A high-transmittance thin film with antireflection and its preparation method

By preparing doped layers of titanium dioxide and silicon dioxide and silicon dioxide layer on glass substrate, the problems of low deposition rate and cumbersome operation of anti-reflection and high-transmittance thin films in the prior art are solved, and the effect of high transmittance and low cost anti-reflection and high-transmittance thin films is achieved.

CN119144925BActive Publication Date: 2026-06-02CNBM RESEARCH INSTITUTE FOR ADVANCED GLASS MATERIALS GROUP CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
CNBM RESEARCH INSTITUTE FOR ADVANCED GLASS MATERIALS GROUP CO LTD
Filing Date
2024-08-15
Publication Date
2026-06-02

AI Technical Summary

Technical Problem

In existing technologies, the antireflection and high transmittance films prepared by chemical vapor deposition have low deposition rates and poor wear resistance, while the films prepared by magnetron sputtering have a large number of layers and are cumbersome to operate.

Method used

The thin film is prepared by magnetron sputtering by sequentially depositing a titanium dioxide doped layer and a silicon dioxide layer on a glass substrate. The combination of titanium dioxide and silicon dioxide layers with specific refractive indices and thicknesses achieves the anti-reflection effect of the thin film.

Benefits of technology

A high-transmittance antireflective film was achieved, with a transmittance of 99.5% at 500nm and an average transmittance of over 97.4% in the 500nm-600nm range. The process is simple and the cost is low.

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Abstract

This invention relates to an antireflective and high-transmittance thin film and its preparation method, characterized in that: (1) ordinary glass is selected as the substrate, and ultrasonically cleaned sequentially with acetone, alcohol, and deionized water, and then dried; (2) the glass is placed on a sample holder, and the target material is bombarded with Ar ions, with the vacuum degree controlled at 2.0 × 10⁻⁶. ‑1 Pa; (3) Titanium dioxide and silicon dioxide doped layers are deposited on glass by magnetron sputtering. Titanium dioxide is sputtered with a DC power of 215W and silicon dioxide is sputtered with an RF power of 75W-150W. Sputtering is performed simultaneously. When depositing TiO2, metallic Ti is used as the target material. When depositing SiO2, a Si target is used. The DC power Ti target and the RF power Si target are deposited simultaneously. Argon gas is introduced at 30 sccm and oxygen gas at 3 sccm; (4) A silicon dioxide layer is further deposited by magnetron sputtering. A Si target is used. The RF power is 100W. Argon gas is introduced at 30 sccm and oxygen gas at 3 sccm. Advantages of this invention: The high transmittance film prepared has a transmittance of up to 99.5% at 500nm and an average transmittance of over 97.4% at 500nm-600nm.
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Description

Technical Field

[0001] This invention belongs to the field of glass surface coating technology, and relates to an anti-reflective and high-transmittance thin film and its preparation method. Background Technology

[0002] Most of the antireflective and high-transmittance films currently on the market are prepared by chemical vapor deposition, magnetron sputtering, etc. Although films prepared by chemical vapor deposition have high transmittance, they have low deposition rate and poor wear resistance. On the other hand, films prepared by magnetron sputtering require more layers and are more complicated to operate in order to achieve the antireflective and high-transmittance effect. Summary of the Invention

[0003] The purpose of this invention is to solve the problems of low deposition rate and poor wear resistance in the preparation of antireflective and high-transmittance films by chemical vapor deposition, and the large number of layers and cumbersome operation in the preparation of antireflective and high-transmittance films by magnetron sputtering, and to provide an antireflective and high-transmittance film and its preparation method.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] An antireflective and high-transmittance thin film includes a glass substrate, characterized in that a titanium dioxide and silicon dioxide doped layer and a silicon dioxide layer are sequentially disposed on the glass substrate from bottom to top.

[0006] Furthermore, the refractive index of the titanium dioxide and silicon dioxide doped layer is 1.57-1.77, and the thickness is 138 nm.

[0007] Furthermore, the refractive index of the titanium dioxide and silicon dioxide doped layer is 1.66.

[0008] Furthermore, the refractive index of the silicon dioxide layer is 1.46, and the thickness is 102 nm.

[0009] A method for preparing an antireflective and high-transmittance film, characterized by comprising the following steps:

[0010] (1) Select ordinary glass as substrate, and use acetone, alcohol and deionized water to ultrasonically clean the glass in sequence to remove surface stains, and blow dry for later use.

[0011] (2) Place the dried glass on the sample holder and bombard the target with Ar ions to remove surface impurities and oxides, controlling the vacuum level to 2.0 × 10⁻⁶. -1 Pa;

[0012] (3) The glass after impurity removal is coated with a titanium dioxide and silicon dioxide doped layer by magnetron sputtering. The titanium dioxide is sputtered with a DC power supply of 215W and the silicon dioxide is sputtered with an RF power supply of 75W-150W. They are sputtered simultaneously. When TiO2 is coated, metallic Ti is used as the target material and SiO2 is coated with a Si target. The DC power supply Ti target and the RF power supply Si target are coated simultaneously. Argon gas is introduced at 30 sccm and oxygen gas at 3 sccm. After preparation, a titanium dioxide and silicon dioxide doped layer with a refractive index of 1.57-1.77 is obtained.

