Refractive index adjusting method, deposition method, antireflection film, assembly and equipment

Abstract

The invention discloses a refractive index adjusting method, a deposition method, an anti-reflection film, an assembly and equipment wherein the anti-reflection film comprises a base material layer and an anti-reflection layer formed on the base material layer, the anti-reflection layer is a composite layer structure formed by low refractive index material layers and high refractive index material layers alternately, wherein the low-refractive-index material layer and the high-refractive-index material layer are respectively layers with different densities which are formed under power supplies with different frequencies and / or different sputtering powers and / or different sputtering gas composition proportions and / or different target-substrate distances, and the density of the low-refractive-index material layer is lower than that of the high-refractive-index material layer. By optimizing the magnetron sputtering deposition technology, in the film layer deposition process of the AR film antireflection structure, the refractive index of the high-refractive-index layer approaches the upper limit of the refractive index interval of the high-refractive-index layer, the refractive index of the low-refractive-index layer approaches the lower limit of the refractive index interval of the low-refractive-index layer, and therefore a larger refractive index difference value between the high-refractive-index layer and the low-refractive-index layer is achieved; therefore, the requirement of the product on the reflectivity is met.

Description

Technical Field

[0001] The present invention belongs to the field of electronic technology, and in particular relates to a method for adjusting a refractive index, a deposition method, an anti-reflection film, a component and a device. Background Art

[0002] The main function of AR film is to reduce or eliminate reflected light from optical surfaces such as lenses, prisms, and plane mirrors, thereby increasing the light transmittance of these components. By effectively increasing the transmittance of glass or film materials and reducing their reflectivity, the reflection and glare problems caused by electronic video screens and image screens under ambient light sources can be reduced, making the contrast stronger and the scene image highly clear. The commonly used preparation method is magnetron sputtering. For general display products, there are no very strict anti-reflection requirements, but there are extremely high requirements in medical or semiconductor applications, which means that when the material is certain, there are higher requirements for the preparation process. A larger refractive index difference can achieve lower reflectivity over a wider wavelength range, so a larger refractive index difference between AR film layer structures is currently desired.

[0003] Table 1 Technical parameters of existing anti-reflection layer deposition

[0004]

[0005] However, as shown in Table 1 above, in the deposition of the prior art, the deposition of the high refractive index layer and the low refractive index layer is achieved only by controlling the deposition power and the composition of the sputtering gas. This solution cannot achieve the requirement of making the “refractive index difference” as large as possible.

[0006] Therefore, in view of the above technical problems, it is necessary to provide a method for adjusting the refractive index, a deposition method, an anti-reflection film, a component and an apparatus.

[0007] The information disclosed in this background technology section is only intended to enhance the understanding of the overall background of the invention and should not be regarded as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to a person skilled in the art. Summary of the invention

[0008] The object of the present invention is to provide a method for adjusting the refractive index, a deposition method, an antireflection film, a component and a device.

[0009] In order to achieve the above object, a technical solution provided by a specific embodiment of the present invention is as follows:

[0010] A method for adjusting the refractive index by vapor deposition applied to a transmittance-enhancing layer comprises depositing a high refractive index layer and / or a low refractive index layer respectively by magnetron sputtering deposition, wherein the magnetron sputtering deposition is adjusted under at least any one of the following parameters: power source type, sputtering power, sputtering gas, and target-substrate distance, so as to adjust the refractive index of the deposited layer to approach the refractive index range limit of the target target material deposition structure.

[0011] In one or more embodiments of the present invention, the magnetron detection deposition includes a high refractive index layer deposition method and / or a low refractive index layer deposition method:

[0012] The high refractive index layer deposition method is: Nb 2 O 5 The target material is deposited by a radio frequency power supply under the condition of a first mixed gas consisting of oxygen, argon and krypton to obtain a dense first deposition structure, and the refractive index of the first deposition structure approaches that of Nb obtained by the deposition method. 2 O 5 The upper limit of the refractive index interval of the structure;

[0013] The low refractive index layer deposition method is: SiO 2 The target material is deposited by a medium frequency power supply under the condition of a second mixed gas composed of oxygen and argon to obtain a loose second deposition structure, and the refractive index of the second deposition structure is close to that of SiO obtained by the deposition method. 2 The lower limit of the refractive index interval of the structure.

[0014] In one or more embodiments of the present invention, the RF power source is: 13 MHz-35 MHz, and the power is 8-13.5 kW.

[0015] In one or more embodiments of the present invention, the medium frequency power supply is: 10kHz-30kHz, and the power is 4-7.3kW.

[0016] In one or more embodiments of the present invention, the sputtering gas composition is selected from: Ar:O 2 The volume ratio of the mixed gas is (3-5):(5-7), Ar:O 2 :The volume ratio of the Kr mixed gas is (4-5):4.5:(0.5-1.5).

[0017] In one or more embodiments of the present invention, the target-substrate distance of the high refractive index layer deposition method ranges from: 80 to 100 mm;

[0018] The target-substrate distance of the low refractive index layer deposition method ranges from 105 to 130 mm.

