A multi-gas source plasma enhanced CVD system

Abstract

The invention discloses a multi-gas source plasma enhanced CVD system, comprising a furnace tube, a three-temperature zone heating furnace, a radio frequency coil, a first air inlet, a first scroll, a feed bin, a transmission motor, a second air inlet, an air outlet, a butterfly valve, a second scroll, a discharge bin, a molecular pump, a mechanical pump, a fan, a baffle valve, a radio frequency power supply, a flow cabinet, a touch screen control panel, a composite vacuum gauge and a butterfly valve controller; the invention adopts a furnace tube with an ultra-large diameter, and can use a larger area of ​​copper foil on the original basis to obtain a larger area of ​​graphene film, and adds independent low vacuum and high vacuum systems, and quickly enables the ultra-large diameter furnace tube to reach the required vacuum degree through high vacuum, and at the same time, the baffle valve can be used without stopping the molecular pump. The furnace tube with the ultra-large diameter can be freely switched between low vacuum and high vacuum, and the working pressure therein can be accurately controlled, so that the chemical reaction in the furnace tube with the ultra-large diameter can be kept uniform and uniform.

Description

Technical Field

[0001] The invention relates to the technical field of plasma-enhanced roll-to-roll graphene film continuous growth equipment, in particular to a multi-gas source plasma-enhanced CVD system. Background Art

[0002] The existing roll-to-roll continuous growth of graphene film mainly adopts horizontal roll-to-roll equipment. The substrate copper foil is horizontally connected to the unwinding shaft and the winding shaft. The winding force is used to ensure that the copper foil is in a horizontal tension state. However, the copper foil is easy to soften and adhere to the quartz support at high temperature, which affects the effective contact of the reaction gas. The copper foil can only grow the graphene film by single-sided nucleation diffusion; the carbon atoms after the carbon source gas is cracked by the radio frequency power supply enter the heating zone, and the plasma excited by the radio frequency power supply fills the entire heating zone. The overly strong plasma bombards the copper foil to produce serious defects and voids; the exhaust port is located at the bottom of the winding cabin, and the carrier gas, protective gas, carbon atoms and uncracked carbon source gas will be discharged to the closed space through the winding cabin after film formation, so that the film deposited and grown in the heating furnace will be disturbed by the mixed gas;

[0003] In order to solve the above defects, a technical solution is now provided. Summary of the invention

[0004] The purpose of the present invention is to provide a multi-gas source plasma enhanced CVD system. The present invention adopts a furnace tube with an ultra-large diameter. On the original basis, a copper foil with a larger area can be used to obtain a graphene film with a larger area. Independent low vacuum and high vacuum systems are added, and the ultra-large diameter furnace tube is quickly made to reach a required vacuum degree through high vacuum. At the same time, the ultra-large diameter furnace tube can be freely switched between low vacuum and high vacuum through a baffle valve without stopping a molecular pump. A butterfly valve controller can accurately control the working pressure therein, so that the chemical reaction in the ultra-large diameter furnace tube can be kept uniform and uniform.

[0005] The technical problems to be solved by the present invention are as follows:

[0006] How to solve the problems in an effective way that copper foil easily softens and sticks to the wall of the quartz tube at high temperature, and can only grow graphene film by single-sided nucleation and diffusion; and the problem that the RF power source excites too strong plasma to bombard the copper foil and produce serious defects and voids; and the mixed gas discharged after the winding cabin easily causes the thin film on the copper foil in the winding cabin to be disturbed by impurities.

[0007] The purpose of the present invention can be achieved through the following technical solutions:

[0008] A multi-gas source plasma enhanced CVD system, comprising a furnace tube, a three-zone heating furnace, a radio frequency coil, a first air inlet, a first scroll, a feed bin, a transmission motor, a second air inlet, an air outlet, a butterfly valve, a second scroll, a discharge bin, a molecular pump, a mechanical pump, a fan, a baffle valve, a radio frequency power supply, a flow cabinet, a touch screen control panel, a compound vacuum gauge and a butterfly valve controller, wherein a three-zone heating furnace is fixed at the top center of the flow cabinet by bolts, a furnace tube is arranged inside the three-zone heating furnace, two fans are correspondingly installed on the top of the flow cabinet, and a touch screen control panel is embedded on one side of the fan;

