CN116493186A - Film preparation device and method - Google Patents
Film preparation device and method Download PDFInfo
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- CN116493186A CN116493186A CN202210057889.1A CN202210057889A CN116493186A CN 116493186 A CN116493186 A CN 116493186A CN 202210057889 A CN202210057889 A CN 202210057889A CN 116493186 A CN116493186 A CN 116493186A
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- container
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- air
- film
- thin film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000758 substrate Substances 0.000 claims abstract description 129
- 239000010408 film Substances 0.000 claims abstract description 86
- 239000010409 thin film Substances 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 230000008569 process Effects 0.000 claims abstract description 23
- 238000004891 communication Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 28
- 238000010926 purge Methods 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002041 carbon nanotube Substances 0.000 claims description 11
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000005684 electric field Effects 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000002238 carbon nanotube film Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 2
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 claims description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 2
- 238000000059 patterning Methods 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 7
- 239000000428 dust Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000000630 rising effect Effects 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 description 11
- 238000000151 deposition Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 6
- 230000008021 deposition Effects 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- QARVLSVVCXYDNA-UHFFFAOYSA-N bromobenzene Chemical compound BrC1=CC=CC=C1 QARVLSVVCXYDNA-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000001976 improved effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 230000018729 macromolecule modification Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/09—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating separate articles
- B05C3/109—Passing liquids or other fluent materials into or through chambers containing stationary articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C13/00—Means for manipulating or holding work, e.g. for separate articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/159—Carbon nanotubes single-walled
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/04—Nanotubes with a specific amount of walls
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention discloses a film preparation device and a film preparation method, comprising the following steps: a first container for holding a thin film solution; a second container in communication with the first container; and a substrate disposed within the second container; the first container is provided with an air port communicated with the inside, the air port is used for ventilating and pressurizing the first container, the film solution in the first container is pressed into the second container until the substrate is immersed, the air in the first container is discharged through the air port, the film solution in the second container flows back to the first container to expose the substrate, and one-time film preparation is completed. The film preparation device realizes the lifting effect by controlling the rising and falling of the liquid level of the solution under the air pressure, and the substrate is kept fixed without lifting movement, so that the mechanical vibration caused by the movement of a clamp for clamping the substrate is avoided; in addition, the film forming process of the film preparation device can isolate the influence of external dust particles or air flow disturbance and the like, and improve the film quality.
Description
Technical Field
The invention relates to the technical field of film forming, in particular to a film preparation device and a film preparation method.
Background
The dip-draw process to form a film is generally: the whole cleaned substrate is immersed in the prepared solution, then the substrate is stably pulled out of the solution at a precisely controlled uniform speed, a uniform liquid film is formed on the surface of the substrate under the action of viscosity and gravity, and then the solvent is rapidly evaporated, so that the solvent of the solution attached to the surface of the substrate is rapidly evaporated and the solute forms a film. The thickness of the film depends on the concentration, viscosity and pull rate of the solution. In the dip-draw process, a chuck is typically used to hold a substrate and a motor drives the chuck up and down to allow the substrate to freely move in and out of solution.
In such a case, the jig may damage the surface of the substrate, and may cause failure of forming a thin film at the nip contact position, thereby deteriorating the uniformity of the surface of the thin film. On the other hand, since the movement stroke of the substrate is large, and the particle size control of the surrounding environment of the substrate is caused by the movement of the clamp and the driving part, when the substrate is pulled out of the solution, the solution attached to the surface of the substrate contacts with dust particles in the air, and the film quality can be influenced.
In addition, in the process of lifting the clamp and the substrate, mechanical vibration is inevitably generated, so that the stability of the liquid level of the solution is affected, and the parallelism and consistency of the downstream film formation are affected. Meanwhile, the existing lifting device is large in size, sealing is difficult to achieve, external influences are isolated, the stability of the liquid level of the solution can be influenced due to disturbance of air flow in the process, and the process of film formation by direct discharge is influenced. And only can realize single-sheet lifting, and the film deposition efficiency is lower.
In view of this, the present invention has been made.