[0019] In one or more embodiments of the present invention, a method for depositing a multilayer structure of an anti-reflection layer includes a high refractive index layer deposition process and a low refractive index layer deposition process that are alternately implemented, wherein the high refractive index layer deposition process and the low refractive index layer deposition process both include the following process:

[0020] Determine the refractive index range of the target target deposition structure and select the target refractive index;

[0021] According to the selected target refractive index, the deposition parameters of the target target material are simulated in the thin film optical software, and the deposition parameters are at least selected from: power type, sputtering power, sputtering gas and target-substrate distance;

[0022] The method of adjusting the refractive index by vapor deposition applied to the anti-reflection layer is used to set parameters and deposit the target material.

[0023] In one or more embodiments of the present invention, the AR antireflection film is deposited by the aforementioned deposition method.

[0024] In one or more embodiments of the present invention, the display assembly includes a display carrier and an AR anti-reflection film disposed thereon. Preferably, the average reflectivity R550 of the AR anti-reflection film at a wavelength of 550 nm is ≤ 0.3%.

[0025] In one or more embodiments of the present invention, the display carrier may be a glass plate, a plastic plate or other transparent material plate. As the substrate of the AR antireflection film, the display carrier is required to have high light transmittance and good surface flatness to ensure the optical performance and visual effect of the AR antireflection film.

[0026] In one or more embodiments of the present invention, the display assembly may further include other functional layers, such as a conductive layer, a hardening layer, an anti-scratch layer, etc., to meet different application requirements. These functional layers can be selected and combined according to specific requirements to achieve versatility and high performance of the display assembly.

[0027] In one or more embodiments of the present invention, an electronic device has a display window, and the display window includes an AR antireflection film or a display component.

[0028] In one or more embodiments of the present invention, the electronic device may be a device having a display window such as a smart phone, a tablet computer, a laptop computer, a display, etc. By applying an AR anti-reflection film or a display component to the display window of the electronic device, the clarity and brightness of the display image can be improved, and the user experience can be improved. In addition, the method for adjusting the refractive index, the deposition method, the anti-reflection film, the component and the device of the present invention may also be applied to other fields, such as optical instruments, solar panels, etc., to improve the optical performance and efficiency of these products.

[0029] Compared with the prior art, the method for adjusting refractive index, deposition method, antireflection film, assembly and equipment of the present invention optimizes the magnetron sputtering deposition technology to achieve that during the film deposition process of the AR film antireflection structure, the refractive index of the high refractive index layer approaches the upper limit of its refractive index range, and the refractive index of the low refractive index layer approaches the lower limit of its refractive index range, thereby achieving a larger refractive index difference between the two, thereby meeting the product's reflectivity requirements. Furthermore, the present invention achieves the effect of significantly increasing the refractive index difference between the high and low refractive index layers at a wavelength of 550nm by adopting a composite deposition process. Through the RF / IF power supply collaborative control technology (13-35MHz / 10-30kHz), combined with Nb 2 O 5 During the target deposition process, Kr doping gas is additionally added to optimize the other ratios of sputtering to make Nb 2 O 5 The layer density approaches the upper limit of the refractive index range. Tests show that the average reflectivity (Rave) of the present invention in the 400-700nm band is ≤0.27%, which is 48.6% lower than that of the traditional process. The AR antireflection film realized by the present invention can meet the requirements of high-precision display equipment, such as high-precision medical imaging display systems and semiconductor wafer detection equipment.

[0030] In summary, the method for adjusting the refractive index, the deposition method, the anti-reflection film, the assembly and the equipment of the present invention have significant technical advantages and broad application prospects. By optimizing the magnetron sputtering deposition technology, a larger refractive index difference between the high refractive index layer and the low refractive index layer in the film deposition process of the AR film anti-reflection structure is achieved, thereby meeting the product's requirements for reflectivity. At the same time, the present invention also has the advantages of simple process, low cost, and easy promotion. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0032] Figure 1 It is a microscopic photograph comparison diagram of the samples of Example 1 of the present invention and Comparative Example 1;

[0033] Figure 2 This is a reflectivity curve diagram of the sample in Example 1 of the present invention in the 400-700nm band;

[0034] Figure 3 This is a reflectivity curve diagram of the sample in Example 2 of the present invention in the 400-700nm band;

[0035] Figure 4 This is a reflectivity curve diagram of the sample of Example 3 of the present invention in the 400-700nm band;

[0036] Figure 5 The reflectivity curve of the sample of Example 4 of the present invention in the 400-700nm band;

[0037] Figure 6 The reflectivity curve of the sample of comparative example 1 of the present invention in the 400-700nm band;

[0038] Figure 7 The reflectivity curve of the sample of comparative example 3 of the present invention in the 400-700nm band;

[0039] Figure 8 It is a reflectivity curve diagram of the sample of comparative example 4 of the present invention in the 400-700nm band. DETAILED DESCRIPTION

[0040] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the technical solutions of the present invention will be clearly and completely described below in conjunction with 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 creative work should fall within the scope of protection of the present invention.