[0009] A feed bin and a discharge bin are fixed to the top of the flow cabinet by bolts, and the feed bin and the discharge bin are located at the sides of adjacent fans, respectively; a first reel is movably connected to the inside of the feed bin by a bearing, and a second reel is movably connected to the inside of the discharge bin by a bearing; a transmission motor is fixed to one side of the feed bin by bolts, and the transmission motor is connected to the first reel via a coupling;

[0010] The outer side of the furnace tube is provided with a first air inlet and a second air inlet, and the outer edges of the first air inlet and the second air inlet are both sleeved with radio frequency coils, the outer side of the furnace tube is movably connected with a molecular pump through a flange, a mechanical pump is fixed to the top of the flow cabinet by bolts, and the mechanical pump is located on the side of the molecular pump, a vacuum pipeline is provided between the mechanical pump and the furnace tube, a butterfly valve is installed on the outer side of the vacuum pipeline, and an air outlet is provided on the vacuum pipeline between the furnace tube and the butterfly valve, and a baffle valve is installed on one side of the molecular pump;

[0011] The sides of the flow cabinet are respectively embedded with a radio frequency power supply, a compound vacuum gauge and a butterfly valve controller, and the butterfly valve controller is electrically connected to the butterfly valve, and the compound vacuum gauge is connected to the furnace pipe through a sealed pipe, and the touch screen control panel is electrically connected to the fan, and the radio frequency power supply is electrically connected to the radio frequency coil, and the transmission motor, molecular pump, mechanical pump and baffle valve are all electrically connected to the external power supply;

[0012] Among them, the furnace tube is used to provide a sealed chamber, and its size is 520mm in diameter * 2200mm in length, the three-zone heating furnace is used to provide a heating heat source, and the sizes of its three temperature zones are 250mm * 400mm * 250mm respectively, the radio frequency coil is used to ionize the gas, the first air inlet and the second air inlet are used for the entrance of the gas source, the first scroll and the second scroll are used to place samples and transmission components, the feed bin and the discharge bin are used to provide an operable closed chamber, the transmission motor is used to provide a transmission drive source, the air outlet is used for the outlet of the gas source, the butterfly valve and the baffle valve are used to open and close the vacuum pipe, the molecular pump is used to finely pump the chamber vacuum, that is, high vacuum, the mechanical pump is used to roughly pump the chamber vacuum, that is, low vacuum, the fan is used to enhance air cooling, the radio frequency power supply is used to control the output size of the radio frequency coil, the flow cabinet is used to place components, the touch screen control panel is used to control fan parameters, the compound vacuum gauge is used to detect the vacuum state, and the butterfly valve controller is used to cooperate with the butterfly valve to open and close the vacuum pipe.

[0013] Furthermore, the first air inlet and the second air inlet are both located near the discharge bin, and the air outlet is located near the feed bin.

[0014] Furthermore, the fan is fixed to the flow cabinet by bolts, and the two fans are respectively located on two sides of the three-temperature zone heating furnace.

[0015] Beneficial effects of the present invention:

[0016] The present invention adopts scroll linkage and PE excitation plasma to continuously and quickly prepare large-area and high-quality graphene films, that is, the carbon source gas containing the film component atoms is ionized by radio frequency power supply, and plasma is formed locally to produce a glow phenomenon. The plasma has strong chemical activity and is easy to react, so that the desired graphene film is deposited on the substrate.

[0017] In addition, the copper foil of the substrate vertically penetrates the first reel and the second reel in the ultra-large diameter furnace tube under high vacuum, and uses its own weight to ensure that the copper foil is in a vertically taut state, that is, in the absence of a quartz carrier, the contact area between the gas and the copper foil is increased, and both sides of the copper foil can form nuclei and diffuse to grow graphene films;

[0018] The RF power supply can control the RF coil to crack the incoming carbon source gas, and the cracked carbon atoms enter the three-temperature zone heating furnace. The distance between the RF power supply and the substrate can avoid excessive plasma bombardment on the copper foil to produce graphene with serious etching defects, thereby improving the film quality and efficiency.

