Coupling agent evaporation deposition device and method, coupling agent layer and application
By setting up a storage section and a steam pipe insulation layer in front of the coupling agent vaporization chamber, combined with the design of the vacuum deposition chamber, the problem of insufficient bonding force between the coupling agent layer and the substrate was solved, and uniform bonding between the phenelzine layer and the substrate was achieved.
Patent Information
- Application Number
- CN202511404695.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-29
- Publication Date
- 2025-10-31
- Estimated Expiration
- 2045-09-29
AI Technical Summary
In the prior art, the bonding force between the coupling agent layer and the substrate is limited, resulting in insufficient bonding force between the phenelzine layer and the substrate, and the coupling agent cannot uniformly form a bonding film on the substrate surface.
An evaporation deposition apparatus and method for coupling agents are provided, including setting up a coupling agent storage section before the coupling agent vaporization chamber, wrapping the steam pipe with an insulation layer, setting coupling agent steam inlets at intervals on the side wall of the vacuum deposition chamber, and controlling the steam flow rate by branching steam pipes to ensure uniform deposition of coupling agent steam on the substrate surface.
It significantly improves the bonding force between the coupling agent layer and the substrate, thereby enhancing the bonding force between the phenelzine layer and the substrate, and ensuring that the coupling agent layer forms a uniform adhesive film on the substrate surface.
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Figure CN120866772A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of Piriton materials technology, specifically relating to the evaporation deposition apparatus, method, coupling agent layer and application of coupling agents. Background Technology
[0002] Parylene is a polymer film polymerized from xylene, providing various properties such as protection, dry lubrication, barrier properties, and insulation withstand voltage. It is increasingly being used in electronic circuit board protection, semiconductor chip protection, insulation protection of high voltage electrode modules, and so on.
[0003] Perylene is a relatively symmetrical (weakly polar) material with low surface energy, making it difficult to bond with the surface of the product substrate. The bonding strength often fails to meet the product's usage requirements. It has been proposed to deposit a coupling agent layer on the product surface as an adhesive layer before the perylene film grows, to enhance the bonding strength between the perylene film and the product surface.
[0004] Currently, when using a coupling agent layer as an intermediate layer to enhance the bonding force between the phenelzine layer and the substrate, the bonding force between the coupling agent layer and the substrate is limited. The coupling agent cannot uniformly form a bonding film on the substrate surface, which in turn affects the bonding between the phenelzine layer and the substrate.
[0005] It should be noted that this part of the present invention only provides background technology related to the present invention, and does not necessarily constitute prior art or known technology. Summary of the Invention
[0006] The purpose of this invention is to overcome the shortcomings of existing technologies, such as limited bonding force between the coupling agent layer and the substrate, and the inability of the coupling agent to uniformly form a bonding film on the substrate surface, which affects the bonding between the phenelzine layer and the substrate. This invention provides an evaporation deposition apparatus, method, coupling agent layer, and application for coupling agents. When used to prepare coupling agent layers, this invention can enhance the bonding force between the coupling agent layer and the substrate, uniformly form a coupling agent bonding film on the substrate surface, and significantly improve the bonding force between the phenelzine layer and the substrate.
[0007] To achieve the above objectives, in a first aspect, the present invention provides an evaporation deposition apparatus for a coupling agent, comprising: The coupling agent storage section is equipped with a coupling agent outlet; A coupling agent vapor generator includes a coupling agent vaporization chamber, a steam generator is provided outside the coupling agent vaporization chamber, and a coupling agent inlet and a coupling agent vapor outlet are provided on the coupling agent vaporization chamber, with the coupling agent inlet and the coupling agent outlet connected together. The vacuum deposition chamber has at least two coupling agent vapor inlets spaced apart on its sidewall. The coupling agent vapor inlets and coupling agent vapor outlets are connected by steam pipes. At least two branch steam pipes are provided on the side of the steam pipes closest to the coupling agent vapor inlets. Each of the at least two branch steam pipes is connected to one of the at least two coupling agent vapor inlets. Valves are provided on the branch steam pipes. The steam pipes are wrapped with an insulation layer. During evaporation deposition, the valves of each branch steam pipe are opened for a preset time and then closed.
[0008] In some preferred embodiments, the coupling agent storage section is provided with a desiccant containment chamber and a humidity sensor. The desiccant in the desiccant containment chamber removes moisture from the coupling agent storage section, and the humidity sensor monitors the humidity inside the coupling agent storage section.
[0009] In some preferred embodiments, the coupling agent vaporization chamber is further provided with a bypass inlet and a bypass outlet.
[0010] In some preferred embodiments, the coupling agent vaporization chamber is externally wrapped with a heat insulation layer; the coupling agent vaporization chamber is equipped with a liquid level sensor, a pressure gauge and a temperature sensor; and a mass flow meter is installed on the steam pipe to control the amount of coupling agent vapor entering the vacuum deposition chamber.
[0011] In some preferred embodiments, a rotating stage is provided on the central axis of the vacuum deposition chamber, the rotating stage is used to support the fixed substrate, and an evacuation hole is provided on the side wall of the vacuum deposition chamber, the evacuation hole and the rotating stage on the side away from the coupling agent vapor inlet are at an angle of 20° to 40°.
[0012] In a second aspect, the present invention provides an evaporation deposition method for a coupling agent applied to an evaporation deposition apparatus for a coupling agent as described in the first aspect, comprising: placing a coupling agent in a coupling agent storage section, introducing dry compressed air into the coupling agent storage section, and forcing the coupling agent from a coupling agent outlet through a coupling agent inlet into a coupling agent vaporization chamber; heating the coupling agent entering the coupling agent vaporization chamber using a steam generator to vaporize it into coupling agent vapor; opening valves in branch steam pipes for a preset time and then closing the valves; and depositing a coupling agent layer on the substrate surface within the vacuum deposition chamber through a steam pipe from a coupling agent vapor outlet into a coupling agent vapor inlet.