Disclosure of Invention
In order to solve the problems, the invention provides a film preparation device and a film preparation method, which can improve the consistency of the film surface and the film forming quality without using a clamp, and the specific technical scheme is as follows:
in a first aspect, an embodiment of the present invention provides a thin film preparation apparatus, including:
a first container for holding a thin film solution, the first container having an air port and a first container port in communication with the interior;
a second container with an opening, wherein the second container is positioned above the first container and is communicated with the first container through a liquid guide pipe, the liquid guide pipe is provided with a sealing plug, and the sealing plug is sealed at the opening of the first container;
the second container is provided with a second container cover outside, and the second container cover seals the first container and the second container to form a sealed space;
and a substrate support disposed within the second container.
In an embodiment of the first aspect of the present invention, the second container is a flat square container, and the second container cover has a purge air inlet, an air outlet, and a pressurized air port.
In an embodiment of the first aspect of the invention, said catheter extends into the bottom of said first container at a distance of between 1 and 10mm from the bottom wall of the first container.
In an embodiment of the first aspect of the present invention, the first container opening is a frosted opening with frosting on the inner ring, and the sealing plug is a frosted plug with frosting on the outer ring.
In an embodiment of the first aspect of the invention, there is a purge vessel in communication with the first vessel and the second vessel, wherein there is a three-way valve between the first vessel, the second vessel and the purge vessel.
In an embodiment of the first aspect of the present invention, the substrate support includes a support tray and substrate clamping columns, the substrate clamping columns are fixed on the left and right sides of the upper surface of the support tray, and the upper ends of the substrate clamping columns are provided with substrate clamping grooves.
In an embodiment of the first aspect of the present invention, the plane of the substrate clamping post is perpendicular to or at an angle to the upper surface of the support tray, or the second container (6), the support tray (18) and the substrate clamping post (16) are all perpendicular to or at an angle to the horizontal liquid surface.
In an embodiment of the first aspect of the present invention, the lower surface of the bracket tray is provided with bracket legs, and the bracket tray is provided with a through hole.
In an embodiment of the first aspect of the present invention, the substrate support includes a support lever connected to the support tray, the support lever has an exhaust passage penetrating to the bottom of the support tray, and the support lever has an exhaust port communicating with the exhaust passage.
In an embodiment of the first aspect of the present invention, an electric field or magnetic field generating means for applying an electric field or magnetic field during the film formation is provided outside the film formation apparatus.
In an embodiment of the first aspect of the present invention, the air control device further comprises an electrical control box, an upper computer, a pressurizing air channel, a pressure relief air channel and a purging air channel.
In an embodiment of the first aspect of the present invention, one end of the pressurizing air path is connected with the main air inlet pipeline, and is sequentially connected with the pressurizing air path needle valve, the pressurizing air path pneumatic diaphragm valve and the pressurizing air path one-way valve, and the other end of the pressurizing air path is connected with the air port of the first container;
one end of the pressure relief air channel is connected with a pressure relief air discharge pipeline, a pressure relief air channel needle valve, a pressure relief pneumatic diaphragm valve and a pressure relief air channel one-way valve are sequentially connected, and the other end of the pressure relief air channel is connected with the air port of the first container.
The second aspect of the present invention also provides a method for preparing a thin film by a thin film preparation apparatus, comprising the steps of:
introducing the thin film solution into a first container;
placing at least one substrate on a substrate holder and placing the substrate holder in a second container (6);
the pressurizing air channel is controlled to be conducted and the pressure releasing air channel is controlled to be closed through the air control device, the pressurizing air channel is used for ventilating and pressurizing the first container through the air port, and the film solution in the first container is pressed into the second container through the liquid guide tube until the substrate is immersed;
the pressurizing air channel is controlled to be closed and the pressure relief air channel is controlled to be conducted through the air control device, air in the first container is discharged from the pressure relief air channel through the air port, the pressure relief speed of the pressure relief air channel is controlled to enable the film solution in the second container to gradually descend and flow back to the first container, the substrate is completely exposed, and nitrogen or compressed air is introduced through the purging air channel to purge the surface of the substrate, so that no solution residue exists on the surface; repeating the above process for multiple times to complete the film preparation, and controlling the film density by controlling the repetition times.
