Oxygen catheter for vacuum coating and method for preventing aluminum from being deposited on surface of oxygen catheter of vacuum evaporation equipment

Abstract

The invention provides an oxygen catheter for vacuum coating, which comprises a hollow oxygen catheter body, and the hollow oxygen catheter body is made of a high-temperature-resistant ceramic material. In this way, the hollow oxygen catheter body is made of the high-temperature ceramic material, so that the high-temperature characteristic and the firm characteristic can be both considered.

Description

Technical Field

[0001] The present invention relates to the technical field of vacuum evaporation coating, and particularly relates to an oxygen delivery pipe for vacuum coating and a method for preventing aluminum deposition on the surface of the oxygen delivery pipe of a vacuum evaporation coating device. Background Art

[0002] In a vacuum evaporation coating device, especially in the process of producing a composite aluminum current collector, it is necessary to first evaporate and deposit aluminum oxide on the surface of a thin film. Specifically, the formation of aluminum oxide is to first evaporate aluminum to form aluminum vapor, and then introduce oxygen near the thin film to turn the aluminum into aluminum oxide and form it on the thin film. However, the existing oxygen delivery pipes for introducing oxygen are not resistant to high temperatures, and when removing aluminum or aluminum oxide residues on the surface of the oxygen delivery pipe, the existing oxygen delivery pipes are prone to cracking, resulting in increased costs. Summary of the Invention

[0003] In view of the deficiencies of the above-mentioned prior art, on the one hand, the purpose of the present invention is to provide an oxygen delivery pipe for vacuum coating to solve the problems that the existing oxygen delivery pipes in the background art are not resistant to high temperatures and are prone to cracking.

[0004] In order to achieve the above purpose, the present invention adopts the following technical solutions: An oxygen delivery pipe for vacuum coating includes a hollow oxygen delivery pipe body, and the material of the hollow oxygen delivery pipe body is a high-temperature-resistant ceramic material. In this way, since the hollow oxygen delivery pipe body adopts a high-temperature ceramic material, it can take into account both high-temperature characteristics and firm characteristics.

[0005] In the present invention, the wall thickness of the hollow oxygen delivery pipe body is 2 mm - 4 mm, and the inner diameter is 6 mm - 8 mm.

[0006] In the present invention, the oxygen delivery pipe for vacuum coating further includes a low surface energy coating, and the low surface energy coating covers the surface of the hollow oxygen delivery pipe body.

[0007] In the present invention, the low surface energy coating is a boron nitride coating, a graphite coating, a silicon carbide or a silicon nitride coating.

[0008] In the present invention, the low surface energy coating is a soft transition layer, and the soft transition layer is one or more of soft metals and their alloys, layered solid lubricating materials, graphite-based materials, fluoride ceramics or organic-inorganic composite materials.

[0009] In the present invention, a surface structure modification layer is further provided on the hollow oxygen delivery pipe body.

[0010] In the present invention, the thickness of the low surface energy coating is 0.1 μm - 5 μm, and the surface roughness Ra ≤ 0.1 μm, which is prepared by a chemical vapor deposition or plasma spraying process.

[0011] On the other hand, the present invention also provides a method for preventing aluminum deposition on the surface of the oxygen delivery pipe of a vacuum evaporation coating device, including the following steps: Step S1, forming a low surface energy coating on the surface of the hollow oxygen delivery pipe body to obtain an oxygen delivery pipe for vacuum coating.

[0012] In the present invention, after the step S1, there is also a step S2, and the step S2 is: in the vacuum evaporation coating process, by controlling the ratio of the oxygen flow rate to the aluminum evaporation rate to be 1:5 - 1:20, and maintaining the temperature of the oxygen delivery pipe at 200°C - 500°C, to inhibit the deposition of aluminum or aluminum oxide on the surface of the oxygen delivery pipe.

[0013] On the other hand, the present invention also provides a vacuum evaporation coating device, including any one of the above-mentioned oxygen delivery pipes for vacuum coating, and the control system of the device is configured to: dynamically adjust the oxygen flow rate according to the real-time power of the aluminum evaporation source, so that the oxygen partial pressure is maintained within the range of 1×10 -3 Pa - 5×10 -2 Pa.

