the deionized water can thoroughly clean the conveying belt assembly, so that impurities are prevented from being adsorbed on the surface of the substrate foil to influence the quality of graphene on the next step.

The etching agent has certain corrosiveness, and the surface of the roller of the conveyor belt assembly, which is positioned in the etching groove, is provided with an anticorrosive layer to prevent the roller from being corroded by the etching agent.

Elastic airtight member 8

Referring to fig. 9 to 18, the outlet end of the sub-chamber 12 is provided with an elastomeric air seal 8 which is sealingly connected to the outlet end of the sub-chamber 12.

The elastomeric seal 8 is provided with a passage in the conveyor belt assembly 5 through which the conveyor belt assembly 5 passes.

The elastomeric seal assembly 8 also includes a clamping portion that applies pressure to the elastomeric seal to control the spacing between the tunnel and the conveyor belt assembly.

The outlet end of the auxiliary chamber 12 is an inlet and an outlet of the conveyor belt assembly 5, the elastic airtight piece 8 is arranged, the conveyor belt can pass through the passage of the elastic airtight piece, the elastic airtight piece is pressurized by the clamping part, the distance between the conveyor belt assembly and the passage can be changed, the side wall of the passage is tightly attached to the conveyor belt assembly, the outlet end of the auxiliary chamber is sealed, the sealing of the preparation chamber is further realized, and the preparation chamber forms a sealed space. The pressure applied by the clamping member against the elastomeric air seal is adjusted while the conveyor belt assembly is in operation. Increasing the spacing between the conveyor belt assembly and the tunnel. The channel is provided with a space for the conveyor belt assembly to run, so that the conveyor belt assembly can run normally.

The elastic air seal 8 includes a first pad 81, a second pad 82, a third pad 83, and a fourth pad 84, which are arranged in this order from top to bottom.

A conveyor belt assembly path 85 is provided between the second pad 82 and the third pad 83, and between the third pad 83 and the fourth pad 84.

The clamping portion includes a pull rod 86 and a tow rod bracket 87.

The second backing plate 82, the third backing plate 83 and the fourth backing plate 84 are all inserted with a towing rod bracket 87.

A pull rod 86 is fixed at the outlet end of the sub-chamber and a plurality of adjustment assemblies are provided on the pull rod 86, one for each tow bar bracket 87.

The adjustment assembly includes a pair of nuts 88 and a spring 89 disposed between the nuts 88. when the adjustment assembly is mated with the backing plate, the backing plate is sleeved over the pull rod and the backing plate is clamped between the spring 89 and the nuts 88.

The position of the adjusting nut relative to the pull rod can be adjusted, the drag rod support can compress the base plates, and therefore the distance between the channels between the base plates is changed.

Furthermore, the two sides of the second pad plate 82, the third pad plate 83 and the fourth pad plate 84 are all provided with a towing rod bracket 87, and the outside-located towing rod bracket 87 is sleeved with a pull rod 86 with an adjusting component. The inner side of the bracket 87 is sleeved on the sliding rod. The slide bar supports and guides the inner side tow bar support, and when the outer side support plate drives the base plate to move, the inner side support plate support also moves synchronously along with the base plate, so that the moving stability of the base plate is improved.

The clamping portion further includes a tightening bolt 90, and the first backing plate 81 is disposed at the outlet end of the sub-chamber 12 by the tightening bolt 90. The threaded connection of the tightening bolt 90 is at the outlet end of the sub-chamber 12, the end of the tightening bolt 90 is connected with the first shim plate 81, and the position of the first shim plate 81 can be adjusted by adjusting the position of the tightening bolt 90 relative to the outlet end of the sub-chamber 12.

The outlet end of the sub-chamber 12 has an embossed structure on the side facing the elastomeric seal 8. Through the arrangement of the embossing structure, the contact area between the elastic airtight piece and the outlet end of the auxiliary chamber 12 can be increased, and the air tightness between the elastic airtight piece and the auxiliary chamber is further improved.