[0041] It is known to those skilled in the art that a larger refractive index difference can achieve a lower reflectivity in a wider wavelength range. This is because materials with different refractive indices will produce destructive interference at different wavelengths, thereby reducing reflection. Refer to the empirical formula for wide-band high transmittance proposed by Willey:

[0042] R ave (W, L, T, D) = (4.38 / D)(1 / T) 0.31 [exp(W-1.4)-1](L-1) 3.5

[0043] Where W is the bandwidth of low reflection; D is the difference between the high and low refractive indices except for the outermost layer; T is the total optical thickness of the antireflection film, and L is the refractive index of the outermost thin film. From the above formula, it can be seen that when designing a broadband ultra-low reflection film, the difference between the high and low refractive indices of the selected material should be as large as possible. Therefore, it is crucial to increase the refractive index difference of the materials used to prepare the AR antireflection film. The refractive index is closely related to the density of the material. Generally speaking, the greater the density of the material, the higher the refractive index. This is because in materials with a relatively high density, the interaction between light and matter is more frequent, thus slowing down the speed of light. On the other hand, the material with the lowest refractive index well-known to those skilled in the art should be vacuum. Air is most similar to vacuum in refractive index, approximately 1. When the density of the same material is greater, the less air it contains, and the refractive index is relatively larger. Conversely, the smaller the density, the smaller the refractive index.

[0044] The prior art sputters using fixed materials, and the theoretical refractive index range that can be achieved by different materials under different process conditions is determined. For example, SiO 2 has a theoretical refractive index of 1.40 - 1.5 at 550 nm, and Nb 2 O 5 has a theoretical refractive index of 2.2 - 2.45 at 550 nm. In the existing solutions, according to the simulation deposition design to achieve the required physical thickness, the refractive index of the deposited layer cannot be approximated to the limit value, thus failing to achieve a greater refractive index difference. This solution optimizes the magnetron sputtering process to increase or decrease the refractive index of the materials prepared, making it approach the limit value, thereby achieving a greater refractive index difference.

[0045] Assuming that the film layer and the substrate have no absorption and the incident medium is air

[0046] Substrate reflectivity

[0047] Substrate refractive index

[0048]

[0049]

[0050] At odd multiples of λ / 4 in thickness, the film layer reflectivity is

[0051]

[0052] Film layer refractive index

[0053]

[0054] First, according to the remaining reflectivity value of the substrate corresponding to the wavelength at odd multiples of λ / 4 of the film layer, calculate the refractive index of the substrate at 550 nm using formula (2), and then substitute the remaining reflectivity value of the film layer and the corresponding substrate refractive index at the same wavelength into formula (4) to obtain SiO2 Layer and Nb 2 O 5 Refractive index of the layer at a wavelength of 550 nm. Where R s Is the substrate reflectivity, n s Is the substrate refractive index, R f Is the film layer reflectivity, n f Is the film layer refractive index.

[0055] In actual production, due to equipment process limitations, the vehicle speed is the same when preparing all antireflection layers. Considering the actual production efficiency, it is necessary to ensure that it is made in one time as much as possible. Under the condition that other process conditions remain unchanged, those skilled in the art know that the power only affects the deposition thickness within a certain range. At this time, the deposited antireflection layers can all reach the same refractive index, but beyond a certain limit, it may affect the density of particle deposition.

[0056] In summary, the present invention provides a method for adjusting the refractive index of a gas-phase deposition applied to an antireflection layer, including magnetron sputtering deposition to respectively deposit a high refractive index layer and / or a low refractive index layer, and the magnetron sputtering deposition is adjusted at least under any one of the following parameters: power supply type, sputtering power, sputtering gas, and target-substrate distance, so as to adjust the refractive index of the deposited layer to approach the refractive index range limit of the target substrate deposition structure.

[0057] The above-mentioned magnetron detection deposition includes a high refractive index layer deposition method and / or a low refractive index layer deposition method, specifically as follows:

[0058] The high refractive index layer deposition method is: Nb 2 O 5 The target is deposited under the condition of a first mixed gas composed of oxygen, argon, and krypton with a radio frequency power supply to obtain a dense first deposition structure, and the refractive index of the first deposition structure approaches the upper limit of the refractive index range of the Nb 2 O 5 structure obtained by the deposition method;

[0059] The low refractive index layer deposition method is: SiO 2 The target is deposited under the condition of a second mixed gas composed of oxygen and argon with an intermediate frequency power supply to obtain a loose second deposition structure, and the refractive index of the second deposition structure approaches the lower limit of the refractive index range of the SiO 2 structure obtained by the deposition method.

[0060] The present invention optimizes the magnetron sputtering process from four aspects of power supply, sputtering power, sputtering gas ratio, and target-substrate distance, and then improves the density of the sputtered film to reach the optimal refractive index. Taking the low refractive index SiO 2 layer and the high refractive index Nb 2 O 5 layer as an example, SiO 2The layer requires a lower refractive index, so the process needs to be adjusted to make the film formation relatively sparse, while Nb 2 O 5 layer requires a higher refractive index and the film formation is relatively dense.