[0014] Compared with the prior art, the oxygen delivery pipe for vacuum coating of the present invention includes a hollow oxygen delivery pipe body, and the material of the hollow oxygen delivery pipe body is a high-temperature resistant ceramic material. In this way, since the hollow oxygen delivery pipe body adopts a high-temperature ceramic material, it can take into account both high-temperature characteristics and strong characteristics. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is a flowchart of the method for preventing aluminum deposition on the surface of the oxygen delivery pipe of a vacuum evaporation coating device provided by the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0016] In order to make the purpose, technical solutions and effects of the present invention clearer and more definite, the following further describes the present invention in detail with reference to the accompanying drawings and by way of examples. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0017] It should be noted that when a component is referred to as being "mounted on", "fixed to" or "disposed on" another component, it can be directly on the other component or there may be an intermediate component at the same time. When a component is referred to as being "connected to" another component, it can be directly connected to the other component or there may be an intermediate component at the same time.

[0018] It should also be noted that the terms of orientation such as left, right, up, and down in the embodiments of the present invention are only relative concepts to each other or are referenced based on the normal use state of the product, and should not be considered restrictive.

[0019] Due to the special high-temperature environment where the oxygen delivery tube is located, the existing oxygen delivery tubes for vacuum coating will experience slight bending during use due to high temperature. This slight bending will cause a slight deviation in the oxygen delivered by the oxygen delivery tube, ultimately affecting the composition of the material formed on the thin film and the physical and chemical properties of the product. More importantly, during the process of evaporating metals such as aluminum, aluminum will form on the oxygen delivery tube. The aluminum slag formed on the oxygen delivery tube is processed by manual removal. However, the existing oxygen delivery tubes will rupture during the process of removing the aluminum slag. For this reason, the inventor has proposed an oxygen delivery tube for vacuum coating. The oxygen delivery tube for vacuum coating includes a hollow oxygen delivery tube body, and the material of the hollow oxygen delivery tube body is a high-temperature-resistant ceramic material. In this way, since the hollow oxygen delivery tube body uses a high-temperature ceramic material, it can take into account both high-temperature characteristics and strong characteristics. Preferably, the hollow oxygen delivery tube body is a hollow cylindrical object with a wall thickness of 2 mm - 4 mm and an inner diameter of 6 mm - 8 mm. With this combination of wall thickness and inner diameter, on the one hand, it can ensure the strength of the hollow oxygen delivery tube body, and on the other hand, it is also suitable for the formation of aluminum oxide on the surface of the composite aluminum current collector. Here, the strength not only refers to the strength of the oxygen delivery tube during the process of removing aluminum slag, but also refers to the pressure generated by oxygen on the oxygen delivery tube during the oxygen delivery process.

[0020] Furthermore, in the present invention, the oxygen delivery tube for vacuum coating further includes a ceramic oxygen delivery tube body and a low surface energy coating, and the coating covers the surface of the ceramic oxygen delivery tube body. This is because during the process of vacuum evaporating aluminum, aluminum will form on the oxygen delivery tube. If not cleaned, the aluminum on the oxygen delivery tube will fall off during the evaporation process, and may fall into the evaporation boat or crucible, causing the aluminum metal liquid in the evaporation boat or crucible to splash. The splashing liquid may form on the thin film and burn through the thin film. Therefore, the inventor has provided a low surface energy coating on the ceramic oxygen delivery tube body. Specifically, the low surface energy coating can be formed on the ceramic oxygen delivery tube body by vacuum coating or can also be formed on the ceramic oxygen delivery tube body by coating or spraying, etc. That is, the way the low surface energy coating is formed on the ceramic oxygen delivery tube body is arbitrary and existing. Preferably, the low surface energy coating is a boron nitride coating, a graphite coating, a silicon carbide or a silicon nitride coating. The boron nitride coating has low surface energy, high lubricity and high temperature stability, which can reduce the adhesion of aluminum, and its layered structure is similar to that of graphite, and the deposits are easy to peel off. The graphite coating has high temperature resistance and self-lubricity. High temperature resistance can prevent it from softening, melting or decomposing, so as to maintain the integrity of the coating structure. Self-lubricity means that by reducing the surface energy and promoting the peeling of deposits, on the one hand, it can reduce the aluminum formed on the graphite coating, and on the other hand, even if aluminum forms on the graphite coating, it can be easily peeled off. For the silicon carbide or silicon nitride coating, due to its high temperature resistance and low reactivity with aluminum, it can inhibit chemical bonding, and thus can reduce or even prevent aluminum from forming on the oxygen delivery tube for vacuum coating.