In the embodiment of the second aspect of the invention, the pressure release speed of the pressure release gas circuit is controlled to enable the film solution in the second container to slowly descend, so that the self-assembly process of carbon nanotube film preparation is realized, the uniform and parallel carbon nanotube array preparation is realized, or the flow rate of the solution in the second container (6) to the first container (1) is controlled by controlling the needle valve.
In the embodiment of the second aspect of the invention, the pressure release speed of the pressure release gas circuit is controlled to enable the film solution in the second container to rapidly descend for a plurality of times, the pressure or nitrogen purging is added to the 2 nd container after the film solution descends to expose the substrate, the residual solution on the surface of the substrate is rapidly volatilized and cleaned, then the processes of substrate immersing and descending and drying are repeated, and the disordered carbon nanotube film preparation is realized by controlling the repetition times and adjusting the density of the carbon nanotubes of the film.
In an embodiment of the second aspect of the present invention, the thin film solution is a carbon nanotube solution, and the substrate surface has an insulating material selected from the group consisting of silicon oxide, glass, polymer, yttrium oxide, and hafnium oxide.
In an embodiment of the second aspect of the present invention, a co-sheet parallel to the substrate is simultaneously placed on the substrate holder, and the distance between the co-sheet and the substrate is 0.5-20mm, preferably 2-10mm; the accompanying sheet and the substrate have an inclined angle in a range of 30-90 degrees relative to the horizontal direction of the liquid surface, and preferably, the surface of the accompanying sheet is provided with surface modification (such as macromolecule modification or deposited medium film) or patterning.
In an embodiment of the second aspect of the present invention, the substrate is purged by introducing nitrogen or compressed air through the purge gas path after exposing the substrate.
In an embodiment of the second aspect of the present invention, a negative pressure pipe is connected to the exhaust port of the holder lift bar after exposing the substrate, and an external atmosphere is introduced from the opening of the second container to purge the substrate, and is then exhausted through the exhaust port.
According to the film preparation device, the lifting effect is realized by controlling the rising and falling of the liquid level of the solution through the air pressure, the substrate is kept fixed without lifting movement, on one hand, no mechanical vibration is generated, the production noise of mechanical equipment is low, the disturbance of the mechanical vibration on the liquid level of the solution is avoided, and the smooth discharge is influenced; on the other hand, impurity ions are prevented from being introduced by the movement of a clamp for clamping the substrate, so that a film with good surface consistency is formed; in addition, the substrate is kept motionless during the film preparation process, so that external fields such as an electric field, a magnetic field and the like can be conveniently applied to induce alignment. Meanwhile, the film preparation device disclosed by the invention is contacted with dust particles as little as possible in the film forming process, and no metal material exists in the whole device, so that the film is prevented from being polluted by metal ions. The film device can be placed in a closed environment, so that air flow disturbance and interference of dust particles in air and the like are avoided, and the device is clean and low in cost. Meanwhile, the scheme of parallel accompanying sheets is easier to realize, the substrate placement angle is easier to adjust, the regulation and control of a double-liquid-phase system interface, the liquid level shape, the surface tension and the like are realized, the liquid level stability is increased, and the improvement of the stability, the new and the consistency of the film downstream is facilitated. In addition, the device can simultaneously place a plurality of substrates, realizes batch preparation, greatly improves the film making efficiency, can also be compatible with wet etching and cleaning processes, and has wide application prospect.
Drawings
FIG. 1 is a schematic view showing the structure of a thin film formation apparatus according to an embodiment of the present invention in which a substrate is vertically placed;
FIG. 2 is an exploded view of a thin film fabrication apparatus according to an embodiment of the present invention in which a substrate is vertically placed;
FIG. 3 is a schematic view showing the structure of a substrate holder of a thin film formation apparatus according to an embodiment of the present invention in which a substrate is vertically placed;
FIG. 4 is an enlarged view of a portion of a substrate clamping post of a thin film fabrication apparatus according to an embodiment of the present invention with a substrate vertically disposed;
FIG. 5 is a schematic diagram of a bypass purge vessel;
FIG. 6 is a schematic diagram of air circuit control;
FIG. 7 shows the results of a fast volatilization and multiple pull mode film pull experiment.