Specifically, the elastic airtight member 8 is made of a rubber material.

As shown in fig. 1 to 19, the present embodiment provides a large-scale production apparatus for CVD-deposited graphene, which includes a production chamber 1, a reaction chamber 2, a cooling chamber 3, a liquid airtight tank 4, and a conveyor belt assembly 5.

The preparation chamber 1 is a closed chamber, the preparation chamber 1 comprises a main chamber 11 and a sub-chamber 12, an outlet end of the main chamber 11 is communicated with an inlet end of the sub-chamber 12, part of the bottom surface of the preparation chamber 1 is downwards sunken to form a liquid airtight pool 4, and the outlet end of the main chamber 11 and the inlet end of the sub-chamber 12 are both located below the liquid level of the liquid airtight pool.

The conveyor assembly 5 is arranged inside the preparation chamber 1, passes through the liquid-tight cell 4 and then extends to the outside of the preparation chamber 1 via the outlet end of the sub-chamber 12.

The reaction chamber 2 and the cooling chamber 3 are arranged in the preparation chamber 1 in sequence along the conveying direction of the conveyor belt assembly 5, and the open ends of the reaction chamber 2 and the cooling chamber 3 are both disposed toward the conveyor belt assembly 5.

In the embodiment, the reaction chamber 2 and the cooling chamber 3 are arranged in the closed preparation chamber 1, and the space in the main chamber is sealed by the liquid airtight pool 4, so that the main chamber 11 is ensured to have good tightness, and the accident that equipment explodes when air enters in the graphene production process is avoided; the conveyer belt subassembly can drive the basement and loop through reaction chamber 2 and cooling chamber 3 in proper order, can realize that the basement is for the continuity output of reaction chamber 2, and then realized the continuity of graphite alkene production, integrality, realized the large-scale production of graphite alkene.

Reaction chamber 2

Referring to fig. 3 to 7, the reaction chamber 2 is a cavity with an opening at the bottom, and the two opposite side plates of the reaction chamber 2 are provided with groove structures 21, and the groove structures 21 are covered on the upper part of the conveyor belt assembly 5.

The reaction chamber 2 can be made to ride on the conveyor assembly 5 by providing a groove structure 21 on the oppositely disposed side plate of the reaction chamber 2. This can reduce the gap between the conveyor assembly 5 and the reaction chamber 2. This reduces the dissipation of heat from the reaction chamber 2.

Further, in the vertical direction, there is a space between the lower end of the reaction chamber 2 (the top surface of the groove structure) and the conveyor belt assembly 5, which is 0.4-0.6mm, in particular, 0.5 mm.

The reaction chamber 2 is made of an insulator, for example, the reaction chamber is made of quartz, ceramic and the like, and the reaction temperature of CVD is about 1000 ℃, so the quartz reaction chamber is most economical and practical, and can have higher temperature rise and drop speed, and the quartz high-temperature reaction chamber can be provided to the reaction zone with the width of 2 meters and the length of 2 meters, even 6 meters and the length of 2 meters; if the ceramic is selected as the high-temperature reaction bin, the wall thickness exceeds 2 cm, the temperature rising and reducing speed is not too fast, and otherwise, the service life of the ceramic reaction bin can be shortened.

There is the heat preservation interval between 2 roof outsides of reacting chamber and the preparation cavity, and the outside parcel of reacting chamber roof and curb plate has insulation material 6. The heat insulating material 6 is made of asbestos fiber, and the heat insulating material 6 can insulate the reaction chamber 2.

The outer side of the top plate of the reaction chamber 2 is hung in the preparation chamber 1 through an insulating structure, the inner side of the top plate of the reaction chamber 2 is hung with a discharge cord 22 through an insulating structure, and the discharge cord 22 is connected with the negative electrode. Specifically, the hoisting structure is an insulating porcelain insulator. The outside of the reaction chamber 2 is provided with an outside hanging hole 23, and the inside of the reaction chamber 2 is provided with an inside hanging hole 24. The outer side hanging hole is connected with the preparation chamber 1 through a hoisting structure, and the inner side hanging hole hoists the discharge wire 22 through the hoisting structure.