[0061] Power supply: When other factors are fixed, the film formation by the radio frequency power supply is denser than that by the medium frequency power supply. The SiO 2 layer uses the medium frequency power supply, and the Nb 2 O 5 layer uses the radio frequency power supply.

[0062] Sputtering power: The sputtering power can adjust the deposition rate of the thin film. When the sputtering power increases, the excitation amount of argon plasma increases, the plasma density increases, the sputtering rate of the target material also increases, the rate of sputtering particles will also be enhanced, and the energy of the particles reaching the substrate increases. This will help the nucleation and growth of the thin film and improve the denseness of the thin film. Therefore, the SiO 2 layer uses low-power sputtering, and the Nb 2 O 5 layer uses high-power sputtering.

[0063] Sputtering gas ratio: Both the SiO 2 layer and the Nb 2 O 5 layer preparation requires introducing argon and oxygen. Among them, argon is a noble gas with a very high atomic mass. High atomic mass means that when ionized and accelerated towards the target material, argon will generate a huge momentum during impact, which will lead to the efficient ejection of target atoms, thus increasing the sputtering rate and making the film formation dense. Here, it should be noted that since both materials require oxygen as the reaction gas, if the oxygen ratio is too low, it will also affect their refractive index. In order to achieve higher denseness, in this solution, a certain proportion of krypton gas is additionally added when preparing the Nb 2 O 5 film layer. Krypton atoms are heavier than argon atoms, and have a larger sputtering coefficient and a lower ionization energy. This means that krypton gas can more effectively sputter out the target atoms during the sputtering process, thereby improving the denseness of the film formation.

[0064] Target-substrate distance: A smaller target-substrate distance usually can obtain a denser and more uniform thin film because high-energy particles can better migrate and recombine on the substrate surface to form an ordered structure.

[0065] The set process parameters are shown in Table 2 below:

[0066] Table 2 Technical parameters during the deposition of the antireflection layer in the technical solution of this application

[0067]

[0068]

[0069] Using the above method, the present invention also provides a deposition method for a multi-layer structure of an antireflection layer, which includes alternately performing a high refractive index layer deposition process and a low refractive index layer deposition process. Both the high refractive index layer deposition process and the low refractive index layer deposition process include the following steps:

[0070] Determine the refractive index range of the target target deposition structure and select the target refractive index;

[0071] According to the selected target refractive index, simulate the deposition parameters of the target target in thin film optical software. The deposition parameters are at least selected from: power supply type, sputtering power, sputtering gas, and target-substrate distance;

[0072] Adopt the above-mentioned method for adjusting the refractive index by gas phase deposition applied to the antireflection layer to set parameters, and deposit the target target to obtain an AR antireflection film.

[0073] In addition, the present invention also provides a display component, including a display carrier and an AR antireflection film disposed thereon.

[0074] An electronic device has a display window, and the display window includes a frame with an installation position and a display component matched to the installation position.

[0075] The following is a detailed description of the deposition process:

[0076] The magnetron sputtering equipment has 8 target positions, and each target position is equipped with a medium frequency power supply and a radio frequency power supply, and is configured with Nb 2 O 5 target and SiO 2 target. Before preparing the AR film, use BK7 glass to magnetron sputter the antireflection layers 1 and 2 respectively, measure their reflectivity, calculate the refractive index at 550 nm, and use TFCalc for optical simulation to determine the thickness of the antireflection layer.

[0077] Table 3 Thickness parameters of the antireflection layer in the technical solution of the present application

[0078] Target Layer thickness Anti-reflection layer 4 <![CDATA[SiO 2 ]]> 90-93nm Anti-reflection layer 3 <![CDATA[Nb 2 THE 5 ]]> 114-116nm Anti-reflection layer 2 <![CDATA[SiO 2 ]]> 29-32nm Anti-reflection layer 1 <![CDATA[Nb 2 THE 5 ]]> 18-21nm Substrate BK7 Glass /

[0079] For example, if the target materials are Si targets with a purity of 99.99% and Nb 2 O 5 targets, and the substrate is BK7 glass. The vehicle speed is 1 m / min, and the antireflection layer Nb 2 O 5 Film formation process: The power supply of the 1st target position uses a radio frequency power supply, the power supply frequency is: 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 8 - 13 kW; the gas flow rate: Ar: 40 - 50 sccm, O2: 45 sccm, Kr: 15 - 5 sccm; the measured refractive index is 2.41. The antireflection layer SiO 2Film formation process: The power supply for the 2nd target position uses a medium-frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is: 120 mm; the power is: 4 - 6 kW; gas flow rate: Ar: 40 sccm, O2: 60 sccm; the measured refractive index is 1.42.