[0013] In some preferred embodiments, the desiccant in the desiccant containment cavity removes moisture from the coupling agent storage section, and when the humidity sensor detects that the humidity in the coupling agent storage section exceeds a preset value, the desiccant is replaced and / or added.
[0014] In some preferred embodiments, the method further includes: before introducing dry compressed air into the coupling agent storage section, repeating the step of removing moisture from the coupling agent vaporization chamber, the step of removing moisture including sequentially evacuating the coupling agent vaporization chamber through a bypass outlet and introducing inert gas into the coupling agent vaporization chamber through a bypass inlet.
[0015] In some preferred embodiments, the method further includes: controlling the flow of coupling agent into the coupling agent vaporization chamber by means of a liquid level sensor according to the amount of coupling agent required for each branch steam pipe; before switching branch steam pipes, raising the temperature in the coupling agent vaporization chamber to above the coupling agent vaporization temperature by means of a steam generator, and evacuating the coupling agent vaporization chamber through a bypass outlet.
[0016] Preferably, the amount of coupling agent required for each branch steam pipe is divided into a preset number of portions, and the coupling agent is controlled by a liquid level sensor to enter the coupling agent vaporization chamber in the preset number of portions.
[0017] In some preferred embodiments, the method further includes: turning on the mass flow meter after the barometer detects that the pressure in the coupling agent vaporization chamber has reached a preset pressure; and adjusting the heating power of the steam generator according to the monitoring results by monitoring the temperature in the coupling agent vaporization chamber.
[0018] Thirdly, the present invention provides a coupling agent layer on the surface of a substrate, which is obtained by evaporation deposition using the coupling agent evaporation deposition apparatus described in the first aspect or the coupling agent evaporation deposition method described in the second aspect.
[0019] Fourthly, the present invention provides an application in the process of preparing a pyrene layer on a substrate surface, using an evaporation deposition apparatus for a coupling agent as described in the first aspect, or an evaporation deposition method for a coupling agent as described in the second aspect, or a coupling agent layer as described in the third aspect.
[0020] The inventors discovered that the bonding strength between the coupling agent layer and the substrate in existing technologies is limited, thus affecting the bonding strength between the phenelzine layer and the substrate. The coupling agent evaporation deposition apparatus of this invention includes a coupling agent storage section before the coupling agent vaporization chamber. The coupling agent is introduced from the storage section into the vaporization chamber as needed, according to the type of coupling agent and the deposition area. This avoids repeated heating of the coupling agent by the steam generator and prevents the coupling agent's molecular weight from being too large to penetrate the pores on the substrate surface, thereby improving the bonding force between the coupling agent and the substrate. It also avoids direct contact between the coupling agent and the vaporization chamber. When the coupling agent is added to the cavity, moisture is introduced into the vaporization cavity, causing hydrolysis of the coupling agent and thus improving the adhesion between the coupling agent layer and the substrate. The steam pipe between the coupling agent vapor inlet and outlet is wrapped with an insulation layer to prevent condensation of the coupling agent vapor upon cooling. After vaporization, the coupling agent transforms from gas into small droplets. These droplets, upon reaching the deposition cavity, easily adhere to the substrate, becoming foreign matter on the substrate surface. This prevents the coupling agent from forming a 'bonding' film between the coupling agent and the substrate, rendering it ineffective as a coupling agent and affecting its function. The bonding strength between the pyrelin layer and the substrate is improved by: At least two coupling agent vapor inlets are spaced apart on the sidewall of the vacuum deposition chamber; at least two branch vapor pipes are located on the side of the vapor pipe closest to the coupling agent vapor inlets, each branch vapor pipe being connected one-to-one with one of the coupling agent vapor inlets; valves are installed on the branch vapor pipes; since the deposition gas flows dynamically inside the deposition chamber, fresh coupling agent vapor enters through the coupling agent vapor inlets, and undeposited coupling agent vapor is extracted through the evacuation port; the valves are opened and closed sequentially through the branch vapor pipes for a preset time; and coupling agent vapor is introduced into the vacuum deposition chamber sequentially through the spaced at least two coupling agent vapor inlets. This ensures uniform adhesion of the coupling agent vapor to the substrate surface, preventing excessive local concentrations of coupling agent gas due to diffusion and overlap, which increases the chance of collisions between coupling agent molecules and causes spontaneous condensation into small droplets in the vacuum deposition chamber. This prevents the coupling agent from forming a 'bonding' film between the pyrelin layer and the substrate, thereby improving the bonding strength between the pyrelin layer and the substrate.
[0021] This invention significantly improves the bonding force between the pyrene layer and the substrate by setting a coupling agent storage section before the coupling agent vaporization chamber, wrapping the steam pipe between the coupling agent vapor inlet and the coupling agent vapor outlet with a heat insulation layer, setting at least two coupling agent vapor inlets at intervals on the side wall of the vacuum deposition chamber, setting at least two branch steam pipes on the side of the steam pipe near the coupling agent vapor inlet, and connecting the at least two branch steam pipes one-to-one with the at least two coupling agent vapor inlets. Valves are set on the branch steam pipes. During evaporation deposition, the valves of the branch steam pipes are opened for a preset time and then closed. Attached Figure Description
[0022] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.
[0023] Figure 1 This is a schematic diagram of the evaporation and deposition apparatus for the coupling agent of the present invention; Figure 2 This is a top view of the vacuum deposition cavity of the present invention.