In this embodiment, a specific structure of the discharge cord 22 is also provided.

The discharge cord includes a top frame 221, a primary boom 222, a secondary boom 223, and barbs 224.

The corners of the top frame 221 are each provided with a downwardly extending primary hanger bar 222, and a plurality of downwardly extending secondary hanger bars 223 are provided on the sides of the top frame.

A plurality of barbs 224 which are uniformly distributed are arranged on the main suspension rod 222 and the secondary suspension rod 223.

The top of the reaction chamber 2 is provided with a binding post which is connected with the discharge cord 22 and is arranged in a binding post hole 25 at the top of the reaction chamber 2.

The reaction chamber 2 is provided with three gas inlets 26, which are a carbon source gas inlet, an argon gas inlet and a hydrogen gas inlet, respectively.

Carbon source gas or liquid enters the reaction chamber through a carbon source gas inlet. The argon gas inlet is used for introducing argon into the reaction chamber, and the hydrogen gas inlet is used for introducing hydrogen into the reaction chamber.

In addition, the amounts of carbon source gas, argon gas and hydrogen gas need to be accurately controlled, and a flow control meter and an electromagnetic valve are arranged at a carbon source gas inlet, an argon gas inlet and a hydrogen gas inlet.

Different parameters can be set for the reaction of different carbon source gases to the reaction gas flow control system through the setting of the flow control meter, so that the automatic processing and preparation of the graphene are realized, and different customer requirements are met.

The reaction chamber further comprises an exhaust pipe, the exhaust pipe is provided with a pressure release valve and is connected with the tail gas combustion device, and the exhaust pipe leads the tail gas exhausted from the reaction chamber into the combustion device to be combusted so as to treat the tail gas.

A thermocouple is arranged in the reaction chamber. The highest temperature in the reaction chamber needs to be controlled at 1000 ℃, and the temperature in the reaction chamber can be monitored by arranging the thermocouple.

The lower part of the reaction chamber 2 is provided with a heating element holder 27, and the heating element holder 27 is provided with a heating element, and the heating element holder 27 and the heating element extend to the opening of the reaction chamber 2 in the vertical direction.

The upper and lower conveyor belts of the conveyor belt assembly 5 are located on the upper and lower sides of the heating element, respectively.

The heating element was a kannel (Kanthal) heater and the control of the heating element was an europey (Eurotherm) controller. The temperature of the heating element can be controlled by the controller, and the situation that the temperature is too high or too low is avoided.

The cavity of the preparation chamber 1 is communicated with a vacuum pump, and before the high-temperature reaction chamber works, the high-temperature reaction chamber must be firstly vacuumized and then put into inert atmosphere for a plurality of times of repetition for removing air or oxygen. In order to achieve higher vacuum degree (0.00001mbar), a molecular pump is required to be arranged in the CVD reaction chamber, and air (or oxygen) in the reaction chamber body is completely removed. The vacuum of the vacuum pump was 0.00001 mbar.

Cooling chamber 3

Referring to fig. 1, the cooling chamber 3 includes a cavity with an opening at the bottom, and a groove structure is provided on two opposite side plates of the cooling chamber, and the groove structure of the cooling chamber is covered on the upper part of the conveyor belt assembly 5.

The cooling chamber 3 has a structure similar to that of the reaction chamber, and can ride on the conveyor belt assembly by providing a groove structure on both side plates of the cooling chamber 3. There is a spacing of 0.4-0.6mm, in particular 0.5mm, between the lower end of the cooling chamber (the top surface of the groove structure) and the conveyor belt assembly 5. By the cooling chamber 3 riding on the conveyor belt assembly, the gap between the cooling chamber 3 and the conveyor belt assembly 5 can be reduced.