Reference numerals in the drawings illustrate: 1-a first container 2-an air port 3-a first clamp connection part 4-a first container port 5-a second clamp connection part 6-a second container 7-an air outlet 8-a second container cover 9-a purging air inlet 10-a liquid guide tube 11-a sealing plug 12-a tray 13-a supporting base surface 14-a support leg 15-a support lifting rod 16-a substrate clamping column 17-a through hole 18-a support tray 19-a support leg 20-a substrate clamping groove 21-a three-way valve 22-a liquid guide tube A-an air outlet B-a purging air inlet C-a pressurizing air hole.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. It will be apparent that the described embodiments are some, but not all, embodiments of the invention.
Thus, the following detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely representative of some embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, under the condition of no conflict, the embodiments of the present invention and the features and technical solutions in the embodiments may be combined with each other. It should be noted that like reference numerals and letters in the present invention denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, the terms "upper", "lower", and the like indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, or an azimuth or a positional relationship conventionally put in use of the inventive product, or an azimuth or a positional relationship conventionally understood by those skilled in the art, such terms are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or element to be referred must have a specific azimuth, be constructed and operated in a specific azimuth, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used merely to distinguish between descriptions and should not be construed as indicating or implying relative importance.
Referring to fig. 1 to 7, the present embodiment provides a thin film manufacturing apparatus and a manufacturing method thereof, and the details are as follows:
a first container 1 for holding a thin film solution, which in this embodiment is a carbon nanotube solution, the first container 1 having a gas port 2 and a first container port 4 communicating with the inside; a second container 6 with an opening, the second container 6 being located above the first container 1 and communicating with the first container 1 via a catheter which extends into the bottom of said first container 1 and is spaced from the bottom wall of the first container 1 by a distance of between 1 and 10mm. In another embodiment the bottom opening of the catheter is a beveled opening preventing the catheter from extending into the first container 1 and being blocked by the bottom wall, resulting in a failure of the solution to circulate therethrough. The first container 1 and the second container 6 are arranged up and down, so that the film solution is pressed into the second container 6 and can naturally flow back to the first container 1 under the action of gravity, meanwhile, as the solvent in the film solution has a certain corrosion effect, a rigid quartz tube is adopted as a liquid guide tube to prevent corrosion to common plastic or rubber hoses in the embodiment, the first container and the second container are also made of all-quartz materials, and the first container and the second container are arranged up and down to be matched with the rigid liquid guide tube to be used, so that external bending is avoided. In another embodiment, the first container and the second container may not necessarily be in the same vertical direction, and may be in communication with each other through a bent catheter.
The catheter 10 is provided with a sealing plug 11, and the sealing plug 11 is blocked at the first container port 4; the first container mouth 4 is a frosted mouth with frosted inner ring, and the sealing plug 11 is a frosted plug with frosted outer ring. In one embodiment the second container 6, the vent 7, and the catheter 10, the sanding plug are integrally formed with a sanding plug outer collar having sanding. The frosted opening of the first container 1 and the frosted plug of the second container 6 are clamped, and the first clamp connection part 3 and the second clamp connection part 5 can be connected through the clamp, so that the connection of the first container 1 and the second container 6 is more fastened, and the air leakage and the disconnection of the connection part of the first container 1 and the second container 6 caused by air inlet and air exhaust are avoided.
In another embodiment, as shown in fig. 1-4, a substrate to be deposited is vertically placed in a substrate holder, the substrate holder includes a holder tray 18 and substrate clamping posts 16, the substrate clamping posts 16 are fixed on left and right sides of an upper surface of the holder tray 18, and a substrate clamping groove 20 is formed at an upper end portion of the substrate clamping posts 16. The plane of the substrate clamping post 16 is perpendicular to the upper surface of the support tray 18. In another embodiment, the substrate clamping posts are angled to the surface of the support tray, and the substrate is placed at an angle to achieve more uniform deposition of the film by generating shear forces at the solution level. In another embodiment, the second container (6), the support tray (18) and the substrate clamping post (16) may be perpendicular or angled to the horizontal liquid surface as a whole.