[0024] Explanation of reference numerals in the attached figures 10. Coupling agent storage section; 11. Coupling agent outlet; 12. Humidity sensor; 20. Coupling agent vapor generator; 21. Coupling agent vaporization chamber; 22. Steam generator; 23. Coupling agent inlet; 24. Coupling agent vapor outlet; 25. Liquid level sensor; 26. Barometer; 27. Temperature sensor; 30. Steam pipeline; 31. Mass flow meter; 32. Branch steam pipeline; 33. Valve; 40. Vacuum deposition chamber; 41. Coupling agent vapor inlet; 42. Evacuation port. Detailed Implementation
[0025] The endpoints and any values of the ranges disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of the various ranges, the endpoint values of the various ranges and individual point values, and individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.
[0026] In this document, unless otherwise stated, directional terms such as "upper" and "lower" generally refer to the orientation shown in the accompanying drawings and in actual application, and "inner" and "outer" refer to the inner and outer contours of the component.
[0027] In the description of this invention, it should be understood that the terms "center," "lateral," "width," "thickness," "upper," "lower," "vertical," "top," "bottom," "inner," "outer," "radial," and "circumferential," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting this invention.
[0028] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0029] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first and second features are in direct contact, or that the first and second features are in indirect contact through an intermediate medium. Furthermore, "above," "over," and "on top" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.
[0030] The inventors of this invention have discovered that the bonding force between the coupling agent layer and the matrix in the prior art is limited, which affects the bonding between the phenelzine layer and the matrix.
[0031] In this first aspect, the present invention provides an evaporation deposition apparatus for a coupling agent, comprising: The coupling agent storage section 10 is provided with a coupling agent outlet 11; The coupling agent vapor generator 20 includes a coupling agent vaporization chamber 21, a steam generator 22 is provided outside the coupling agent vaporization chamber 21, and a coupling agent inlet 23 and a coupling agent vapor outlet 24 are provided on the coupling agent vaporization chamber 21. The coupling agent inlet 23 is connected to the coupling agent outlet 11. The vacuum deposition chamber 40 has at least two coupling agent vapor inlets 41 spaced apart on its side wall. The coupling agent vapor inlets 41 are connected to the coupling agent vapor outlet 24 via a steam pipe 30. At least two branch steam pipes 32 are provided on the side of the steam pipe 30 near the coupling agent vapor inlets 41. The at least two branch steam pipes 32 are connected one-to-one with the at least two coupling agent vapor inlets 41. Valves 33 are provided on the branch steam pipes 32. The steam pipe 30 is wrapped with a heat insulation layer. During evaporation deposition, the valves 33 of each branch steam pipe 32 are opened for a preset time and then closed.
[0032] The inventors discovered that the bonding strength between the coupling agent layer and the substrate in the prior art is limited, thus affecting the bonding strength between the phenelzine layer and the substrate. Further investigation revealed that repeated heating of the coupling agent before deposition easily leads to molecular polymerization within the coupling agent. The polymerized molecules, due to their excessively long molecular chains and large molecular weight, cannot penetrate the pores on the substrate surface, reducing the anchoring effect between the coupling agent and the substrate, thereby weakening the bonding force between them. Furthermore, after vaporization, the coupling agent easily transforms from gas into small droplets, which adhere to the substrate, forming a foreign droplet on the substrate surface. The coupling agent cannot form a 'bonding' film between the phenelzine and the substrate, thus failing to function as a coupling agent and affecting the bonding force between the phenelzine layer and the substrate.
[0033] The evaporation deposition apparatus for coupling agents of the present invention provides a coupling agent storage section 10 before the coupling agent vaporization chamber 21. The coupling agent is introduced from the coupling agent storage section 10 into the coupling agent vaporization chamber 21 as needed according to the type of coupling agent and the deposition area. This avoids the coupling agent being repeatedly heated by the steam generator 22 and prevents the coupling agent molecular weight from being too large, which would prevent it from entering the pores on the surface of the substrate, thereby improving the bonding force between the coupling agent and the substrate. The steam pipe 30 between the coupling agent vapor inlet 41 and the coupling agent vapor outlet 24 is wrapped with an insulation layer to prevent the coupling agent vapor from condensing upon cooling. After the coupling agent vaporizes, it turns from gas into small droplets. These droplets easily adhere to the substrate upon reaching the deposition chamber, becoming foreign matter on the substrate surface. This prevents the coupling agent from forming a 'bonding' film between the pyrene layer and the substrate, thus failing to function as a coupling agent and affecting the bonding force between the pyrene layer and the substrate. At least two coupling agent vapor inlets 41 are spaced apart on the side wall of the vacuum deposition chamber 40. At least two branch steam pipes 32 are provided on the side of the steam pipe 30 near the coupling agent vapor inlets 41. Each branch steam pipe 32 is connected to one of the at least two coupling agent vapor inlets 41. Valves 33 are installed on the branch steam pipes 32. Since the deposition gas flows dynamically inside the deposition chamber, fresh coupling agent vapor enters through the coupling agent vapor inlet 41, and undeposited coupling agent vapor is extracted through the evacuation port 42. After a preset time, the valve 33 is opened and then closed through the branched vapor pipes 32. Coupling agent vapor is then introduced into the vacuum deposition chamber 40 through at least two spaced coupling agent vapor inlets 41 in sequence. This ensures that the coupling agent vapor is uniformly attached to the substrate surface, avoiding excessive local concentration of coupling agent gas due to diffusion and overlap. This increases the chance of coupling agent molecules colliding with each other, and the coupling agent vapor spontaneously condenses into small droplets in the vacuum deposition chamber 40. This prevents the coupling agent from forming a 'bonding' film between the pyrene layer and the substrate, thereby improving the bonding force between the pyrene layer and the substrate.