A cold discharge pipe 31 is arranged in the cooling chamber 3, a liquid nitrogen inlet 32 and a liquid nitrogen outlet 33 of the cold discharge pipe 31 extend to the outer side of the preparation chamber 1, and the cold discharge pipe 31 is arranged at the upper part of the conveyor belt assembly 5.

Specifically, the distance between the cold row pipe 31 and the conveyor belt is 20 cm. Liquid nitrogen is conveyed into the cold exhaust pipe 31, and the graphene on the substrate can be cooled through the heat absorption of the liquid nitrogen through gasification.

Heat insulation cotton is arranged between the reaction chamber 2 and the cooling chamber 3 to prevent the reaction chamber 2 and the cooling chamber 3 from being influenced mutually.

A flow control system is provided at the liquid nitrogen inlet 32 to regulate the amount of liquid nitrogen entering the cold leg.

Conveyor belt assembly 5

Referring to fig. 19, the conveyor belt assembly includes a drum, and a conveyor belt wound on the drum, an upper surface of the conveyor belt being provided with a substrate, and the substrate being connected to the anode.

The substrate on the conveyor belt is copper foil, nickel foil and the like, preferably, the copper foil is used as the substrate, and the copper foil substrate needs to be calcined at high temperature by hydrogen and argon to increase the copper quality.

The rollers on the conveyor belt comprise a main roller and an auxiliary roller, and the main roller is rotated under the power of a motor. The linear speeds of the main drum and the supplementary drum are identical and the speeds are manually adjustable. In addition, it should be noted that the rollers located in the etching grooves are made of anticorrosive plastic, the rollers are made of stainless steel, and the surface of the roller must be subjected to external grinding.

It should be noted that, one embodiment of the conveyor belt assembly is: most of the entire loop structure of the conveyor belt is located within the preparation chamber, with only one end of the loop structure extending outside the preparation chamber.

In another embodiment, the conveyor belt may be a belt-like structure, for example, after the substrate in the conveyor belt is prepared with graphene, a new conveyor belt is replaced. After the conveyor belt with the graphene strips the graphene, the conveyor belt is wound into a roll for standby.

In order to further explain the CVD deposited graphene scale preparation equipment, the embodiment also provides a preparation method of the scale preparation equipment.

After the preparation equipment is assembled and debugged, deionized water and low-concentration acid (etching solution) special for etching are respectively injected into the cleaning tank and the etching tank to reach the specified depth.

And a closed space is formed in the preparation chamber by adjusting the clamping part of the elastic airtight component.

It should be noted that: the preparation chamber can be sealed for the first time through deionized water and etching liquid, and the preparation chamber can be sealed for the second time through the elastic airtight assembly. Carry out the effect of secondary seal through the airtight subassembly of elasticity, prevent when preparation cavity evacuation, because of the first sealed inefficacy that the liquid level of deionized water and etching liquid changes and leads to.

After the elastic airtight assembly seals the outlet end of the auxiliary chamber, vacuumizing the preparation chamber at room temperature, introducing argon, and repeating for 4-7 times for removing oxygen or air in the preparation chamber. And after the operation of vacuumizing and argon introducing is circulated for a plurality of times, the vacuum pump is closed, argon is refilled, the preparation chamber is consistent with the atmospheric pressure, the rubber sealing pressing plate is loosened, and air is blocked from entering the main chamber by using the deionized water of the cleaning tank and the low-concentration acid liquor of the etching tank.

