High-performance aluminum reflecting film and preparation method thereof

Through the preparation method of multi-layer structure and vacuum annealing treatment, the problem of insufficient reflectivity and adhesion of the aluminum reflective film is solved, the optical performance and stability of the aluminum reflective film are improved, and it is suitable for a wider range of optical applications.

CN120577907APending Publication Date: 2025-09-02SUZHOU TULANE ELECTRIC TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510767166.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-10
Publication Date
2025-09-02

AI Technical Summary

Technical Problem

Traditional aluminum reflective films have shortcomings in reflectivity, adhesion and weather resistance, which affects its performance and stability in high-end optical applications.

Method used

The multi-layer structural design is adopted, including a substrate, a first metal layer, a second metal layer, a first protective layer and a second protective layer. The aluminum oxide protective layer is formed by in-situ oxidation, and combined with vacuum annealing treatment, the preparation process is optimized to improve reflectivity and adhesion.

Benefits of technology

The reflectivity and adhesion of the aluminum reflective film is significantly improved, its performance in the visible to infrared spectral range is enhanced, weather resistance is improved, and application range is expanded.

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Abstract

The invention discloses a high-performance aluminum reflecting film, which comprises a substrate, a first metal layer, a second metal layer, a first protective layer and a second protective layer, and is characterized in that the first metal layer is deposited on the substrate, the second metal layer is deposited on the first metal layer, and the second metal layer is subjected to in-situ oxidation to form the first protective layer; and preparing a second protective layer on the first protective layer, obtaining a deposited film, and carrying out vacuum annealing treatment to form a stable and reliable high-performance aluminum reflecting film, the method for depositing the aluminum oxide film protective layer in situ is provided, so that the overall performance of the high-performance aluminum reflecting film is greatly improved, the reflecting capacity is enhanced, and the service life of the aluminum reflecting film is prolonged. According to the high-performance aluminum reflecting film, the reflectivity of the high-performance aluminum reflecting film in the range from visible light to infrared spectrum is remarkably improved, and the adhesive force of the aluminum film and the substrate is also improved, so that the stability and durability of the film layer are ensured, the adhesive force of the second protective layer on the first protective layer is improved, and the application range of the high-performance aluminum reflecting film is expanded.
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Description

Technical Field

[0001] The present invention relates to the field of aluminum reflective films, and in particular to a high-performance aluminum reflective film and a preparation method thereof. Background Art

[0002] Aluminum high-performance reflective films are widely used in the optical field due to their excellent optical properties, such as in key components such as mirrors and optical coatings.

[0003] Traditional aluminum reflective film preparation technology often faces some challenges, such as suboptimal reflectivity, insufficient adhesion, and poor weather resistance. After the aluminum film is prepared, the vacuum is broken for subsequent thin film deposition, which greatly affects the quality of the aluminum film. These problems limit the potential of aluminum film in higher-end optical applications.

[0004] In the prior art, the utility model patent application number 2022205040950 discloses an optical aluminum reflective film, which has an anti-corrosion effect by adding neodymium to aluminum. However, the reflectivity of aluminum and neodymium is different, which affects the improvement of the reflectivity of the aluminum reflective film. Moreover, the silica protective layer is only a simple coating, and its protective effect on the surface of the aluminum-neodymium alloy layer is relatively limited, which needs to be improved. Summary of the Invention

[0005] The main technical problem solved by the present invention is to provide a high-performance aluminum reflective film and a preparation method thereof, thereby improving the reflectivity, enhancing the adhesion of the aluminum film and the protective effect on the aluminum film.

[0006] In order to solve the above technical problems, a technical solution adopted by the present invention is: to provide a high-performance aluminum reflective film, including: a substrate, a first metal layer, a second metal layer, a first protective layer and a second protective layer, the first metal layer is deposited on the substrate, the second metal layer is deposited on the first metal layer, the first protective layer is in-situ oxidized to form on the surface of the second metal layer, the second metal layer is made of aluminum thin film, and the second protective layer is arranged on the surface of the first protective layer.