[0034] This invention significantly improves the bonding force between the pyrene layer and the substrate by setting a coupling agent storage section 10 before the coupling agent vaporization chamber 21, wrapping a heat insulation layer around the steam pipe 30 between the coupling agent vapor inlet 41 and the coupling agent vapor outlet 24, and setting at least two coupling agent vapor inlets 41 at intervals on the side wall of the vacuum deposition chamber 40. At least two branch steam pipes 32 are set on the side of the steam pipe 30 near the coupling agent vapor inlet 41, and the at least two branch steam pipes 32 are connected one-to-one with the at least two coupling agent vapor inlets 41. A valve 33 is set on the branch steam pipe 32. During evaporation deposition, the valve 33 is opened for a preset time and then closed after each branch steam pipe 32 is opened.
[0035] The polymerization growth of phenelzine is a low-temperature preferential growth mechanism. The steam pipe 30 is wrapped with an insulation layer, which can also prevent the phenelzine layer from growing inside the steam pipe 30 downstream of the solenoid valve or inside the solenoid valve during the phenelzine deposition stage after the coupling agent evaporates and deposits, thus preventing the steam pipe 30 from becoming blocked.
[0036] If at least two branch steam pipes 32 simultaneously introduce coupling agent gas into the vacuum deposition chamber 40, it cannot be guaranteed that the gas in each branch pipe is uniform. The coupling agent adheres uniformly to the substrate surface, and the coupling agent gas is prone to diffusion and overlap. The coupling agent vapor is prone to spontaneously condense into small droplets in the vacuum deposition chamber 40.
[0037] In some preferred embodiments, the coupling agent storage section 10 is provided with a desiccant container and a humidity sensor 12. The desiccant in the desiccant container removes moisture from the coupling agent storage section 10, and the humidity sensor 12 monitors the humidity inside the coupling agent storage section 10. This preferred embodiment is more conducive to preventing hydrolysis of the coupling agent before deposition. The hydrolysis process is the chemical process by which the coupling agent reacts with the substrate to form a bond, thereby improving the adhesion between the coupling agent and the substrate surface and enhancing the adhesion between the pyrene layer and the substrate.
[0038] In some preferred embodiments, the coupling agent vaporization chamber 21 is further provided with a bypass inlet and a bypass outlet. In this preferred embodiment, by bypassing the water vapor in the coupling agent vaporization chamber 21, hydrolysis of the coupling agent before deposition can be prevented, thus improving the adhesion between the coupling agent and the substrate surface, and enhancing the adhesion between the phenelzine layer and the substrate. The steam generator 22 raises the temperature inside the coupling agent vaporization chamber 21 to above the vaporization temperature of the coupling agent. The bypass evacuates the coupling agent vaporization chamber 21, preventing dead zones from existing within the chamber, which would hinder the heating and evaporation of the coupling agent, causing it to remain in a liquid state for extended periods and polymerize, thus preventing it from entering the pores on the substrate surface. This further enhances the adhesion between the coupling agent and the substrate, and improves the adhesion between the phenelzine layer and the substrate.
[0039] In some preferred embodiments, the coupling agent vaporization chamber 21 is wrapped with an insulation layer; the coupling agent vaporization chamber 21 is equipped with a liquid level sensor 25, a pressure gauge 26 and a temperature sensor 27; and a mass flow meter 31 is installed on the steam pipe 30 to control the amount of coupling agent vapor entering the vacuum deposition chamber 40. In this preferred embodiment, the coupling agent vaporization chamber 21 is equipped with a liquid level sensor 25 to control the coupling agent to enter the vaporization chamber 21 in small amounts multiple times. Even if there is uneven heating in some areas of the vaporization chamber 21, resulting in slightly higher local temperatures, the small amount of coupling agent liquid added will allow it to evaporate completely in a short time. This prevents molecular polymerization within the coupling agent from affecting the bonding force between the coupling agent layer and the substrate. A mass flow meter 31 is installed on the steam pipe 30 to control the flow rate of coupling agent vapor entering the vacuum deposition chamber 40. This prevents excessively high flow rates, which could lead to excessively high concentrations of coupling agent vapor in the vacuum deposition chamber 40, spontaneous condensation of the coupling agent vapor into small droplets, and excessively fast deposition rates that could result in a loose coupling agent layer structure. The meter can also measure the flow rate of coupling agent vapor entering the vacuum deposition chamber. The total vapor volume of 40 prevents the coupling agent from failing to deposit in certain locations on the substrate or from forming an excessively thin or thick coupling agent layer, thereby fully utilizing the coupling agent and improving the bonding force between the pyrene layer and the substrate. The coupling agent vaporization chamber 21 is equipped with a pressure gauge 26 to prevent insufficient pressure, which could affect the accurate measurement of the coupling agent vapor flow rate from the mass flow meter 31, and to prevent excessive pressure from damaging the mass flow meter 31. Inaccurate vapor flow rate measurement can lead to deviations in the total vapor volume entering the vacuum deposition chamber 40, thus affecting the full utilization of the coupling agent and the bonding force between the pyrene layer and the substrate. The coupling agent vaporization chamber 21 is also equipped with a temperature sensor 27, which further facilitates the control of molecular polymerization within the coupling agent, enhancing the bonding force between the coupling agent layer and the substrate.