[0080] Including but not limited to the following embodiments, the target materials selected are Si target and Nb2O5 target with a purity of 99.99%, and the substrate selected is BK7 glass. The vehicle speed is 1 m / min. Anti-reflection layer Nb 2 O 5 Film formation process: The power supply for the 1st target position uses a radio-frequency power supply, the power supply frequency is: 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 12 kW; gas flow rate: Ar: 40 sccm, O 2 : 45 sccm, Kr: 15 sccm; the measured refractive index is 2.41. Anti-reflection layer SiO 2 Film formation process: The power supply for the 2nd target position uses a medium-frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is: 120 mm; the power is: 6 kW; gas flow rate: Ar: 40 sccm, O 2 : 60 sccm; the measured refractive index is 1.42. Based on this refractive index data, TFCalc is used for optical simulation to determine the thicknesses of the anti-reflection layers in sequence as: (1) 19.95 nm (2) 31.25 nm (3) 115.5 nm (4) 91.96 nm.

[0081] Example 1:

[0082] In this example, the AR film process is specifically as follows: The vehicle speed is 1 m / min. Anti-reflection layer 1: The power supply for the 1st target position uses a radio-frequency power supply, the power supply frequency is 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 8 kW; gas flow rate: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; Anti-reflection layer 2: The power supply for the 2nd target position uses a medium-frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is: 120 mm; the power is: 4 kW; gas flow rate: Ar: 40 sccm, O2: 60 sccm; Anti-reflection layer 3: The power supplies for the 3rd, 4th, 5th, and 6th target positions use radio-frequency power supplies, the power supply frequency is 15.5 MHz, the target-substrate distance is: 90 mm; the power of a single target is: 11.25 kW; gas flow rate: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; Anti-reflection layer 4: The power supplies for the 7th and 8th target positions use medium-frequency power supplies, the power supply frequency is 20 kHz, the target-substrate distance is: 120 mm; the power of a single target is: 5.5 kW; gas flow rate: Ar: 40 sccm, O2: 60 sccm.

[0083] Example 2:

[0084] In this embodiment, the AR film process is specifically as follows: the vehicle speed is 1.2 m / min. For antireflection layer 1: the power supply for the 1st target position uses a radio frequency power supply, the power supply frequency is 15.5 MHz, the target-substrate distance is 90 mm; the power is 9.6 kW; the gas flow rate: Ar is 50 sccm, O2 is 45 sccm, Kr is 5 sccm. For antireflection layer 2: the power supply for the 2nd target position uses an intermediate frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is 120 mm; the power is 4.8 kW; the gas flow rate: Ar is 40 sccm, O2 is 60 sccm. For antireflection layer 3: the power supplies for the 3rd, 4th, 5th, and 6th target positions use radio frequency power supplies, the power supply frequency is 15.5 MHz, the target-substrate distance is 90 mm; the power of a single target is 13.5 kW; the gas flow rate: Ar is 48 sccm, O2 is 45 sccm, Kr is 7 sccm. For antireflection layer 4: the power supplies for the 7th and 8th target positions use intermediate frequency power supplies, the power supply frequency is 20 kHz, the target-substrate distance is 120 mm; the power of a single target is 6.6 kW; the gas flow rate: Ar is 40 sccm, O2 is 60 sccm.

[0085] Example 3:

[0086] In this embodiment, the AR film process is specifically as follows: the vehicle speed is 1 m / min. For antireflection layer 1: the power supply for the 1st target position uses a radio frequency power supply, the power supply frequency is 13 MHz, the target-substrate distance is 85 mm; the power is 9.5 kW; the gas flow rate: Ar is 40 sccm, O2 is 45 sccm, Kr is 15 sccm. For antireflection layer 2: the power supply for the 2nd target position uses an intermediate frequency power supply, the power supply frequency is 15 kHz, the target-substrate distance is 118 mm; the power is 5.3 kW; the gas flow rate: Ar is 30 sccm, O2 is 70 sccm. For antireflection layer 3: the power supplies for the 3rd, 4th, 5th, and 6th target positions use radio frequency power supplies, the power supply frequency is 13 MHz, the target-substrate distance is 85 mm; the power of a single target is 13.4 kW; the gas flow rate: Ar is 40 sccm, O2 is 45 sccm, Kr is 15 sccm. For antireflection layer 4: the power supplies for the 7th and 8th target positions use intermediate frequency power supplies, the power supply frequency is 15 kHz, the target-substrate distance is 118 mm; the power of a single target is 7.3 kW; the gas flow rate: Ar is 30 sccm, O2 is 70 sccm.

[0087] Example 4:

[0088] In this embodiment, the AR film process is specifically as follows: the vehicle speed is 2 m / min. For the anti-reflection layer 1, the power supply of the 1st target position uses a radio frequency power supply with a power frequency of 25 MHz, the target-substrate distance is 95 mm, the power is 14 kW, and the gas flow rates are: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm. For the anti-reflection layer 2, the power supply of the 2nd target position uses an intermediate frequency power supply with a power frequency of 20 kHz, the target-substrate distance is 130 mm, the power is 7.0 kW, and the gas flow rates are: Ar: 50 sccm, O2: 50 sccm.