[0019] The butterfly valve can control the working pressure in the three-zone heating furnace, so that the carbon source gas is fully decomposed and evenly deposited on the copper foil substrate. Due to the difference in molecular weight between the carrier gas and the protective gas, the protective gas is mainly concentrated in the middle and lower part of the three-zone heating furnace, so that the deposited film outside the three-zone heating furnace will not be disturbed by the reaction gas. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to facilitate understanding by those skilled in the art, the present invention is further described below in conjunction with the accompanying drawings;

[0021] Figure 1 It is the overall axonometric diagram of the present invention;

[0022] Figure 2 It is a schematic diagram of the overall side view structure of the present invention;

[0023] Figure 3 It is an overall top view cross-sectional view of the present invention;

[0024] In the figure: 1. furnace tube; 2. three-temperature zone heating furnace; 3. radio frequency coil; 4. first air inlet; 5. first scroll; 6. feed bin; 7. transmission motor; 8. second air inlet; 9. air outlet; 10. butterfly valve; 11. second scroll; 12. discharge bin; 13. molecular pump; 14. mechanical pump; 15. fan; 16. baffle valve; 17. radio frequency power supply; 18. flow cabinet; 19. touch screen control panel; 20. compound vacuum gauge; 21. butterfly valve controller. DETAILED DESCRIPTION

[0025] like Figure 1-3 As shown, a multi-gas source plasma enhanced CVD system includes a furnace tube 1, a three-temperature zone heating furnace chamber 2, a radio frequency coil 3, a first air inlet 4, a first reel 5, a feed bin 6, a transmission motor 7, a second air inlet 8, an air outlet 9, a butterfly valve 10, a second reel 11, a discharge bin 12, a molecular pump 13, a mechanical pump 14, a fan 15, a baffle valve 16, a radio frequency power supply 17, a flow cabinet 18, a touch screen control panel 19, a compound vacuum gauge 20 and a butterfly valve controller 21, the three-temperature zone heating furnace chamber 2 is fixed to the top center of the flow cabinet 18 by bolts, the three-temperature zone heating furnace chamber 2 is provided with a furnace tube 1 inside, two fans 15 are correspondingly installed on the top of the flow cabinet 18, a touch screen control panel 19 is embedded on one side of the fan 15, the fan 15 is fixed to the flow cabinet 18 by bolts, and the two fans 15 are respectively located on the two sides of the three-temperature zone heating furnace chamber 2;

[0026] The top of the flow cabinet 18 is respectively fixed with a feed bin 6 and a discharge bin 12 by bolts, and the feed bin 6 and the discharge bin 12 are respectively located at the sides of the adjacent fans 15, the inside of the feed bin 6 is movably connected with the first reel 5 by a bearing, the inside of the discharge bin 12 is movably connected with the second reel 11 by a bearing, and a transmission motor 7 is fixed with bolts on one side of the feed bin 6, and the transmission motor 7 is connected to the first reel 5 via a coupling;

[0027] A first air inlet 4 and a second air inlet 8 are provided on the outer side of the furnace tube 1, and a radio frequency coil 3 is sleeved on the outer edges of the first air inlet 4 and the second air inlet 8. A molecular pump 13 is movably connected to the outer side of the furnace tube 1 through a flange, a mechanical pump 14 is fixed to the top of the flow cabinet 18 through bolts, and the mechanical pump 14 is located on the side of the molecular pump 13, a vacuum pipeline is provided between the mechanical pump 14 and the furnace tube 1, and a butterfly valve 10 is installed on the outer side of the vacuum pipeline, and an air outlet 9 is provided on the vacuum pipeline between the furnace tube 1 and the butterfly valve 10, a baffle valve 16 is installed on one side of the molecular pump 13, the first air inlet 4 and the second air inlet 8 are both located near the discharge bin 12, and the air outlet 9 is located near the feed bin 6;

[0028] A radio frequency power supply 17, a compound vacuum gauge 20 and a butterfly valve controller 21 are respectively embedded in the sides of the flow cabinet 18, and the butterfly valve controller 21 is electrically connected to the butterfly valve 10, and the compound vacuum gauge 20 is connected to the furnace tube 1 through a sealed pipe, and the touch screen control panel 19 is electrically connected to the fan 15, and the radio frequency power supply 17 is electrically connected to the radio frequency coil 3, and the transmission motor 7, the molecular pump 13, the mechanical pump 14 and the baffle valve 16 are all electrically connected to the external power supply.