[0040] In some preferred embodiments, a rotating stage is provided on the central axis of the vacuum deposition chamber 40, the rotating stage is used to support and fix the substrate, and an evacuation hole 42 is provided on the side wall of the vacuum deposition chamber 40. The angle between the evacuation hole 42 and the side of the rotating stage away from the coupling agent vapor inlet 41 is 20° to 40°. In this preferred embodiment, a rotating platform supporting the fixed substrate is set on the central axis of the vacuum deposition chamber 40. The substrate can rotate, which improves the uniformity of coupling agent deposition in the circumferential direction, preventing the inability to deposit coupling agent at certain locations in the circumferential direction or preventing the coupling agent layer from being too thin or too thick. It also prevents excessively thick local coupling agent layers caused by slightly higher coupling agent gas concentrations at certain locations in the vacuum deposition chamber 40, thus fully utilizing the coupling agent's role and improving the bonding force between the pyrelin layer and the substrate. The rotating platform on the central axis of the vacuum deposition chamber 40 also promotes the flow and diffusion of coupling agent gas within the deposition chamber, resulting in a more uniform coupling agent concentration. This prevents excessively high local coupling agent gas concentrations in the deposition chamber, which could cause the coupling agent vapor to spontaneously condense into small droplets, failing to form a 'bonding' film between the pyrelin and the substrate, thus negating the coupling agent's function and affecting the bonding force between the pyrelin layer and the substrate. Based on this, if... Figure 2 As shown, the angle between the vent 42 and the side of the rotating stage away from the coupling agent vapor inlet 41 is 20°~40°, which can be 20°, 23°, 25°, 28°, 30°, 33°, 35°, 38°, 40° and any value between them, more preferably 30°, which can further promote the diffusion of coupling agent gas, make the coupling agent concentration in the deposition cavity more uniform, and prevent the coupling agent from condensing into small droplets. The possible principle is as follows: This angled design breaks the straight path of gas from the vapor inlet to the evacuation port, forcing the coupling agent vapor to flow along a longer and more complex trajectory within the vacuum deposition chamber 40. In addition, this angle is coordinated with the spatial constraints of the pyrene inlet and the rotation direction of the substrate, ensuring that the gas diffuses naturally along the longest path in the vacuum (the coupling agent enters from the coupling agent vapor inlet 41 and gradually diffuses towards the evacuation port 42 along an arc-shaped path along the rotation direction of the substrate), further optimizing the uniformity of gas distribution. Ultimately, this allows the coupling agent to adhere uniformly to the substrate surface in gaseous form, forming a continuous and stable adhesive film, significantly improving the bonding force between the pyrene layer and the substrate.
[0041] In a second aspect, the present invention provides a method for evaporating and depositing a coupling agent in an evaporation deposition apparatus for the coupling agent described in the first aspect, comprising: placing the coupling agent in a coupling agent storage section 10; introducing dry compressed air into the coupling agent storage section 10; the coupling agent being forced into a coupling agent vaporization chamber 21 from a coupling agent outlet 11 through a coupling agent inlet 23; heating the coupling agent entering the coupling agent vaporization chamber 21 by a steam generator 22 to vaporize it into coupling agent vapor; opening valve 33 for a preset time and then closing valve 33 in a branch steam pipe 32; the coupling agent vapor entering the coupling agent vapor inlet 41 of a vacuum deposition chamber 40 from a coupling agent vapor outlet 24 through a steam pipe 30; and depositing a coupling agent layer on the substrate surface within the vacuum deposition chamber 40.
[0042] In the evaporation deposition method of the present invention, the coupling agent is placed in the coupling agent storage section 10. During evaporation deposition, the coupling agent is forced into the coupling agent vaporization chamber 21 from the coupling agent outlet 11 through the coupling agent inlet 23. The coupling agent is introduced from the coupling agent storage section 10 into the coupling agent vaporization chamber 21 as needed according to the type of coupling agent and the deposition area. This avoids the coupling agent being repeatedly heated by the steam generator 22, and prevents the coupling agent molecular weight from being too large to enter the pores on the substrate surface, thereby improving the bonding force between the coupling agent and the substrate. It also avoids the need to directly add the coupling agent into the vaporization chamber. Moisture is introduced into the coupling agent vaporization chamber 21 during coupling, causing hydrolysis of the coupling agent and thus improving the adhesion between the coupling agent layer and the substrate. The step of opening valve 33 for a preset time and then closing valve 33 in each branch steam pipe 32 ensures uniform adhesion of coupling agent vapor to the substrate surface. This avoids excessive local concentration of coupling agent gas due to diffusion and overlap, which could cause spontaneous condensation of the coupling agent gas into small droplets, preventing the coupling agent from forming a 'bonding' film between the coupling agent and the substrate, thereby improving the adhesion between the coupling agent layer and the substrate. The method of introducing compressed air into the coupling agent storage section 10 to force the coupling agent into the coupling agent vaporization chamber 21 is safer because the coupling agent is an organic liquid.
[0043] In some preferred embodiments, the method further includes: using desiccant in the desiccant container to remove moisture from the coupling agent storage section 10; and replacing and / or adding the desiccant when the humidity sensor 12 detects that the humidity in the coupling agent storage section 10 exceeds a preset value. This preferred embodiment is more conducive to preventing hydrolysis of the coupling agent before deposition, thereby improving the adhesion between the coupling agent and the substrate surface.
[0044] In some preferred embodiments, the method further includes repeating the step of removing moisture from the coupling agent vaporization chamber 21 before introducing dry compressed air into the coupling agent storage section 10. This moisture removal step includes sequentially evacuating the coupling agent vaporization chamber 21 through a bypass outlet and introducing inert gas into the coupling agent vaporization chamber 21 through a bypass inlet. In this preferred embodiment, repeatedly performing the sequential evacuation of the coupling agent vaporization chamber 21 through the bypass outlet and the introduction of inert gas into the coupling agent vaporization chamber 21 through the bypass inlet, and removing the moisture from the coupling agent vaporization chamber 21 through gas washing, further helps prevent hydrolysis of the coupling agent before deposition and improves the adhesion between the coupling agent and the substrate surface.