And starting the electric roller to drive the conveying belt to drive the substrate to move, opening liquid nitrogen to refrigerate the refrigerating bin, starting the electric heater to heat the high-temperature reaction chamber, introducing a proper amount of hydrogen gas when the temperature is 1000 ℃, then slowly opening reaction gas methane or acetylene to carry out CVD reaction, observing the forming condition of graphene on the conveying belt substrate through the display screen, gradually increasing the supply amount of carbon source gas until the graphene is well formed, and then carrying out large-scale stable production. The conveyer belt slowly conveys the base reaction zone into the cooling chamber, the base on the conveyer belt of the cooling chamber is rapidly cooled by 300 degrees at 1000 degrees, and the conveyer belt drives the base to be naturally cooled after the cooling of the cooling chamber is finished. And (3) slowly conveying the cooled substrate (such as copper) into an etching solution pool to perform chemical etching reaction, and stripping the graphene from the substrate to prepare for post-process composite coiling. Because the reaction gas safety device is arranged, the reaction gas can not be introduced into the high-temperature reaction bin when the temperature is lower than 950 ℃, thereby ensuring the safety.

The reaction gas safety device is very important if methane and acetylene are used as carbon sources, so that the two gases can be used correctly and safely. The main hazards of the hazardous gas are suffocation, poisoning and explosion, and when methane and acetylene are used, the problem of explosion of combustible gas is mainly considered. Theoretically, the combustible gas must satisfy the following three conditions simultaneously to "explode":

3.1 the combustible atmosphere is present together with air (or oxygen)

3.2 the volume of the combustible gas and air (or oxygen) mixed with each other reaches a certain ratio (explosion limit) at a temperature lower than the ignition temperature

The gas mixture above 3.3 is under the action of an ignition source with enough temperature or energy.

Therefore, the flammable gas CO + H2+ CH4(Max. < 1%) > 5% is susceptible to explosion, and thus accurate gas flow control is required.

In view of the above, the reaction gas safety device may be a flow meter, a gas detection sensor, and a temperature sensor. Therefore, parameters such as the amount, the components, the reaction temperature and the like of the reaction gas in the preparation chamber can be monitored.

The preparation chamber is provided with a vacuum pump and a vacuum gauge, and the whole preparation chamber can be monitored whether to have a leakage phenomenon or not due to the installation of the vacuum pump and the vacuum gauge. Once an accident happens, the safety gas tank is flushed with argon and nitrogen immediately. In the aspect of tail gas treatment, an industrial-grade high-end combustion device is adopted, and redundant reaction gas can be combusted, so that the reaction gas is not directly discharged into the atmosphere, and potential danger is avoided. Therefore, the scheme is necessary to configure equipment for preparing graphene by CVD from the aspects of performance and use safety of the reaction bin.

Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention.

Claims

1. A preparation chamber is characterized by being a closed chamber and comprising a main chamber and a secondary chamber, wherein the outlet end of the main chamber is communicated with the inlet end of the secondary chamber, part of the bottom surface of the preparation chamber is sunken downwards to form a liquid airtight pool, and the outlet end of the main chamber and the inlet end of the secondary chamber are both positioned below the liquid level of the liquid airtight pool;

2. The preparation chamber of claim 1, wherein the liquid-tight cell comprises an etching tank and a cleaning tank nested together;

3. The preparation chamber of claim 2, wherein an etchant is disposed in the etching tank, and deionized water is disposed in the cleaning tank;

4. The preparation chamber of claim 2, wherein an ultrasonic generator is disposed within the etch trench.

5. The preparation chamber according to claim 1, wherein the outlet end of the secondary chamber is closed with an elastomeric seal;

6. The preparation chamber according to claim 5, wherein the elastic air seal comprises a first pad, a second pad, a third pad and a fourth pad arranged in sequence from top to bottom;

7. The preparation chamber of claim 6, wherein the clamping portion comprises a draw bar and a tow bar support;

8. The preparation chamber of claim 7, wherein the clamping portion further comprises a tightening bolt, and the first shim plate is disposed at an outlet end of the sub-chamber by the tightening bolt.

9. The preparation chamber according to claim 1, wherein the outlet end of the sub-chamber has an embossed structure on the side facing the elastomeric seal.

10. An apparatus for scale-up preparation of CVD deposited graphene, comprising the preparation chamber according to any one of claims 1-9.