[0029] Working principle:

[0030] The copper foil plug is installed on the second reel 11, and after the copper foil is pulled through the furnace tube 1, the copper foil is connected to the first reel 5, the furnace tube 1 is sealed, and the mechanical pump 14 is turned on to evacuate to 5*10 -1 Pa, then start the molecular pump 13 to make the vacuum degree in the furnace tube 1 reach 5*10 -3Pa, at this time, the baffle valve 16 is closed, and the first air inlet 4 is used to continuously introduce 50sccm of hydrogen, and after the three-temperature zone heating furnace 2 is heated to 800°C, 30sccm of hydrogen is introduced, and the 30W radio frequency power supply 17 is started to generate a uniform and equivalent plasma glow in the furnace tube 1 to clean the surface of the copper foil, while also promoting the cracking of the carbon source methane and the growth rate of graphene, thereby effectively reducing the graphene growth temperature in the three-temperature zone heating furnace 2, and then 30sccm of hydrogen and 10sccm of methane are introduced. After heating for 100min of growth, the introduction of methane is stopped, and after the temperature drops to 200°C, the introduction of hydrogen is stopped, and then the cracked carbon atoms are deposited and attached to the copper foil under the action of the carrier gas. At a suitable growth temperature, as the growth time increases, the uniformly nucleated carbon atoms gradually diffuse and extend into a film, and are tightened into a roll by the cooperation of the first reel 5 and the second reel 11, and the finished product is taken out after the temperature drops to room temperature.

[0031] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.

Claims

1. A multi-gas source plasma enhanced CVD system, comprising a furnace tube (1), a three-temperature zone heating furnace (2), a radio frequency coil (3), a first air inlet (4), a first scroll (5), a feed bin (6), a transmission motor (7), a second air inlet (8), an air outlet (9), a butterfly valve (10), a second scroll (11), a discharge bin (12), a molecular pump (13), a mechanical pump (14), a fan (15), a baffle valve (16), a radio frequency power supply (17), a flow cabinet (18), a touch screen control panel (19), a compound vacuum gauge (20) and a butterfly valve controller (21), characterized in that: A three-temperature zone heating furnace (2) is fixed at the top center of the flow cabinet (18) by bolts, a furnace tube (1) is arranged inside the three-temperature zone heating furnace (2), two fans (15) are correspondingly installed on the top of the flow cabinet (18), and a touch screen control panel (19) is embedded on one side of the fan (15); A feed bin (6) and a discharge bin (12) are fixed to the top of the flow cabinet (18) by bolts, and the feed bin (6) and the discharge bin (12) are respectively located on the sides of adjacent fans (15); a first scroll (5) is movably connected to the inside of the feed bin (6) by a bearing, and a second scroll (11) is movably connected to the inside of the discharge bin (12) by a bearing; a transmission motor (7) is fixed to one side of the feed bin (6) by bolts, and the transmission motor (7) is connected to the first scroll (5) via a coupling; The furnace tube (1) is provided with a first air inlet (4) and a second air inlet (8) on the outside, and the outer edges of the first air inlet (4) and the second air inlet (8) are sleeved with a radio frequency coil (3); the outside of the furnace tube (1) is movably connected to a molecular pump (13) via a flange; a mechanical pump (14) is fixed to the top of the flow cabinet (18) via bolts, and the mechanical pump (14) is located on the side of the molecular pump (13); a vacuum pipeline is provided between the mechanical pump (14) and the furnace tube (1), and a butterfly valve (10) is installed on the outside of the vacuum pipeline; an air outlet (9) is provided on the vacuum pipeline between the furnace tube (1) and the butterfly valve (10), and a baffle valve (16) is installed on one side of the molecular pump (13); A radio frequency power supply (17), a compound vacuum gauge (20) and a butterfly valve controller (21) are respectively embedded in the side of the flow cabinet (18), and the butterfly valve controller (21) is electrically connected to the butterfly valve (10), and the compound vacuum gauge (20) is connected to the furnace tube (1) via a sealed pipe, and the touch screen control panel (19) is electrically connected to the fan (15), and the radio frequency power supply (17) is electrically connected to the radio frequency coil (3), and the transmission motor (7), the molecular pump (13), the mechanical pump (14) and the baffle valve (16) are all electrically connected to an external power supply; The first air inlet (4) and the second air inlet (8) are both located near the discharge bin (12), and the air outlet (9) is located near the feed bin (6); The fan (15) is fixed to the flow cabinet (18) by means of bolts, and the two fans (15) are respectively located on two sides of the three-temperature zone heating furnace (2).

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