[0045] In some preferred embodiments, the coupling agent is controlled by the level sensor 25 to enter the coupling agent vaporization chamber 21 according to the amount of coupling agent required for each branch steam pipe 32; before switching the branch steam pipe 32, the temperature inside the coupling agent vaporization chamber 21 is increased to a temperature higher than the coupling agent vaporization temperature by the steam generator 22, and the coupling agent vaporization chamber 21 is evacuated through the bypass outlet. In this preferred embodiment, the amount of coupling agent required for each branch steam pipe 32 is controlled by the liquid level sensor 25 to allow the coupling agent to enter the coupling agent vaporization chamber 21. Even if there is uneven heating in some areas of the coupling agent vaporization chamber 21, and the temperature is higher in some areas, the coupling agent liquid can evaporate completely in a short time due to the small amount of coupling agent added. The molecular polymerization within the coupling agent will not affect the bonding force between the coupling agent layer and the substrate. Before switching the branch steam pipe 32, the temperature inside the coupling agent vaporization chamber 21 is increased to a level higher than the coupling agent vaporization temperature by the steam generator 22. The coupling agent vaporization chamber 21 is evacuated through the bypass outlet, which is more conducive to preventing the coupling agent from being difficult to heat and evaporate when there are dead corners in the coupling agent vaporization chamber 21. It will remain in liquid form for a long time and polymerize, making it unable to enter the pores on the surface of the substrate, thereby improving the bonding force between the coupling agent and the substrate, and improving the bonding force between the pyrene layer and the substrate.
[0046] Preferably, the amount of coupling agent required for each branch steam pipe 32 is divided into a predetermined number of portions, and the coupling agent is controlled by the liquid level sensor 25 to enter the coupling agent vaporization chamber 21 in the predetermined number of portions. Under this preferred scheme, it is more conducive to preventing uneven local heating in the coupling agent vaporization chamber 21, where the local temperature is higher, which would lead to molecular polymerization within the coupling agent and affect the bonding force between the coupling agent layer and the substrate.
[0047] In some preferred embodiments, the method further includes: activating the mass flow meter 31 when the pressure gauge 26 detects that the pressure inside the coupling agent vaporization chamber 21 has reached a preset pressure; and adjusting the heating power of the steam generator 22 based on the temperature sensor 27 monitoring the temperature inside the coupling agent vaporization chamber 21. In this preferred embodiment, activating the mass flow meter 31 after the pressure gauge 26 detects that the pressure inside the coupling agent vaporization chamber 21 has reached a preset pressure avoids excessively low pressure in the coupling agent vaporization chamber 21, which would affect the accuracy of the mass flow meter 31 in measuring the flow rate of steam exiting the coupling agent vaporization chamber 21 and consequently affect the total amount of steam entering the vacuum deposition chamber 40. This fully utilizes the coupling agent, improves the bonding force between the pyrene layer and the substrate, and also avoids excessive pressure that could damage the mass flow meter 31. The temperature sensor 27 monitoring the temperature inside the coupling agent vaporization chamber 21 and adjusting the heating power of the steam generator 22 based on the monitoring results further facilitates the control of molecular polymerization within the coupling agent and enhances the bonding force between the coupling agent layer and the substrate.
[0048] Thirdly, the present invention provides a coupling agent layer on a substrate surface, obtained by evaporation deposition using the coupling agent evaporation deposition apparatus described in the first aspect or the coupling agent evaporation deposition method described in the second aspect. The coupling agent layer of the present invention exhibits significantly improved adhesion to the substrate surface.
[0049] Fourthly, the present invention provides an application in the preparation of a phenelzine layer on a substrate surface, using an evaporation deposition apparatus for a coupling agent as described in the first aspect, an evaporation deposition method for a coupling agent as described in the second aspect, or a coupling agent layer as described in the third aspect. The phenelzine layer of the present invention exhibits significantly improved adhesion to the substrate surface.
[0050] The present invention will be further described in detail below with reference to specific embodiments.
[0051] Example 1 An evaporation deposition apparatus for a coupling agent includes: a coupling agent storage section 10, a coupling agent outlet 11, a desiccant containment chamber and a humidity sensor 12, wherein a desiccant in the desiccant containment chamber removes moisture from the coupling agent storage section 10, and the humidity sensor 12 monitors the humidity inside the coupling agent storage section 10. The coupling agent vapor generator 20 includes a coupling agent vaporization chamber 21, a steam generator 22 is provided outside the coupling agent vaporization chamber 21, the coupling agent vaporization chamber 21 is wrapped with a heat insulation layer, the coupling agent vaporization chamber 21 is provided with a liquid level sensor 25, a pressure gauge 26 and a temperature sensor 27, the coupling agent vaporization chamber 21 is provided with a coupling agent inlet 23 and a coupling agent vapor outlet 24, the coupling agent inlet 23 is connected to the coupling agent outlet 11, and the coupling agent vaporization chamber 21 is also provided with a bypass inlet and a bypass outlet; The vacuum deposition chamber 40 has at least two coupling agent vapor inlets 41 spaced apart on its side wall. The coupling agent vapor inlets 41 and coupling agent vapor outlets 24 are connected by a steam pipe 30. A mass flow meter 31 is installed on the steam pipe 30 to control the amount of coupling agent vapor entering the vacuum deposition chamber 40. The steam pipe 30 is wrapped with an insulation layer. At least two branch steam pipes 32 are provided on the side of the steam pipe 30 near the coupling agent vapor inlets 41. The at least two branch steam pipes 32 are connected one-to-one with the at least two coupling agent vapor inlets 41. A valve 33 is installed on the branch steam pipes 32. During evaporation deposition, the valves 33 are opened for a preset time and then closed after each branch steam pipe 32 is evacuated. A rotating platform is provided on the central axis of the vacuum deposition chamber 40 to support and fix the substrate. An evacuation hole 42 is provided on the side wall of the vacuum deposition chamber 40. The angle between the evacuation hole 42 and the side of the rotating platform away from the coupling agent vapor inlets 41 is 30°.