[0089] For the second pass, the vehicle speed is 1 m / min. For the anti-reflection layer 3, the power supplies of the 3rd, 4th, 5th, and 6th target positions use radio frequency power supplies with a power frequency of 15.5 MHz, the target-substrate distance is 90 mm, the power of each target is 13.5 kW, and the gas flow rates are: Ar: 48 sccm, O2: 45 sccm, Kr: 7 sccm. For the anti-reflection layer 4, the power supplies of the 7th and 8th target positions use intermediate frequency power supplies with a power frequency of 20 kHz, the target-substrate distance is 120 mm, the power of each target is 6.6 kW, and the gas flow rates are: Ar: 40 sccm, O2: 60 sccm.

[0090] Comparative Example 1:

[0091] The target materials selected are Si target with a purity of 99.99% and Nb 2 O 5 target, and the substrate selected is BK7 glass. The vehicle speed is 1 m / min. For the anti-reflection layer Nb 2 O 5 film forming process: the power supply of the 1st target position uses an intermediate frequency power supply with a power frequency of 100 kHz, the target-substrate distance is 90 mm, the power is 12 kW, and the gas flow rates are: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; the measured refractive index is (2.28). For the anti-reflection layer SiO 2Film formation process: The power supply for the 2nd target position uses a radio frequency power supply with a power frequency of 10.5 MHz, a target-substrate distance of 120 mm, a power of 6 kW, a gas flow rate of Ar: 40 sccm, O2: 60 sccm, and the measured refractive index is (1.47). TFCalc is used for optical simulation to determine the thicknesses of the anti-reflection layers as follows: (1) 16.06 nm (2) 47.81 nm (3) 22.79 nm (4) 106.83 nm. The AR film process is as follows: The vehicle speed is 1 m / min. For anti-reflection layer 1, the power supply for the 1st target position uses an intermediate frequency power supply with a power frequency of 100 kHz, a target-substrate distance of 90 mm, a power of 6.5 kW, a gas flow rate of Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm. For anti-reflection layer 2, the power supply for the 2nd target position uses a radio frequency power supply with a power frequency of 10.5 MHz, a target-substrate distance of 120 mm, a power of 6 kW, a gas flow rate of Ar: 40 sccm, O2: 60 sccm. For anti-reflection layer 3, the power supply for the 3rd target position uses an intermediate frequency power supply with a power frequency of 100 kHz, a target-substrate distance of 90 mm, a power of 8.8 kW, a gas flow rate of Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm. For anti-reflection layer 4, the power supplies for the 4th, 5th, and 6th target positions use radio frequency power supplies with a power frequency of 10.5 MHz, a target-substrate distance of 120 mm, a single target power of 4.25 kW, and a gas flow rate of Ar: 40 sccm, O2: 60 sccm.

[0092] Comparative Example 2:

[0093] The target materials selected are Si targets with a purity of 99.99% and Nb 2 O 5 targets, and the substrate selected is BK7 glass. The vehicle speed is 1 m / min. For the anti-reflection layer Nb 2 O 5 Film formation process: The power supply for the 1st target position uses a radio frequency power supply with a power frequency of 15.5 MHz, a target-substrate distance of 90 mm, a power of 15 kW, a gas flow rate of Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm, and the measured refractive index is (2.42). For the anti-reflection layer SiO 2 Film formation process: The power supply for the 2nd target position uses an intermediate frequency power supply with a power frequency of 20 kHz, a target-substrate distance of 120 mm, a power of 3 kW, a gas flow rate of Ar: 40 sccm, O2: 60 sccm, and the measured refractive index is (1.41). Since the energy of the particles in the first layer is too high due to the high power, excessive surface rearrangement or stress accumulation occurs, resulting in larger film defects, and finally the adhesion of this layer is NG.

[0094] Optical simulation was carried out using TFCalc to determine that the thicknesses of the anti-reflection layers are successively: (1) 15.49 nm, (2) 30.99 nm, (3) 115.96 nm, (4) 92.43 nm.

[0095] Comparative Example 3:

[0096] The target materials used are a Si target with a purity of 99.99% and a Nb 2 O 5 target, and the substrate is BK7 glass. The vehicle speed is 1 m / min, and for the anti-reflection layer Nb 2 O 5 Film-forming process: The power supply for the 1st target position uses a radio frequency power supply with a power frequency of 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 12 kW; the gas flow rates are: Ar: 35 sccm, O2: 35 sccm, Kr: 30 sccm; the measured refractive index is (2.26). For the anti-reflection layer SiO 2 Film-forming process: The power supply for the 2nd target position uses an intermediate frequency power supply with a power frequency of 20 kHz, the target-substrate distance is: 120 mm; the power is: 6 kW; the gas flow rates are: Ar: 60 sccm, O2: 40 sccm; the measured refractive index is (1.48). Optical simulation was carried out using TFCalc to determine that the thicknesses of the anti-reflection layers are successively: (1) 13.46 nm, (2) 34.88 nm, (3) 122.23 nm, (4) 85.39 nm.