[0013] (4) A silicon dioxide layer was deposited on the titanium dioxide and silicon dioxide doped layer by magnetron sputtering. A Si target was used, the radio frequency power was 100W, and argon gas was introduced at 30 sccm and oxygen gas at 3 sccm. After preparation, a silicon dioxide layer with a refractive index of 1.46 was obtained.

[0014] Compared with the prior art, the present invention has the following advantages:

[0015] 1. The present invention uses magnetron sputtering to prepare a two-layer thin film consisting of a titanium dioxide and silicon dioxide doped layer and a silicon dioxide layer. Compared with other high-transmittance thin films prepared by chemical vapor deposition and magnetron sputtering, the present invention has a simple structure, stable process, fast preparation speed, good film quality and low cost.

[0016] 2. This invention achieves the purpose of enhancing light transmittance by combining a doped layer of titanium dioxide and silicon dioxide with a silicon dioxide layer of a specific refractive index. The high transmittance film prepared by this invention has a transmittance of up to 99.5% at 500nm and an average transmittance of over 97.4% in the 500nm-600nm range. Attached Figure Description

[0017] Figure 1 The transmittance spectrum of the high-transmittance antireflection film described in Example 1;

[0018] Figure 2 The transmittance spectrum of the high-transmittance antireflection film described in Example 2;

[0019] Figure 3 This is the transmittance spectrum of an antireflective high-transmittance film as described in Example 3. Detailed Implementation

[0020] A method for preparing an antireflective and high-transmittance film, the specific implementation steps of which are as follows: Example 1

[0021] (1) Select 1.1mm ordinary glass as substrate material and perform strict ultrasonic cleaning on the glass: use acetone, alcohol and deionized water in sequence for ultrasonic cleaning to remove surface stains, and then blow dry for later use.

[0022] (2) Place the dried glass into the magnetron sputtering equipment and evacuate the magnetron sputtering equipment. When the vacuum degree of the sputtering chamber reaches 1.0×10 -4 At Pa, argon gas was introduced at 30 sccm, and the vacuum degree was adjusted to 2.0 × 10⁻⁶. -1 Pa was used to pre-sputter Ti and Si targets respectively;

[0023] (3) After the pre-sputtering is completed, the first layer of titanium dioxide and silicon dioxide doped layer (refractive index 1.66) is prepared. During the coating, the Ti target is sputtered with DC power supply. The process is as follows: power supply power is 215W, Ar is 30sccm, O2 is 3sccm, and sputtering time is 41min45s. The Si target is sputtered with screen power supply. The process is as follows: power supply power is 100W, Ar is 30sccm, O2 is 3sccm, and sputtering time is 41min45s. Both materials are sputtered at the same time, and the working pressure is maintained at 2.0×10-1Pa to obtain a titanium dioxide and silicon dioxide doped layer with a film thickness of 138nm.

[0024] (4) Then, the second silicon dioxide layer (refractive index 1.46) is prepared. The Si target is sputtered by a screen power supply. The process is as follows: power supply power 100W, Ar 30sccm, O2 3sccm, sputtering time 40min, working pressure maintained at 2.0×10-1Pa, and a silicon dioxide layer with a thickness of 102nm is obtained. After the deposition is completed, an anti-reflection and high-transmittance film is obtained. The average transmittance of the anti-reflection and high-transmittance film in the visible light region is 97.4%, and the transmittance at 500nm is 99.5%. Example 2

[0025] (1) Select 1.1mm ordinary glass as substrate material and perform strict ultrasonic cleaning on the glass: use acetone, alcohol and deionized water in sequence for ultrasonic cleaning to remove surface stains, and then blow dry for later use.

[0026] (2) Place the dried glass into the magnetron sputtering equipment and evacuate the magnetron sputtering equipment. When the vacuum degree of the sputtering chamber reaches 1.0×10 -4 At Pa, argon gas was introduced at 30 sccm, and the vacuum degree was adjusted to 2.0 × 10⁻⁶. -1 Pa was used to pre-sputter Ti and Si targets respectively;

[0027] (3) After pre-sputtering, the first layer of titanium dioxide and silicon dioxide doped layer (refractive index 1.57) is prepared. During the coating process, the Ti target is sputtered using a DC power supply with the following parameters: power supply power of 215W, Ar at 30sccm, O2 at 3sccm, and sputtering time of 26min30s; the Si target is sputtered using a screen power supply with the following parameters: power supply power of 150W, Ar at 30sccm, O2 at 3sccm, and sputtering time of 26min30s; both materials are sputtered simultaneously, and the working pressure is maintained at 2.0×10 -1 Pa yielded a titanium dioxide and silicon dioxide doped layer with a film thickness of 138 nm;