[0007] In a preferred embodiment of the present invention, the substrate is a glass layer or a metal layer.

[0008] In a preferred embodiment of the present invention, the first metal layer is a chromium thin film or a titanium thin film.

[0009] In a preferred embodiment of the present invention, the second protective layer is made of lithium fluoride, magnesium fluoride, a metal fluoride composite film or a metal oxide.

[0010] In a preferred embodiment of the present invention, the thickness of the first metal layer is 8-12 nanometers.

[0011] To solve the above technical problems, the present invention adopts a technical solution: providing a method for preparing an aluminum reflective film, comprising the following steps: a. Provide a substrate and clean it to remove oil, dirt and impurities; b. depositing a first metal layer on the substrate; c. depositing a second metal layer on the first metal layer; d. performing in-situ oxidation on the second metal layer to form a first protective layer; f. forming a second protective layer on the first protective layer to obtain a deposited thin film; e. The deposited thin film is subjected to vacuum annealing treatment to form a stable and reliable high-performance aluminum reflective film.

[0012] In a preferred embodiment of the present invention, the deposition method of the first metal layer includes physical vapor deposition techniques such as electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering, and the deposition method of the second metal layer includes physical vapor deposition techniques such as electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering, and the vacuum degree is required to be less than 10 -4 Pa.

[0013] In a preferred embodiment of the present invention, the purity of aluminum in the second metal layer is higher than 99.99%, and the deposition rate of the second metal layer is lower than 1 nm / s.

[0014] In a preferred embodiment of the present invention, the thickness of the first protective layer is 4-6 nanometers, and the thickness of the second protective layer is 5-20 nanometers.

[0015] In a preferred embodiment of the present invention, the vacuum annealing process comprises the following steps: In a vacuum environment, the deposited film is heated to 300°C, kept at this temperature for n hours, and then allowed to cool naturally to room temperature.

[0016] The beneficial effects of the present invention are: a high-performance aluminum reflective film and a preparation method thereof pointed out by the present invention, through careful optimization of the preparation process and innovative material combination, proposes a method of in-situ deposition of an aluminum oxide thin film protective layer, so that the overall performance of the high-performance aluminum reflective film is greatly improved, not only the reflection ability is enhanced, so that its reflectivity in the visible light to infrared spectrum range is significantly improved, but also the adhesion of the aluminum film to the substrate is improved, thereby ensuring the stability and durability of the film layer. In addition, by introducing new protective layer technology and surface treatment methods, the adhesion of the second protective layer on the first protective layer is improved, and the weather resistance is also enhanced, so that it can better resist the erosion of environmental factors such as humidity, temperature changes and ultraviolet radiation, which not only expands the application range of high-performance aluminum reflective films, but also improves their performance and reliability in various optical systems, thereby bringing new possibilities for the development of the optical field. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. Those skilled in the art can also derive other drawings based on these drawings without inventive work, among which: Figure 1 It is a structural schematic diagram of a preferred embodiment of a method for preparing an aluminum reflective film of the present invention; Figure 2 This is a schematic structural diagram of a substrate used in a method for preparing an aluminum reflective film according to the present invention; Figure 3 This is a schematic structural diagram of a method for preparing an aluminum reflective film according to the present invention, in which a first metal layer is deposited on a substrate; Figure 4 It is a structural schematic diagram of a method for preparing an aluminum reflective film according to the present invention, in which a second metal layer is deposited on a first metal layer; Figure 5 It is a schematic structural diagram of a first protective layer formed by in-situ oxidation of a second metal layer in a method for preparing an aluminum reflective film according to the present invention; Figure 6 It is a structural schematic diagram of a second protective layer formed on a first protective layer in a method for preparing an aluminum reflective film of the present invention; Figure 7 The present invention is a schematic structural diagram of a high-performance aluminum reflective film subjected to vacuum annealing treatment in a method for preparing the aluminum reflective film. DETAILED DESCRIPTION

[0018] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0019] See also Figures 1 to 7 , embodiments of the present invention include: like Figures 2 to 7 The high-performance aluminum reflective film shown includes: a substrate 101, a first metal layer 201, a second metal layer 301, a first protective layer 401 and a second protective layer 501. In this embodiment, the substrate 101 is made of a glass layer or a metal layer, and the size and shape of the substrate 101 can be cut according to needs.