[0052] An evaporation deposition method for a coupling agent using the aforementioned evaporation deposition apparatus involves placing the coupling agent in a coupling agent storage unit 10 and repeatedly performing a water vapor removal step in the coupling agent vaporization chamber 21. This water vapor removal step includes sequentially evacuating the coupling agent vaporization chamber 21 through a bypass outlet, introducing an inert gas into the coupling agent vaporization chamber 21 through a bypass inlet, and introducing dry compressed air into the coupling agent storage unit 10. The coupling agent is forced into the coupling agent vaporization chamber 21 from the coupling agent outlet 11 through the coupling agent inlet 23. A steam generator 22 heats the coupling agent entering the coupling agent vaporization chamber 21, causing it to vaporize and form coupling agent vapor. When the pressure gauge 26 detects that the pressure inside the coupling agent vaporization chamber 21 has reached a preset pressure, a mass flow meter 31 is activated, and valves 33 are opened and closed sequentially through branch steam pipes 32 for a preset time. The coupling agent vapor then enters the vacuum chamber from the coupling agent vapor outlet 24 through steam pipes 30. The coupling agent vapor inlet 41 of the deposition chamber 40 deposits a coupling agent layer on the substrate surface within the vacuum deposition chamber 40. The temperature sensor 27 monitors the temperature inside the coupling agent vaporization chamber 21 and adjusts the heating power of the steam generator 22 based on the monitoring results. The desiccant in the desiccant container removes moisture from the coupling agent storage section 10. When the humidity sensor 12 detects that the humidity inside the coupling agent storage section 10 exceeds a preset value, the desiccant is replaced. The coupling agent is introduced into the coupling agent vaporization chamber 21 according to the amount of coupling agent required for each branch steam pipe 32. The amount of coupling agent required for each branch steam pipe 32 is divided into a preset number of portions. The liquid level sensor 25 controls the coupling agent to be introduced into the coupling agent vaporization chamber 21 in a preset number of portions. Before switching the branch steam pipe 32, the temperature inside the coupling agent vaporization chamber 21 is raised to a level higher than the coupling agent vaporization temperature by the steam generator 22. The coupling agent vaporization chamber 21 is evacuated through the bypass outlet. After the coupling agent is deposited, the solenoid valve between the coupling agent storage section 10 and the coupling agent vaporization chamber 21 is closed, and the bypass outlet on the coupling agent vaporization chamber 21 is opened to allow the residual coupling agent vapor in the coupling agent vaporization chamber 21 to be pumped away by the vacuum system. When the pressure in the coupling agent vaporization chamber 21 returns to atmospheric pressure, the heating device of the steam generator 22 is turned off to allow the coupling agent vaporization chamber 21 to cool down. After the vacuum system evacuates the vacuum deposition chamber 40 to the vacuum level before coupling agent deposition, the Perylene evaporation deposition process is started to deposit and grow the Perylene film.
[0053] The coupling agent is uniformly adhered to the substrate surface. The adhesion between the phenelzine layer and the substrate is tested according to the ASTM D3359 cross-cut adhesion test. The test results are graded from 0B to 5B, with higher numbers indicating stronger adhesion. The cross-cut adhesion test involves scribing lines on the coating surface according to a standard, then applying a specific adhesive tape. The adhesion is assessed by observing whether the tape can be removed from the coating. In this example, the adhesion between the phenelzine layer and the substrate is rated as 5B.
[0054] Example 2 The coupling agent evaporation deposition method of Example 1 is followed, except that the following steps are not performed: before switching the branch steam pipe 32, the temperature inside the coupling agent vaporization chamber 21 is increased to a level higher than the coupling agent vaporization temperature by the steam generator 22, and the coupling agent vaporization chamber 21 is evacuated through the bypass outlet. In this example, the test result of the bonding force between the pyrene layer and the substrate is 4B.
[0055] Example 3 The coupling agent evaporation deposition method of Example 1 was followed, except that the following steps were omitted: the amount of coupling agent required for each branch steam pipe 32 was divided into a predetermined number of portions, and the coupling agent was controlled by the liquid level sensor 25 to enter the coupling agent vaporization chamber 21 in the predetermined number of portions. In this example, the test result of the bonding force between the pyrene layer and the substrate was 4B.
[0056] Example 4 The evaporation deposition method of the coupling agent was performed according to Example 1, except that the angle between the evacuation port 42 and the side of the rotating stage away from the coupling agent vapor inlet 41 was 40°. In this example, the test result of the bonding force between the pyrene layer and the substrate was 4B.
[0057] Comparative Example 1 The evaporation deposition apparatus and method for the coupling agent were used in Example 1, except that the valves 33 on the branch steam pipes 32 were opened simultaneously, and coupling agent vapor was introduced into the vacuum deposition chamber 40 through at least two branch steam pipes 32 at the same time, instead of opening the valves 33 of each branch steam pipe 32 for a preset time and then closing them. The uniformity of the coupling agent adhesion on the substrate surface was poor, and the bonding force between the pyrene layer and the substrate was tested, with a result of 2B.
[0058] Comparative Example 2 The evaporation deposition apparatus and method for coupling agent in Example 1 were used, except that only one coupling agent vapor inlet 41 was provided on the side wall of the vacuum deposition chamber 40. The uniformity of the coupling agent on the substrate surface was poor. The bonding force between the pyrene layer and the substrate was tested, and the test result was 1B.
[0059] Compared to the comparative examples, when valves 33 on branch steam pipes 32 are opened simultaneously, coupling agent vapor is introduced into the vacuum deposition chamber 40 through at least two branch steam pipes 32, and only one coupling agent vapor inlet 41 is provided on the side wall of the vacuum deposition chamber 40, and valves 33 are closed after a preset time of opening valves 33 on each branch steam pipe 32, a uniform coupling agent bonding film can be formed on the substrate surface, improving the bonding force between the pyrene layer and the substrate. Compared to Examples 1 and 2, before switching branch steam pipes 32, the temperature inside the coupling agent vaporization chamber 21 is increased to above the coupling agent vaporization temperature by the steam generator 22, and the coupling agent vaporization chamber 21 is evacuated through the bypass outlet, which is more conducive to improving the bonding force between the pyrene layer and the substrate. Compared to Examples 1 and 3, the amount of coupling agent required for each branch steam pipe 32 is divided into a preset number of portions, and the coupling agent is controlled by the liquid level sensor 25 to enter the coupling agent vaporization chamber 21 in the preset number of portions, which is more conducive to improving the bonding force between the pyrene layer and the substrate.