[0097] The AR film process is as follows: The vehicle speed for the first pass is 1 m / min. For anti-reflection layer 1: The power supply for the 1st target position uses a radio frequency power supply with a power frequency of 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 8.5 kW; the gas flow rates are: Ar: 35 sccm, O2: 35 sccm, Kr: 30 sccm; for anti-reflection layer 2: The power supply for the 2nd target position uses an intermediate frequency power supply with a power frequency of 20 kHz, the target-substrate distance is: 120 mm; the power is: 4.2 kW; the gas flow rates are: Ar: 60 sccm, O2: 40 sccm.

[0098] The vehicle speed for the second pass is 1 m / min. For anti-reflection layer 3: The power supply for the 1-6th target positions uses a radio frequency power supply with a power frequency of 15.5 MHz, the target-substrate distance is: 90 mm; the power is: 12.8 kW; the gas flow rates are: Ar: 35 sccm, O2: 35 sccm, Kr: 30 sccm; for anti-reflection layer 4: The power supply for the 7th and 8th target positions uses an intermediate frequency power supply with a power frequency of 20 kHz, the target-substrate distance is: 120 mm; the power is: 5.1 kW; the gas flow rates are: Ar: 60 sccm, O2: 40 sccm.

[0099] Comparative Example 4:

[0100] The target materials used are a Si target with a purity of 99.99% and a Nb 2O 5 Target, the substrate is BK7 glass. The vehicle speed is 1 m / min, and the antireflection layer is Nb 2 O 5 Film formation process: The power supply of the No. 1 target position uses a radio frequency power supply, the power supply frequency is 15.5 MHz, the target-substrate distance is: 120 mm; the power is: 12 kW; the gas flow rate: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; the measured refractive index is (2.30). The antireflection layer is SiO 2 Film formation process: The power supply of the No. 2 target position uses an intermediate frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is: 80 mm; the power is: 6 kW; the gas flow rate: Ar: 40 sccm, O2: 60 sccm; the measured refractive index is (1.46). Use TFCalc for optical simulation to determine that the thicknesses of the antireflection layers are successively: (1) 12.75 nm (2) 34.38 nm (3) 118.04 nm (4) 86.12 nm.

[0101] The AR film process is as follows: The vehicle speed in the first pass is 1 m / min. Antireflection layer 1: The power supply of the No. 1 target position uses a radio frequency power supply, the power supply frequency is 15.5 MHz, the target-substrate distance is: 120 mm; the power is: 8 kW; the gas flow rate: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; Antireflection layer 2: The power supply of the No. 2 target position uses an intermediate frequency power supply, the power supply frequency is 20 kHz, the target-substrate distance is: 80 mm; the power is: 4 kW; the gas flow rate: Ar: 40 sccm, O2: 60 sccm;

[0102] The vehicle speed in the second pass is 1 m / min. Antireflection layer 3: The power supplies of the No. 1-6 target positions use radio frequency power supplies, the power supply frequency is 15.5 MHz, the target-substrate distance is: 120 mm; the power of a single target is: 12.5 kW; the gas flow rate: Ar: 40 sccm, O2: 45 sccm, Kr: 15 sccm; Antireflection layer 4: The power supplies of the No. 7 and 8 target positions use intermediate frequency power supplies, the power supply frequency is 20 kHz, the target-substrate distance is: 80 mm; the power of a single target is: 5 kW; the gas flow rate: Ar: 40 sccm, O2: 60 sccm.

[0103] Table 4 Performance comparison table of the examples and comparative examples of the present invention

[0104]

[0105] It can be seen from the above table that for the multi-layer structures of the antireflection layers prepared in Examples 1-4, the adjustment of the refractive index difference is realized. Compared with the products prepared by the traditional process, the present invention examples respectively achieve: Nb 2 O 5 The refractive index of the layer is increased to approach the upper limit of the refractive index range of the high refractive index layer and SiO 2The refractive index of the layer decreases to approach the lower limit of the refractive index range of the low-refractive-index layer. The deposition thickness is determined through optical simulation using TFCalc, so that the refractive index difference between layers of the AR antireflection film can achieve a better transmittance difference. As shown in Comparative Example 1, when the power supplies of the deposited Nb 2 O 5 layer and the SiO 2 layer are swapped, at this time, due to the change in the compactness of the Nb 2 O 5 layer and the SiO 2 layer, the refractive index cannot reach a higher difference (the refractive index of the SiO 2 layer increases to approach the upper limit of the refractive index range of the high-refractive-index layer and the refractive index of the Nb 2 O 5 layer decreases to approach the lower limit of the refractive index range of the low-refractive-index layer), resulting in a relatively low transmittance of the AR antireflection film. As shown in Comparative Example 2, during the deposition process, a relatively high power is used, and the high-refractive-index layer achieves extreme compactness, which will cause excessive stress in the film and thus affect its adhesion. As shown in Comparative Examples 3 and 4, it shows that adjusting the gas ratio and the target-substrate distance will affect the compactness of the coated film layer and cannot meet the requirement of a large refractive index difference between layers, thereby affecting the transmittance of the AR antireflection film. This fully shows that even if similar target materials, substrate materials, and vehicle speeds are used as in the examples, if the film-forming process parameters of each antireflection layer, especially key factors such as the type of power supply, sputtering power, sputtering gas, and target-substrate distance, cannot be precisely controlled, it is difficult to obtain an ideal refractive index difference between layers and excellent transmittance performance.