[0020] The first metal layer 201 is deposited on the substrate 101, and the second metal layer 301 is deposited on the first metal layer 201. In this embodiment, the second metal layer 301 is made of an aluminum film, and the first metal layer 201 is made of a chromium film or a titanium film. The chromium film and the titanium film have high adhesion performance and chemical stability, and both have good adhesion and compatibility with the aluminum film and the substrate 101.

[0021] The thickness of the first metal layer 201 is controlled to be about 10 nanometers, which does not affect the deposition of the second metal layer 301 and can improve the overall adhesion strength.

[0022] like Figure 5 As shown, the first protective layer 401 is formed by in-situ oxidation on the surface of the second metal layer 301. The aluminum film is subjected to in-situ oxidation to form a dense aluminum oxide protective layer, namely the first protective layer 401. In-situ oxidation is performed on the surface of the deposited aluminum film (a few nanometers thick), and the first protective layer 401 can be directly formed during the deposition process.

[0023] The first protective layer 401 can be oxidized using pure oxygen or mixed oxygen. By varying the oxidation pressure and duration, the thickness of the aluminum oxide protective layer can be precisely adjusted, allowing the thickness of the first protective layer 401 to be controlled to approximately 5 nanometers. In-situ oxidation of the surface of the second metal layer 301 not only improves its adhesion to subsequent protective layers and the reflectivity of the aluminum film, but also protects the core aluminum film, preventing the vacuum-deposited protective layer from breaking and affecting the properties of the aluminum reflective film.

[0024] The second protective layer 501 is disposed on the surface of the first protective layer 401. In this embodiment, the second protective layer 501 is made of lithium fluoride, magnesium fluoride, a metal fluoride composite film, or a metal oxide, which exhibits excellent weather resistance and optical properties. The second protective layer 501 can be a single layer or a multilayer film, with a thickness of 5 to 20 nanometers, to reduce light scattering and further improve reflectivity.

[0025] A method for preparing an aluminum reflective film comprises the following steps: a. providing a substrate 101 and cleaning the substrate to remove oil stains and impurities; like Figure 2 As shown, the cleaning process of the substrate 101 may adopt ultrasonic cleaning, chemical cleaning and / or plasma cleaning to ensure the cleanliness of the surface of the substrate 101; b. Figure 3 As shown, chromium (Cr) or titanium (Ti) material is selected and deposited on the substrate 101 to obtain a first metal layer 201 with a thickness of 10 nanometers; c. Figure 4 As shown, an aluminum film, i.e., a second metal layer 301, is deposited on the first metal layer 201. To improve the reflectivity and roughness of the aluminum film, the purity of the aluminum film is higher than 99.99%. At the same time, by controlling deposition parameters such as power, gas flow rate, and pressure, the deposition rate of the second metal layer is ensured to be lower than 1 nm / s, thereby improving the uniformity and density of the aluminum film and thus enhancing its optical performance. In this embodiment, the deposition method of the first metal layer 201 includes physical vapor deposition techniques such as electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering. The deposition method of the second metal layer 301 includes physical vapor deposition techniques such as electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering. The selection is flexible and the vacuum degree requirement is less than 10 -4 Pa; d. Figure 5 As shown, in-situ oxidation is performed on the second metal layer 301 to form a dense aluminum oxide protective layer, namely the first protective layer 401. Since the first protective layer 401 is formed by in-situ oxidation directly during the deposition process of the second metal layer 301, it has a stable structure, high adhesion strength, good protection for the second metal layer 301, and does not affect the emissivity of the second metal layer 301. f. Figure 6 As shown, a second protective layer 501 is formed on the first protective layer 401 to obtain a deposited thin film. The second protective layer 501 is made of a material with good weather resistance and optical properties, such as lithium fluoride (LiF), magnesium fluoride (MgF), a metal fluoride composite film or a metal oxide, with a thickness of 5-20 nm, which is beneficial to reducing light scattering and further improving reflectivity. e. Figure 7 As shown, the deposited film is subjected to vacuum annealing treatment. In a vacuum environment, the deposited film is heated to 300°C, kept warm for 1 hour, and then allowed to cool naturally to room temperature to form a stable and reliable high-performance aluminum reflective film. By precisely controlling the annealing temperature and time, the microstructure of the film layer can be optimized to ensure its stability and reliability in various application environments. The residual stress in the high-performance aluminum reflective film can be reduced, the surface flatness can be improved, and the film defects can be improved, thereby improving the reflectivity and weather resistance.