The substrate card slot 20 is much less shielded from the substrate surface than the clamping structure and can be ignored. In fig. 4, there are two substrate card slots 20, and there may be one or more card slots; the substrate card slot 20 may be placed at other than 90 degrees. The lower surface of the support tray 18 is also provided with support legs 19, the support tray 18 is provided with through holes 17, when the solution in the first container 1 is pressed into the second container 6' and the substrate is immersed, the solution passes through the periphery of the support tray 18 and the through holes 17, and the through holes 17 can avoid shaking instability of the support tray 18 caused by high hydraulic pressure.
In another embodiment, a cosheet can be arranged beside the substrate to be deposited, so that the film is induced during deposition, and even deposition of the film is further realized. The distance between the cosheet and the substrate is 0.5-20mm, preferably 2-10mm. In addition, the accompanying sheet and the substrate have an inclined angle in the range of 30-90 degrees, preferably 45-90 degrees, compared with the horizontal direction of the liquid level, and the adoption of the interval range and the inclined angle can lead the shearing force between the substrate and the solution to realize induction during the deposition of the substrate film, so as to obtain a more uniform film. In another embodiment, the surface of the accompanying sheet can be modified or patterned so as to adjust the surface property of the accompanying sheet, control the infiltration characteristic and the surface tension characteristic of the accompanying sheet with the liquid level, adjust the shape of the liquid level between the substrate and the accompanying sheet, and better play a role in inducing when the film is deposited.
In the conventional pulling method for depositing a thin film, the substrate is usually pulled at a vertical angle to the solution, so that the substrate cannot be pulled at an inclined angle, and thus a more uniform thin film deposited cannot be obtained by using a shearing force. Therefore, in the embodiment of the invention, the substrate placement angle is easier to adjust, the interface, the liquid level shape, the surface tension and the like of the double-liquid-phase system are regulated and controlled, the liquid level stability is improved, and the improvement of the stability and the consistency of the thin film in-line is facilitated.
Further, the substrate support comprises a support lifting rod 15 connected with the support tray 18, an exhaust channel penetrating to the bottom of the support tray 18 is arranged in the support lifting rod 15, and an exhaust port communicated with the exhaust channel is arranged on the support lifting rod 15. In the above embodiment in which the substrate is placed vertically, the second container 6 is a flat square container, so that the amount of solution required is minimized. In this embodiment, the second container cover 8 may be provided to cover all the first container 1 and the second container 6 integrally to form a sealed space, and nitrogen or inert gas is filled into the sealed space as a protective gas, so as to avoid pollution caused by contact between the substrate and air during film preparation, prevent gas from overflowing during film preparation, and reduce pollution to external environment. The second container cover 8 generally has a through hole therein connected to an external gas path. In other embodiments, an electric field or magnetic field generating device is provided outside the thin film formation apparatus to apply an electric field or magnetic field during the thin film formation process, thereby generating an external force upon the thin film deposition to enhance the thin film formation uniformity.
Further, as shown in fig. 6, the embodiment of the invention further comprises a gas control device, wherein the gas control device comprises an electric control box, an upper computer, a pressurizing gas circuit, a pressure relief gas circuit and a purging gas circuit. One end of the pressurizing air passage is connected with the main air inlet pipeline, the pressurizing air passage needle valve 1, the pressurizing air passage pneumatic diaphragm valve 2 and the pressurizing air passage one-way valve 2 are sequentially connected, and the other end of the pressurizing air passage is connected with an air port of the first container; one end of the pressure relief air passage is connected with a pressure relief air discharge pipeline, a pressure relief air passage needle valve 2, a pressure relief pneumatic diaphragm valve 3 and a pressure relief air passage one-way valve are sequentially connected, and the other end of the pressure relief air passage is connected with the air port of the first container. The purging gas circuit and the pressurizing gas circuit have a common air inlet end, and are sequentially connected with a pneumatic diaphragm valve 1 of the purging gas circuit and a one-way valve 2 of the purging gas circuit;
the thin film preparation device of the embodiment realizes the lifting effect by arranging the first container 1 and the second container 6 which are mutually communicated and controlling the rising and the falling of the liquid level of the solution through the air pressure, and the substrate is kept fixed without lifting movement, so that impurity ions are prevented from being introduced by the movement of the clamp for clamping the substrate, the vibration of the substrate caused by the lifting movement of the clamp is avoided, and the thin film with good consistency is formed. In addition, the thin film preparation device of the embodiment is contacted with dust particles as little as possible in the process of forming the thin film, so that the quality of the thin film is improved.
