Composite laminated waterproof coating preparation device

Abstract

The invention discloses a composite laminated waterproof coating preparation device, and relates to the technical field of multilayer film deposition. A main body is a quartz tube chamber, the quartz tube chamber is divided into a high-temperature heating area where a heating device is located and a cooling area, a sample needing to be coated is placed on a sample objective table in the chamber, and the sample objective table is connected with an external conveying rod; the sample is driven to reciprocate in the high-temperature heating area and the cooling area through the conveying rod, so that the composite laminated waterproof coating of the sample at different deposition temperatures is prepared.

Description

Technical Field

[0001] The invention relates to the technical field of multilayer thin film deposition. Background Art

[0002] Parylene is a good electrical insulation, moisture-proof, mildew-proof and salt-fog-proof coating material in the contemporary world. It has the best water-blocking ability among organic materials and is widely used in the preparation of micron-level high-conformal waterproof film coatings. However, its preparation requires the gaseous Parylene raw material to be cracked into reactive monomers under high-temperature 600-700℃ pyrolysis conditions, and the gaseous monomers are then deposited and polymerized into thin film coatings at room temperature; nano-scale metal oxide films deposited using ALD technology, such as aluminum oxide films, can also be used to prepare dense pinhole-free water-blocking coatings, but they also have the disadvantage that thin film coatings are easily disturbed by surface particles. By adding the ALD thin film deposition process on the basis of the Parylene vacuum vapor deposition process, the composite laminated waterproof coating of ALD coating plus Parylene can be prepared, which can greatly improve the waterproof effect of the coating compared with the single Parylene thin film coating. Summary of the invention

[0003] In view of the problems in the prior art, the present invention provides a device for preparing a laminated waterproof coating, which solves the technical problem of preparing a repeatedly laminated waterproof coating of ALD coating plus Parylene by moving the position under the same cavity, and improves the waterproof effect of the coating. It avoids the high time consumption of changing the cavity and the high cost of temperature rise and fall in the traditional preparation process. At the same time, the present invention can achieve the laminated preparation of thin films with different deposition temperatures by moving the sample position under the same cavity, which can better fit the production process.

[0004] The technical solution adopted by the present invention is: A composite laminated waterproof coating preparation device, the main body of which is a quartz tube chamber, the quartz tube chamber is provided with a chamber air inlet, the chamber air inlet is connected to a precursor gas path and a carrier gas path, a high-temperature heating zone where a heating device is located, a cooling zone, a conveying rod and an air extraction path, the sample is placed on a sample stage connected to the conveying rod after opening the chamber sealing cover, and then the chamber sealing cover is closed, and the sample on the sample stage is driven to reciprocate in the high-temperature heating zone and the cooling zone by the conveying rod to realize the preparation of a composite laminated waterproof coating with different deposition temperatures of the sample.

[0005] Furthermore, the gas path structure of the chamber includes a chamber air inlet path and an air exhaust path provided on the quartz tube chamber, the chamber air inlet path is connected to the precursor gas path and the carrier gas path, and the air exhaust path is connected to a cold trap and a vacuum pump.

[0006] Furthermore, the present invention can achieve stacking preparation of thin films with different deposition temperatures by moving the sample position under the same chamber conditions, which can better fit the production process.

[0007] Furthermore, a method for preparing a composite laminated waterproof coating is implemented by the above-mentioned device, wherein the quartz tube chamber is connected to the precursor source and the carrier gas through the chamber air inlet, the precursor gas path is turned on for preheating, the sample is placed on the sample stage and then the chamber is sealed, the sample is placed in the chamber cooling zone through the transfer rod, the sample chamber heating device is turned on to raise the temperature to 600-700°C, and the carrier gas path valve is opened to allow N 2 Purge. Open the precursor gas valve, then adjust the temperature of the heating device to deposit another thin film, and use the conveyor rod to drive the sample on the sample stage to reciprocate between the high-temperature heating zone and the cooling zone to achieve multi-layer film coating of the sample at different deposition temperatures.

[0008] The intended technical effects of the present invention are: This patent is a vacuum vapor deposition device, which uses ALD technology and vacuum vapor deposition technology to realize the preparation of repeated laminated waterproof coatings on the sample surface. For example, Parylene and aluminum oxide laminates. If the traditional deposition preparation process is followed, it is necessary to switch back and forth between the Parylene vacuum vapor deposition device and the ALD deposition device to realize the preparation of thin film laminates. The traditional process has low preparation efficiency and will greatly increase the time cost and economic cost in the preparation process. Therefore, in the design of this patent, by dividing the quartz tube chamber into a high-temperature heating zone and a cooling zone, the high-temperature heating zone can provide a temperature of 600-700°C to decompose the precursor into an active monomer, which is blown to the chamber cooling zone through the carrier gas to deposit a polymerized thin film coating at room temperature. At the same time, the high-temperature heating zone can provide reaction temperature conditions for the ALD process, such as 80°C. The function of the cooling zone is to provide a room temperature deposition environment for the deposition of certain precursors. Therefore, this patent can move the position of the sample back and forth between the high-temperature heating zone and the cooling zone under the condition of the same cavity through the conveying rod to realize the preparation of repeated laminations of ALD coating plus Parylene. Therefore, compared with the traditional preparation process, the time cost and economic cost are greatly reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1 It is a quartz tube composite laminated thin film deposition equipment.