[0026] In summary, the high-performance aluminum reflective film and its preparation method pointed out in the present invention greatly improve the optical performance, and the reflectivity in the visible light to infrared spectrum range is significantly improved. By introducing the first metal layer, the adhesion between the aluminum film and the substrate is enhanced. On the basis of the multi-layer protective structure, the vacuum annealing technology is introduced, so that the overall weather resistance is significantly improved, and it can maintain stable performance in harsh environments, and has a wider range of applications.

[0027] The above are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A high-performance aluminum reflective film, characterized in that: include: A substrate, a first metal layer, a second metal layer, a first protective layer and a second protective layer, wherein the first metal layer is deposited on the substrate, the second metal layer is deposited on the first metal layer, the first protective layer is in-situ oxidized to form a surface of the second metal layer, the second metal layer is made of an aluminum film, and the second protective layer is arranged on the surface of the first protective layer.

2. The high-performance aluminum reflective film according to claim 1, characterized in that: The substrate is a glass layer or a metal layer.

3. The high-performance aluminum reflective film according to claim 1, characterized in that: The first metal layer is a chromium thin film or a titanium thin film.

4. The high-performance aluminum reflective film according to claim 1, characterized in that: The second protective layer is made of lithium fluoride, magnesium fluoride, a metal fluoride composite film or a metal oxide.

5. The high performance aluminum reflective film according to claim 1, characterized in that: The thickness of the first metal layer is 8-12 nanometers.

6. A method for preparing an aluminum reflective film, used for preparing the high-performance aluminum reflective film according to any one of claims 1 to 5, characterized in that: The following steps are involved: a. Provide a substrate and clean it to remove oil, dirt and impurities; b. depositing a first metal layer on the substrate; c. depositing a second metal layer on the first metal layer; d. performing in-situ oxidation on the second metal layer to form a first protective layer; f. forming a second protective layer on the first protective layer to obtain a deposited thin film; e. The deposited thin film is subjected to vacuum annealing treatment to form a stable and reliable high-performance aluminum reflective film.

7. The method for preparing an aluminum reflective film according to claim 6, wherein: The deposition methods of the first metal layer include electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering, and the deposition methods of the second metal layer include electron beam evaporation, thermal evaporation, ion beam sputtering and magnetron sputtering.

8. The method for preparing an aluminum reflective film according to claim 6, wherein: The purity of aluminum in the second metal layer is higher than 99.99%, and the deposition rate of the second metal layer is lower than 1 nm / s.

9. The method for preparing an aluminum reflective film according to claim 6, wherein: The thickness of the first protective layer is 4-6 nanometers, and the thickness of the second protective layer is 5-20 nanometers.

10. The method for preparing an aluminum reflective film according to claim 6, wherein: The vacuum annealing process comprises the following steps: In a vacuum environment, the deposited film is heated to 300°C, kept at this temperature for n hours, and then allowed to cool naturally to room temperature.