In another embodiment of the present invention, a method for preparing a thin film using the thin film preparation apparatus is also provided, which specifically includes the steps of first introducing a thin film solution, in which carbon nanotubes are dissolved in one or more halogenated hydrocarbons, preferably chloroform, dichloroethane, trichloroethane, chlorobenzene, dichlorobenzene, bromobenzene, etc., into a first container. Wherein the carbon nanotubes are selected from single-walled carbon nanotubes, double-walled carbon nanotubes or multi-walled carbon nanotubes. Then placing at least one substrate on the substrate support, and placing the substrate support in a second container, wherein the substrate is a silicon oxide wafer in the embodiment, and glass, metal or plastic in other embodiments; the pressurizing air channel is controlled to be conducted and the pressure releasing air channel is controlled to be closed through the air control device, the pressurizing air channel is used for ventilating and pressurizing the first container through the air port, and the film solution in the first container is pressed into the second container through the liquid guide tube until the substrate is immersed; then, the pressurizing air channel is controlled to be closed and the pressure relief air channel is controlled to be conducted through the air control device, air in the first container is discharged from the pressure relief air channel through the air port, the pressure relief speed of the pressure relief air channel is controlled to enable the film solution in the second container to slowly descend or rapidly descend, the film solution flows back to the first container and is completely exposed out of the substrate, and nitrogen or compressed air is introduced through the purging air channel to purge the surface of the substrate, so that no solution remains on the surface; repeating the above process for multiple times to complete the film preparation, and controlling the film density by controlling the repetition times.
For the situation that the substrate is vertically placed to prepare disordered carbon nanotubes, the liquid level is lowered, the pressure of a pressure relief gas circuit is regulated, so that the liquid level is quickly lowered, the residual solution on the surface of the substrate is quickly volatilized and cleaned by adding pressure or nitrogen purging to a second container, the processes of immersing and lowering the substrate and drying the substrate are repeated, the film preparation is realized, the carbon nanotube density of the film is regulated by controlling the repetition times, and the film prepared by the method is shown in a figure 7; for the forward discharge process, the pressure of the pressure relief gas circuit is controlled, or the flow rate of the solution in the second container to the first container is controlled by controlling the needle valve, so that the liquid level slowly descends, the self-assembly process of the carbon nanotube film preparation is realized, and the uniform forward discharge carbon nanotube array is realized.
In this embodiment, the film solution in the second container 6 is hydraulically returned to the first container 1 by means of air pressure, and specifically, the film solution may be communicated with the second container 6 by means of an air pressure device, and after the air in the first container 1 is depressurized, the air pressure device is controlled to pressurize the second container 6 to hydraulically return the film solution to the first container 1. This method requires an additional air pressure device, but is not required for the installation of the first container 1 and the second container 6, and is not limited to the installation site.
In another embodiment, by means of the positional relationship between the first container 1 and the second container 6, the thin film solution is returned to the first container 1 by gravity, and in particular, referring to the manner in which the second container 6 is disposed above the first container 1 in fig. 1 of the present embodiment, after the gas in the first container 1 is depressurized, the thin film solution in the second container 6 is returned to the first container 1 under the action of gravity.
In another embodiment, the substrate is purged by passing nitrogen or compressed air through a purge gas path after exposing the substrate. In other embodiments, the negative pressure pipeline may be connected to the exhaust port of the support lifting rod after the substrate is exposed, and the external atmosphere is purged from the opening of the second container and then exhausted from the exhaust port, where the external atmosphere is a clean gas such as nitrogen or inert gas. Through purging to the second container, can let the solution that remains on the substrate surface volatilize fast, shorten the process time of film preparation, promote production efficiency.