[0060] The preferred embodiments of the present invention have been described in detail above; however, the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other suitable manner. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention.
Claims
1. An evaporation and deposition apparatus for a coupling agent, characterized in that, include: The coupling agent storage section is equipped with a coupling agent outlet; A coupling agent vapor generator includes a coupling agent vaporization chamber, a steam generator is provided outside the coupling agent vaporization chamber, and a coupling agent inlet and a coupling agent vapor outlet are provided on the coupling agent vaporization chamber, with the coupling agent inlet and the coupling agent outlet connected together. The vacuum deposition chamber has at least two coupling agent vapor inlets spaced apart on its sidewall. The coupling agent vapor inlets and coupling agent vapor outlets are connected by steam pipes. At least two branch steam pipes are provided on the side of the steam pipes closest to the coupling agent vapor inlets. Each of the at least two branch steam pipes is connected to one of the at least two coupling agent vapor inlets. Valves are provided on the branch steam pipes. The steam pipes are wrapped with an insulation layer. During evaporation deposition, the valves of each branch steam pipe are opened for a preset time and then closed.
2. The evaporation deposition apparatus according to claim 1, characterized in that, The coupling agent storage section is provided with a desiccant container and a humidity sensor. The desiccant in the desiccant container removes moisture from the coupling agent storage section, and the humidity sensor monitors the humidity inside the coupling agent storage section.
3. The evaporation deposition apparatus according to claim 1, characterized in that, The coupling agent vaporization chamber is also provided with a bypass inlet and a bypass outlet.
4. The evaporation deposition apparatus according to claim 1, characterized in that, The coupling agent vaporization chamber is externally wrapped with a heat insulation layer; the coupling agent vaporization chamber is equipped with a liquid level sensor, a pressure gauge and a temperature sensor; the steam pipe is equipped with a mass flow meter to control the amount of coupling agent vapor entering the vacuum deposition chamber.
5. The evaporation deposition apparatus according to claim 1, characterized in that, A rotating stage is provided on the central axis of the vacuum deposition chamber. The rotating stage is used to support and fix the substrate. An evacuation hole is provided on the side wall of the vacuum deposition chamber. The angle between the evacuation hole and the side of the rotating stage away from the coupling agent vapor inlet is 20°~40°.
6. A method for evaporating and depositing a coupling agent using an evaporation deposition apparatus for the coupling agent according to any one of claims 1 to 5, characterized in that, include: The coupling agent is placed in the coupling agent storage compartment, and dry compressed air is introduced into the coupling agent storage compartment. The coupling agent is forced into the coupling agent vaporization chamber from the coupling agent outlet through the coupling agent inlet. The steam generator heats the coupling agent entering the coupling agent vaporization chamber to vaporize it into coupling agent vapor. The valves of the branch steam pipes are opened for a preset time and then closed. The coupling agent vapor enters the coupling agent vapor inlet of the vacuum deposition chamber from the coupling agent vapor outlet through the steam pipe, and a coupling agent layer is deposited on the substrate surface in the vacuum deposition chamber.
7. The evaporation deposition method according to claim 6, characterized in that, Also includes: The desiccant in the desiccant container removes moisture from the coupling agent storage section. When the humidity sensor detects that the humidity in the coupling agent storage section exceeds a preset value, the desiccant is replaced and / or added.
8. The evaporation deposition method according to claim 6, characterized in that, Also includes: Before introducing dry compressed air into the coupling agent storage section, the process of removing moisture from the coupling agent vaporization chamber is repeated. The moisture removal process includes sequentially evacuating the coupling agent vaporization chamber through the bypass outlet and introducing inert gas into the coupling agent vaporization chamber through the bypass inlet.
9. The evaporation deposition method according to claim 6, characterized in that, According to the amount of coupling agent required for each branch steam pipe, the coupling agent is controlled by the liquid level sensor to enter the coupling agent vaporization chamber; before switching the branch steam pipe, the temperature in the coupling agent vaporization chamber is increased to a level higher than the coupling agent vaporization temperature by the steam generator, and the coupling agent vaporization chamber is evacuated through the bypass outlet.
10. The evaporation deposition method according to claim 9, characterized in that, The amount of coupling agent required for each branch steam pipe is divided into a preset number of portions, and the coupling agent is controlled by a liquid level sensor to enter the coupling agent vaporization chamber in the preset number of portions.
11. The evaporation deposition method according to claim 6, characterized in that, Also includes: Once the barometer detects that the pressure inside the coupling agent vaporization chamber has reached the preset pressure, the mass flow meter is activated. A temperature sensor monitors the temperature inside the coupling agent vaporization chamber, and adjusts the heating power of the steam generator based on the monitoring results.
12. A coupling agent layer on the surface of a substrate, characterized in that, It is obtained by evaporation deposition using the evaporation deposition apparatus of the coupling agent according to any one of claims 1 to 5 or the evaporation deposition method of the coupling agent according to any one of claims 6 to 11.
13. An application in the process of preparing a phenelzine layer on a substrate surface, characterized in that, The application is based on the evaporation deposition apparatus of the coupling agent according to any one of claims 1 to 5, or the evaporation deposition method of the coupling agent according to any one of claims 6 to 11, or the coupling agent layer according to claim 12.
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