[0028] (4) Then, the second silicon dioxide layer (refractive index 1.46) was prepared. The Si target was sputtered using a screen power supply. The process was as follows: power supply 100W, Ar 30sccm, O2 3sccm, sputtering time 40min, and working pressure maintained at 2.0×10 -1 Pa was used to obtain a silicon dioxide layer with a thickness of 102 nm. After the deposition was completed, a thin film was obtained. The thin film had an average transmittance of 95% in the visible light region and a transmittance of 97.9% at 550 nm. Example 3

[0029] (1) Select 1.1mm ordinary glass as substrate material and perform strict ultrasonic cleaning on the glass: use acetone, alcohol and deionized water in sequence for ultrasonic cleaning to remove surface stains, and then blow dry for later use.

[0030] (2) Place the dried glass into the magnetron sputtering equipment and evacuate the magnetron sputtering equipment. When the vacuum degree of the sputtering chamber reaches 1.0×10 -4 At Pa, argon gas was introduced at 30 sccm, and the vacuum degree was adjusted to 2.0 × 10⁻⁶. -1 Pa was used to pre-sputter Ti and Si targets respectively;

[0031] (3) After pre-sputtering, the first layer of titanium dioxide and silicon dioxide doped layer (refractive index 1.77) is prepared. During the coating process, the Ti target is sputtered using a DC power supply with the following parameters: power supply power of 215W, Ar at 30sccm, O2 at 3sccm, and sputtering time of 53min40s; the Si target is sputtered using a screen power supply with the following parameters: power supply power of 75W, Ar at 30sccm, O2 at 3sccm, and sputtering time of 53min40s; both materials are sputtered simultaneously, and the working pressure is maintained at 2.0×10 -1 Pa yielded a titanium dioxide and silicon dioxide doped layer with a film thickness of 138 nm;

[0032] (4) Then, the second silicon dioxide layer (refractive index 1.46) was prepared. The Si target was sputtered using a screen power supply. The process was as follows: power supply 100W, Ar 30sccm, O2 3sccm, sputtering time 40min, and working pressure maintained at 2.0×10 -1 Pa was used to obtain a silicon dioxide layer with a thickness of 102 nm. After the deposition was completed, a thin film was obtained. The thin film had an average transmittance of 89% in the visible light region and a transmittance of 97.6% at 550 nm.

[0033] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any person skilled in the art can make many possible variations and modifications to the technical solutions of the present invention, or modify them into equivalent embodiments, without departing from the scope of the present invention. Therefore, any simple modifications, equivalent substitutions, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention, without departing from the scope of the present invention, shall still fall within the protection scope of the present invention.

Claims

1. An antireflective and high-transmittance thin film, comprising a glass substrate, characterized in that... A titanium dioxide and silicon dioxide doped layer and a silicon dioxide layer are sequentially disposed on a glass substrate from bottom to top; the refractive index of the titanium dioxide and silicon dioxide doped layer is 1.57-1.77 and the thickness is 138nm; the refractive index of the silicon dioxide layer is 1.46 and the thickness is 102nm.

2. The antireflective and high-transmittance film according to claim 1, characterized in that: The refractive index of the titanium dioxide and silicon dioxide doped layer is 1.

66.

3. A method for preparing an antireflective and high-transmittance thin film, characterized in that... Includes the following steps: (1) Select ordinary glass as substrate, and use acetone, alcohol and deionized water to ultrasonically clean the glass in sequence to remove surface stains, and blow dry for later use. (2) Place the dried glass on the sample holder and bombard the target with Ar ions to remove surface impurities and oxides, controlling the vacuum level to 2.0 × 10⁻⁶. -1 Pa; (3) The glass after impurity removal is coated with a titanium dioxide and silicon dioxide doped layer by magnetron sputtering. The titanium dioxide is sputtered with a DC power supply of 215W and the silicon dioxide is sputtered with an RF power supply of 75W-150W. They are sputtered simultaneously. When TiO2 is coated, metallic Ti is used as the target material and SiO2 is coated with a Si target. The DC power supply Ti target and the RF power supply Si target are coated simultaneously. Argon gas is introduced at 30 sccm and oxygen gas at 3 sccm. After preparation, a titanium dioxide and silicon dioxide doped layer with a refractive index of 1.57-1.77 is obtained. (4) A silicon dioxide layer was deposited on the titanium dioxide and silicon dioxide doped layer by magnetron sputtering. A Si target was used, the radio frequency power was 100W, and argon gas was introduced at 30 sccm and oxygen gas at 3 sccm. After preparation, a silicon dioxide layer with a refractive index of 1.46 was obtained.