In another embodiment, a bypass with a cleaning solvent may be provided at the same time, and when cleaning of the device is desired, the device may be switched to another tank containing cleaning agent, by introducing the cleaning solvent. After the cleaning is completed, the solvent tank for depositing the film is switched. As shown in fig. 7, a cleaning vessel 1' containing the same cleaning solution as the first vessel is provided beside the first vessel 1, for example, toluene or chloroform. The first container 1 and the washing container 1' and the second container 6 are connected together by means of a valve 21 and a catheter 22. In this embodiment, the catheter between the first container 1 and the second container 6 may be bent so that the first container 1 and the second container 6 are not in the vertical direction, which is more convenient to flexibly adapt to the space. In another embodiment, the first container 1 and the second container 6 may be in a vertical direction, with the catheter therebetween being a straight tube.
In summary, the thin preparation device of the invention realizes the lifting effect by controlling the rising and falling of the solution liquid level by the air pressure, the substrate keeps fixed without carrying out lifting movement, on one hand, no mechanical vibration is generated, the interference of vibration on film formation, especially the interference of the thin film in the parallel direction, and on the other hand, the impurity ions are prevented from being introduced by the movement of the clamp for clamping the substrate, thereby being beneficial to forming the thin film with good surface consistency; meanwhile, the film preparation device disclosed by the invention is contacted with dust particles as little as possible in the film forming process, and no metal material exists in the whole device, so that the film is prevented from being polluted by metal ions. The device is clean and low in cost. In addition, the device can simultaneously place a plurality of substrates, realizes batch preparation, greatly improves the film-making efficiency, can prepare high-quality parallel carbon nanotube films, is combined with wet etching and cleaning processes, and has wide application prospects in carbon-based integrated circuit processes.
The above embodiments are only for illustrating the present invention and not for limiting the technical solutions described in the present invention, and although the present invention has been described in detail in the present specification with reference to the above embodiments, the present invention is not limited to the above specific embodiments, and thus any modifications or equivalent substitutions are made to the present invention; all technical solutions and modifications thereof that do not depart from the spirit and scope of the invention are intended to be included in the scope of the appended claims.
Claims (18)
1. A thin film formation apparatus, comprising:
a first container (1) for holding a film solution, the first container (1) having a gas port (2) and a first container port (4) communicating with the inside;
a second container (6) with an opening, wherein the second container (6) is positioned above the first container (1) and is communicated with the first container (1) through a liquid guide pipe (10), the liquid guide pipe (10) is provided with a sealing plug (11), and the sealing plug (11) is sealed at the first container opening (4);
the second container (6) is provided with a second container cover (8) outside, and the second container cover (8) seals the first container (1) and the second container (6) to form a sealed space;
and a substrate holder disposed within the second container (6).
2. A thin film production apparatus according to claim 1, wherein the second container (6) is a flat square container, and the second container cover (8) has a purge air inlet, an air outlet, and a pressurizing air port.
3. A film-forming device according to claim 1, wherein the liquid conduit extends into the bottom of the first container (1) at a distance of between 1 and 10mm from the bottom wall of the first container (1).
4. A film forming apparatus according to claim 1, wherein the first container mouth (4) is a frosted mouth with frosting on an inner ring, and the sealing plug (11) is a frosted plug with frosting on an outer ring.
5. The thin film formation apparatus according to any one of claims 1 to 4, characterized by having a cleaning vessel (1 ') in communication with the first vessel (1) and the second vessel (6), wherein a three-way valve (21) is provided between the first vessel (1), the second vessel (6) and the cleaning vessel (1').
6. The thin film formation apparatus as claimed in claim 1, wherein the substrate holder comprises a holder tray (18) and substrate clamping posts (16), the substrate clamping posts (16) are fixed on both left and right sides of an upper surface of the holder tray (18), and substrate clamping grooves (20) are formed in upper end portions of the substrate clamping posts (16).
7. A film forming apparatus according to claim 6, wherein the plane of the substrate-chucking post (16) is perpendicular to or at an angle to the upper surface of the support tray (18);
or the second container (6), the bracket tray (18) and the substrate clamping column (16) are vertical or form a certain angle with the horizontal liquid level.
8. The film forming apparatus according to claim 6, wherein the support tray (18) has support legs (19) on a lower surface thereof, and at least one through hole (17) is formed in the support tray (18).
9. The thin film formation apparatus according to claim 6, wherein the substrate holder comprises a holder lever (15) connected to the holder tray (18), the holder lever (15) having an exhaust passage penetrating to a bottom of the holder tray (18) inside, and the holder lever (15) having an exhaust port communicating with the exhaust passage.