[0021] Furthermore, in the present invention, the low surface energy coating is a soft transition layer, and the soft transition layer is one or more of soft metals and their alloys, layered solid lubricating materials, graphite-based materials, fluoride ceramics, or organic-inorganic composite materials. Due to the significant difference in the thermal expansion coefficients between the soft transition layer material and the ceramic substrate, during the evaporation process, the oxygen delivery pipe expands when heated, and when cooled, the soft layer and the ceramic substrate shrink to different extents, generating shear stress at the interface, which causes the aluminum dross to peel off from the surface of the soft transition layer. Specifically, the soft metals and their alloys can be silver, indium, or tin-based alloys or aluminum thin layers, and the layered solid lubricating materials can be boron nitride or molybdenum disulfide. The graphite-based material can be a high-purity graphite coating. The fluoride ceramic can be calcium fluoride or magnesium fluoride. The organic-inorganic composite material can be a polyimide-boron nitride composite coating, etc. Preferably, a surface structure modification layer is further provided on the ceramic oxygen delivery pipe body. By reducing the surface roughness of the ceramic oxygen delivery pipe body, the adhesion points are reduced. The surface structure modification layer can be formed on the ceramic oxygen delivery pipe body by precision polishing. Preferably, the thickness of the low surface energy coating is 0.1 μm to 5 μm, and the surface roughness Ra ≤ 0.1 μm, which is prepared by chemical vapor deposition or plasma spraying process. Such thickness and roughness can reduce costs on the one hand and reduce the adhesion of aluminum on the other hand.

[0022] On the other hand, the present invention also provides a method for preventing aluminum deposition on the surface of the oxygen delivery pipe of a vacuum evaporation device, as Figure 1As shown, it includes the following steps: Step S1, forming a low surface energy coating on the surface of the hollow oxygen delivery tube body to obtain an oxygen delivery tube for vacuum coating. By setting the low surface energy coating, the adhesion of aluminum can be reduced. Preferably, after step S1, there is also step S2, and step S2 is: in the vacuum evaporation process, by controlling the ratio of the oxygen flow rate to the aluminum evaporation rate to be 1:5 - 1:20, and maintaining the temperature of the oxygen delivery tube at 200 - 500 °C, to inhibit the deposition of aluminum or aluminum oxide on the surface of the oxygen delivery tube. Through step S2, the deposition of aluminum or aluminum oxide on the surface of the oxygen delivery tube can be further prevented. In the present invention, controlling the ratio of the oxygen flow rate to the aluminum evaporation rate to be 1:5 - 1:20 can reduce or even avoid the formation of aluminum on the surface of the oxygen delivery tube. This is because if the ratio < 1:20, the oxygen input on the surface is insufficient, indicating that the aluminum vapor is not fully oxidized, and the remaining aluminum atoms are likely to condense and deposit on the surface of the oxygen delivery tube. If the ratio > 1:5, it indicates that the oxygen is excessive, which may affect the vacuum degree in the vacuum coating equipment. In addition, maintaining the temperature of the oxygen delivery tube at 200 °C - 500 °C aims to regulate the phase state and adhesion of aluminum oxide. When the temperature is lower than 200 °C, aluminum oxide is deposited in an amorphous or loose porous structure, with strong adhesion and difficult to remove. When the temperature is in the range of 200 °C - 500 °C, aluminum oxide crystallizes into dense α-aluminum oxide or γ-aluminum oxide, with a weak bonding force with the tube wall and is easy to remove.