[0010] In the figure: 1. Quartz chamber; 2. Chamber air inlet; 3. Needle valve; 4. ALD valve; 5. Precursor A; 6. Carrier gas line; 7. Precursor B; 8. Precursor C; 9. Heating device; 10. Sample stage; 11. Cooling zone; 12. Air extraction line; 13. Cold trap; 14. Vacuum pump; 15. Transfer rod; 16. Chamber sealing cover. DETAILED DESCRIPTION

[0011] The technical solution of the present invention is further described below in conjunction with the accompanying drawings.

[0012] By the attached Figure 1 It can be seen that the technical solution adopted in the present invention is that the main body is a quartz tube chamber 1, and the quartz tube chamber 1 is provided with a chamber air inlet 2, a high-temperature heating zone where the heating device 9 is located, a cooling zone 11, a conveying rod 15 and an air exhaust path 12. The sample is placed on a sample stage 10 connected to the conveying rod 15 after opening the chamber sealing cover 16. The conveying rod 15 drives the sample on the sample stage 10 to reciprocate in the high-temperature heating zone and the cooling zone to realize the coating of multi-layer films with different deposition temperatures of the sample.

[0013] The gas inlet of the quartz chamber 1 is connected to the precursor 5 and the carrier gas 6, and the air extraction path 12 is connected to the cold trap 13 and the vacuum pump 14. The chamber heating device 9 and the precursor gas path heating are turned on, the quartz chamber 1 is sealed after the sample is loaded, and the valves 3 of the precursor and carrier gas paths are opened to realize sample coating.

[0014] Taking the deposition of Parylene and aluminum oxide repeated layer waterproof coating as an example, the gas inlet 2 of the quartz chamber 1 is connected to the precursor A (such as Parylene), the precursor B (such as H 2 O), precursor C (such as TMA) and inert gas (such as N 2 ), open the precursor gas circuit for preheating, place the sample on the stage 10 and seal the chamber, place the sample in the chamber cooling zone 11 through the transfer rod 15, start heating the sample chamber to 600-700℃, open the carrier gas circuit valve 3 to pass N 2 Purge. Open the valve 3 of the precursor A gas circuit, close the valve 3 of the precursor B and C gas circuits, and the precursor A (such as Parylene) is pyrolyzed at a high temperature of 600-700°C to crack the gaseous precursor raw material into a monomer with reactive activity. The carrier gas blows the gaseous monomer to the chamber cooling zone 11 to deposit a polymerized thin film coating on the sample at room temperature. The excess precursor A is condensed and captured by the cold trap 13 to prevent leakage. After the deposition of precursor A is completed, close the valve 3 of the precursor A gas circuit, open the valve 3 of the precursor B and C gas circuits, set the sample chamber heating temperature to 80°C, and send the sample to the chamber heating zone through the conveying rod 15. Through the process of precursor B adsorption-carrier gas purge-precursor C adsorption reaction-carrier gas purge, the aluminum oxide film is deposited on the sample surface by ALD. Repeat the above steps to achieve the preparation of repeated laminated waterproof coatings of ALD coating plus Parylene by position movement under the conditions of the same chamber.

[0015] It should be further explained that the above is the basic method of use of the present invention. In practical applications, it is mainly used to achieve the stacking preparation of thin films with different deposition temperatures by moving the sample position under the same chamber conditions, which can better fit the production application. For example, the preparation of Parylene and aluminum oxide repeatedly stacked waterproof coatings. The above embodiments of the present invention are only an explanation of the technical concept of the present invention, which is used to understand the technical solution of the present invention, and it is not a limitation on the protection scope of the present invention. Obvious changes made to the embodiments of the present invention that belong to the technical concept of the present invention should fall within the protection scope of the present invention.

Claims

1. A composite laminated waterproof coating preparation device, characterized by: The main body is a quartz tube chamber (1), and the quartz tube chamber (1) is provided with a chamber air inlet (2), a high-temperature heating zone where a heating device (9) is located, a cooling zone (11), a conveying rod (15), and an air exhaust path (12). After the chamber sealing cover (16) is opened, the sample is placed on a sample stage (10) connected to the conveying rod (15). The conveying rod (15) drives the sample on the sample stage (10) to reciprocate between the high-temperature heating zone and the cooling zone to realize the preparation of a composite laminated waterproof coating with different deposition temperatures for the sample.

2. The composite laminated waterproof coating preparation device according to claim 1 is characterized in that: The gas path structure of the quartz tube chamber (1) comprises: a chamber air inlet path (2) and an air exhaust path (12) are provided on the quartz tube chamber (1); a precursor gas path (5) and a carrier gas path (6) are connected to the chamber air inlet path (2); and a cold trap (13) and a vacuum pump (14) are connected to the air exhaust path.

3. The composite laminated waterproof coating preparation device according to claim 1 is characterized in that: Under the same chamber conditions, the preparation of composite laminated waterproof coatings with different deposition temperatures can be achieved by moving the sample position.

4. The composite laminated waterproof coating preparation device according to claim 1 is characterized in that: The device described in claim 1 is used to connect the precursor source and carrier gas to the quartz tube chamber (1), start the precursor gas circuit for preheating, place the sample on the sample stage (10), seal the chamber, place the sample in the chamber cooling zone (11) through the transfer rod (15), start the sample chamber heating device (9) to raise the temperature to 600-700°C, open the carrier gas circuit valve (3) to introduce N2 for purging. The precursor gas circuit valve (3) is opened, and then another thin film coating is deposited by adjusting the temperature of the heating device (9). The sample on the sample stage (10) is driven to reciprocate between the high-temperature heating zone and the cooling zone through the transfer rod (15) to achieve the preparation of a waterproof coating with repeated lamination of samples at different deposition temperatures.

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