10. A thin film formation apparatus according to claim 1, wherein an electric field or magnetic field generating means for applying an electric field or magnetic field during the thin film formation is provided outside the thin film formation apparatus.
11. The thin film formation apparatus according to claim 1, further comprising a gas control device including an electrical control box, an upper computer, a pressurized gas circuit, a depressurized gas circuit, and a purge gas circuit.
12. The thin film preparation device according to claim 11, wherein one end of the pressurizing air path is connected with a main air inlet pipeline, a pressurizing air path needle valve, a pressurizing air path pneumatic diaphragm valve and a pressurizing air path one-way valve are sequentially connected, and the other end of the pressurizing air path needle valve, the pressurizing air path pneumatic diaphragm valve and the pressurizing air path one-way valve are connected with the air port of the first container;
one end of the pressure relief air channel is connected with a pressure relief air discharge pipeline, a pressure relief air channel needle valve, a pressure relief pneumatic diaphragm valve and a pressure relief air channel one-way valve are sequentially connected, and the other end of the pressure relief air channel is connected with the air port of the first container.
13. A method for producing a thin film by using the thin film production apparatus according to any one of claims 1 to 12, comprising the steps of:
introducing the film solution into a first container (1);
placing at least one substrate on a substrate holder and placing the substrate holder in a second container (6);
the pressurizing air passage is controlled to be conducted and the pressure releasing air passage is controlled to be closed by the air control device, the pressurizing air passage is used for ventilating and pressurizing the first container (1) through the air opening, and the film solution in the first container (1) is pressed into the second container (6) through the liquid guide tube until the substrate is immersed;
the pressurizing air channel is controlled to be closed and the pressure relief air channel is controlled to be conducted through the air control device, air in the first container (1) is discharged from the pressure relief air channel through the air port, the pressure relief speed of the pressure relief air channel is controlled to enable the film solution in the second container (6) to descend and flow back to the first container (1), the substrate is completely exposed, and nitrogen or compressed air is introduced through the purging air channel to purge the surface of the substrate, so that no solution remains on the surface; repeating the above process for multiple times to complete the film preparation, and controlling the film density by controlling the repetition times.
14. The method for preparing the film according to claim 13, wherein the pressure release speed of the pressure release gas path is controlled or the flow rate of the solution in the second container (6) flowing to the first container (1) is controlled by controlling a needle valve, so that the film solution in the second container (6) slowly descends, the self-assembly process of preparing the carbon nano tube film is realized, and the uniform and parallel carbon nano tube array preparation is realized.
15. The method of claim 13, wherein the thin film solution is a carbon nanotube solution and the substrate surface has an insulating material selected from the group consisting of silicon oxide, glass, polymer, yttrium oxide, and hafnium oxide.
16. The method of producing a film according to claim 13, wherein a co-sheet parallel to the substrate is placed on the substrate holder at a distance of 0.5 to 20mm, preferably 2 to 10mm from the substrate; the accompanying sheet and the substrate have an inclined angle in the range of 30-90 degrees compared with the horizontal liquid level direction, and preferably, the surface of the accompanying sheet has surface modification or patterning.
17. The method of claim 15, wherein the substrate is purged by passing nitrogen or compressed air through a purge gas line after exposing the substrate.
18. A method of producing a film according to claim 15, characterized in that after exposing the substrate, a negative pressure pipe is connected to the exhaust port of the holder lift bar, and the external atmosphere is introduced from the opening of the second container (6) to purge the substrate, and is then exhausted through the exhaust port.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210057889.1A CN116493186A (en) | 2022-01-19 | 2022-01-19 | Film preparation device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210057889.1A CN116493186A (en) | 2022-01-19 | 2022-01-19 | Film preparation device and method |
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| Publication Number | Publication Date |
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| CN116493186A true CN116493186A (en) | 2023-07-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210057889.1A Pending CN116493186A (en) | 2022-01-19 | 2022-01-19 | Film preparation device and method |
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| Country | Link |
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| CN (1) | CN116493186A (en) |
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- 2022-01-19 CN CN202210057889.1A patent/CN116493186A/en active Pending
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