[0023] Furthermore, the present invention also provides a vacuum evaporation device, including an oxygen delivery tube for vacuum coating, and the control system of the device is configured to: dynamically adjust the oxygen flow rate according to the real-time power of the aluminum evaporation source, so that the oxygen partial pressure is maintained within the range of 1×10-3 Pa - 5×10-2 Pa. The vacuum evaporation device using the oxygen delivery tube for vacuum coating can reduce the adhesion of aluminum on the oxygen delivery tube, and maintaining the oxygen partial pressure within the range of 1×10-3 Pa - 5×10-2 Pa makes the aluminum oxide formed on the film mainly γ-aluminum oxide, with a grain size of 2 nm - 5 nm, so that the obtained aluminum oxide film is dense and has few defects. The oxygen partial pressure here refers to the pressure component generated by oxygen alone in the vacuum system.

[0024] In summary, the present invention provides an oxygen delivery tube for vacuum coating, including a hollow oxygen delivery tube body, and the material of the hollow oxygen delivery tube body is a high-temperature resistant ceramic material. In this way, since the hollow oxygen delivery tube body uses a high-temperature ceramic material, the high-temperature characteristics and firm characteristics can be taken into account.

[0025] It can be understood that for those of ordinary skill in the art, equivalent substitutions or changes can be made according to the technical solutions and inventive concepts of the present invention, and all such changes or substitutions should fall within the protection scope of the appended claims of the present invention.

Claims

1. An oxygen supply tube for vacuum coating, characterized in that: It comprises a hollow oxygen delivery tube body, and the hollow oxygen delivery tube body is made of high-temperature resistant ceramic material.

2. The oxygen supply tube for vacuum coating according to claim 1, characterized in that: The wall thickness of the hollow oxygen supply tube body is 2mm-4mm, and the inner diameter is 6mm-8mm.

3. The oxygen supply pipe for vacuum coating according to claim 1, characterized in that: The oxygen supply tube for vacuum coating further comprises a low surface energy coating, and the low surface energy coating covers the surface of the hollow oxygen supply tube body.

4. The oxygen supply pipe for vacuum coating according to claim 3, characterized in that: The low surface energy coating is a boron nitride coating, a graphite coating, a silicon carbide coating or a silicon nitride coating.

5. The oxygen supply pipe for vacuum coating according to claim 3, characterized in that: The low surface energy coating is a soft transition layer, and the soft transition layer is one or more of soft metals and their alloys, layered solid lubricating materials, graphite-based materials, fluoride ceramics or organic-inorganic composite materials.

6. The oxygen supply tube for vacuum coating according to claim 1, characterized in that: A surface structure modification layer is also arranged on the hollow oxygen supply pipe body.

7. The oxygen supply pipe for vacuum coating according to claim 3, characterized in that: The low surface energy coating has a thickness of 0.1 μm-5 μm and a surface roughness Ra≤0.1 μm, and is prepared by chemical vapor deposition or plasma spraying process.

8. A method for preventing aluminum from being deposited on the surface of an oxygen delivery pipe of a vacuum evaporation equipment, characterized in that: The following steps are involved: Step S1, forming a layer of low surface energy coating on the surface of the hollow oxygen delivery tube body to obtain an oxygen delivery tube for vacuum coating.

9. The method for preventing aluminum from being deposited on the surface of the oxygen delivery pipe of vacuum evaporation equipment according to claim 8, characterized in that: The method further includes step S2, wherein the step S2 is: in the vacuum evaporation process, the ratio of oxygen flow rate to aluminum evaporation rate is controlled to be 1:5-1:20, and the temperature of the oxygen supply pipe is maintained at 200°C-500°C to inhibit the deposition of aluminum or aluminum oxide on the surface of the oxygen supply pipe.

10. A vacuum evaporation device, characterized in that: The vacuum coating oxygen supply tube comprises any one of claims 1 to 7, and the control system of the device is configured to dynamically adjust the oxygen flow rate according to the real-time power of the aluminum evaporation source so that the oxygen partial pressure is maintained at 1×10 -3 Pa-5×10 -2 Pa range.

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