[0106] Figure 1 This is a comparison of the scanning electron microscope microtopographies of the samples of Example 1 of the present invention and Comparative Example 1, showing the adjustment effect of the radio frequency / medium frequency power supply on the film layer density. Among them, the Nb 2 O 5 layer of Example 1 presents a typical columnar dense structure (packing density > 92%), while in Comparative Example 1, the opposite power supply combination is used, resulting in a loose structure (packing density < 85%).

[0107] Figure 2-4 The reflectivity test curves corresponding to Examples 1-3 respectively show that the reflectivity is lower than 0.3% in the 400 - 700 nm band. Among them, the reflectivity peak of Example 1 at 550 nm is 0.12%, meeting the strict standard of R550 < 0.15% for medical displays.

[0108] Figure 5-7 For the verification of the performance deterioration of the comparative example samples: Figure 5 It shows that the mismatch of power supply parameters leads to a sharp increase in reflectivity (R550 = 0.75%); Figure 6 It shows that the deviation of gas ratio makes the effective band narrower; Figure 7Verify the stress defects caused by too small target base distance.

[0109] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be embraced by the present invention.

[0110] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for adjusting the refractive index by vapor deposition applied to a transmittance-enhancing layer, comprising depositing a high refractive index layer and / or a low refractive index layer by magnetron sputtering deposition, wherein the magnetron sputtering deposition is adjusted under at least any one of the following parameters: power type, sputtering power, sputtering gas, and target-substrate distance, so as to adjust the refractive index of the deposited layer to approach the refractive index range limit of the target target material deposition structure.

2. The method for adjusting the refractive index by vapor deposition applied to an anti-reflection layer according to claim 1, characterized in that: The magnetron detection deposition includes a high refractive index layer deposition method and / or a low refractive index layer deposition method: The high refractive index layer deposition method is as follows: a Nb2O5 target material is deposited by a radio frequency power supply under a first mixed gas condition consisting of oxygen, argon and krypton to obtain a dense first deposition structure, wherein the refractive index of the first deposition structure approaches the upper limit of the refractive index range of the Nb2O5 structure obtained by the deposition method; The low refractive index layer deposition method is as follows: SiO2 target material is deposited with a medium frequency power supply under the conditions of a second mixed gas composed of oxygen and argon to obtain a loose second deposition structure, and the refractive index of the second deposition structure approaches the lower limit of the refractive index range of the SiO2 structure obtained by the deposition method.

3. The method for adjusting the refractive index by vapor deposition applied to an anti-reflection layer according to claim 2, characterized in that: The radio frequency power supply is: 13MHz-35MHz, power 8-13.5kW.

4. The method for adjusting the refractive index by vapor deposition applied to an anti-reflection layer according to claim 2, characterized in that: The intermediate frequency power supply is 10kHz-30kHz and has a power of 4-7.3kW.

5. The method for adjusting the refractive index by vapor deposition applied to an anti-reflection layer according to claim 2, characterized in that: The sputtering gas composition is selected from: the volume ratio of Ar:O2 mixed gas is (3-5):(5-7), the volume ratio of Ar:O2:Kr mixed gas is (4-5):4.5:(0.5-1.5).

6. The method for adjusting the refractive index by vapor deposition applied to an anti-reflection layer according to claim 2, characterized in that: The target-substrate distance of the high refractive index layer deposition method is in the range of: 80 to 100 mm; The target-substrate distance of the low refractive index layer deposition method ranges from: 105 to 130 mm.

7. A method for depositing a multilayer structure of an anti-reflection layer, comprising alternately implementing a high refractive index layer deposition process and a low refractive index layer deposition process, wherein the high refractive index layer deposition process and the low refractive index layer deposition process both include the following process: Determine the refractive index range of the target target deposition structure and select the target refractive index; According to the selected target refractive index, simulating deposition parameters of the target target material in thin film optical software, wherein the deposition parameters are at least selected from: power type, sputtering power, sputtering gas, and target-substrate distance; The method for adjusting the refractive index by vapor deposition applied to an anti-transmission layer according to any one of claims 1 to 6 is used to set parameters and deposit the target material.

8. An AR antireflection film deposited by the deposition method according to claim 7.

9. A display assembly, comprising a display carrier and the AR antireflection film according to claim 8 arranged thereon.

10. An electronic device having a display window, the display window comprising a frame having a mounting position and the display assembly according to claim 9 matched to the mounting position.

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