Antireflection and antifouling film and preparation process thereof

Abstract

The present invention discloses an antireflection and antireflection film and a preparation process thereof. The antireflection and antireflection film includes a substrate layer, a flexible transition layer, a first antireflection layer, a second antireflection layer, a third antireflection layer, a fourth antireflection layer, and a fifth antireflection layer which are sequentially stacked; the refractive index of the first antireflection layer is n1, the refractive index of the second antireflection layer is n2, the refractive index of the third antireflection layer is n3, the refractive index of the fourth antireflection layer is n4, and the refractive index of the fifth antireflection layer is n5, satisfying: n1 < n2 < n3, and n5 < n4 < n3; the material of the flexible transition layer is amorphous silicon carbide; the material of the first antireflection layer is a mixed oxide of silicon and aluminum; the material of the second antireflection layer is a mixed oxide of silicon and niobium; the material of the third antireflection layer is a mixed oxide of silicon, niobium and yttrium; the material of the fourth antireflection layer is a mixed oxide of silicon and zirconium; the material of the fifth antireflection layer is silicon dioxide. The present invention adopts a magnetron sputtering process and optimizes process parameters to solve the problems of rainbow patterns and poor bending resistance.

Description

Technical Field

[0001] This invention belongs to the field of optical film technology, specifically relating to an anti-reflective and anti-reflective film and its preparation process. Background Technology

[0002] In an era of fierce competition for existing market share, product homogenization and innovation bottlenecks have become core challenges restricting market growth. The emergence of foldable phones, like a key to breaking this deadlock, has redefined the physical boundaries and functional possibilities of mobile terminals with its revolutionary "foldable screen" form factor. Since the first mass-produced foldable phone was launched in 2019, this category has not only completed the leap from "technology verification" to "mature commercialization," but has also demonstrated its market vitality with a compound annual growth rate exceeding 50% (global shipments reaching 21 million units in 2023). Its significance extends far beyond the iteration of a single product; it leverages flexible display technology to drive systemic innovation in materials science, precision manufacturing, human-computer interaction, and even consumer culture.

[0003] However, under the visual impact of large screens, conventional methods for preparing anti-reflective coatings for the outer layer of foldable screens still have some shortcomings, resulting in a slightly less than ideal visual experience. Currently, the commonly used technique for preparing anti-reflective coatings for foldable screens is wet coating. Although it has advantages such as low cost and simple process in the preparation of optical films for foldable screen phones, it has significant limitations in terms of anti-reflection effect and precision control.

[0004] The patent, "A Sol-Gel Antireflective Film for Flexible Displays and Its Preparation Method," uses hollow SiO2 nanoparticles for coating, but the refractive index only drops to 1.38, and the reflectivity is >1.2% (measured data), which cannot meet the requirements of high-end foldable screens. The curing temperature needs to be 180℃, which causes thermal deformation of the polyimide substrate (CPI) (Tg≈260℃), requiring additional annealing compensation, resulting in high process complexity.

[0005] Another patent, "Refractive Index Matching Film, Method for Fabricating Refractive Index Matching Film, and Touch Screen," employs a sol-gel method to coat multilayer films. It achieves refractive index gradient matching by mixing a solution of nano-titanium oxide (TiO2) and acrylic resin. However, it suffers from several drawbacks: a narrow refractive index control range (only 1.48-1.68, see patent example data), failing to cover the wide-band (400-800nm) anti-reflection requirements of foldable screens, resulting in a reflectivity >1.5% (compared to below 0.3% with magnetron sputtering); insufficient adhesion (solvent-based coating solution leaves >15% micropores after curing), with interfacial bonding only at ASTM level 3B, leading to delamination after 50,000 bends; and high process temperature (final curing temperature requires 160℃, exceeding the temperature threshold of the CPI substrate, increasing the risk of substrate warping and deformation).

[0006] Due to the relatively limited precision of wet coating, the coating thickness is uneven, and the difference in interference conditions in different regions leads to the mixed interference of multi-wavelength light, thereby forming rainbow-like stripes. Summary of the Invention

[0007] The purpose of the present invention is to provide an antireflection and antireflection film and its preparation process. The antireflection and antireflection film has excellent bending resistance, small color difference, and is not prone to rainbow patterns.

[0008] In order to achieve the above purpose, the technical solutions provided by a specific embodiment of the present invention are as follows:

[0009] An antireflection and antireflection film includes a substrate layer, a flexible transition layer, a first antireflection layer, a second antireflection layer, a third antireflection layer, a fourth antireflection layer, and a fifth antireflection layer that are sequentially stacked;

[0010] Among them, the refractive index of the first antireflection layer is n1, the refractive index of the second antireflection layer is n2, the refractive index of the third antireflection layer is n3, the refractive index of the fourth antireflection layer is n4, and the refractive index of the fifth antireflection layer is n5, satisfying: n1 < n2 < n3, and n5 < n4 < n3;

[0011] The material of the flexible transition layer is amorphous silicon carbide;

[0012] The material of the first antireflection layer is a mixed oxide of silicon and aluminum;

[0013] The material of the second antireflection layer is a mixed oxide of silicon and niobium;

[0014] The material of the third antireflection layer is a mixed oxide of silicon, niobium, and yttrium;

[0015] The material of the fourth antireflection layer is a mixed oxide of silicon and zirconium;

[0016] The material of the fifth antireflection layer is silicon dioxide.

[0017] In one or more embodiments of the present invention, the refractive index n1 of the first antireflection layer is 1.440 - 1.460; and / or,

[0018] The thickness of the first antireflection layer is 38 nm - 41 nm.

[0019] In one or more embodiments of the present invention, the refractive index n2 of the second antireflection layer is 1.650 - 1.680; and / or,

[0020] The thickness of the second antireflection layer is 115 nm - 120 nm.

[0021] In one or more embodiments of the present invention, the refractive index n3 of the third antireflection layer is 2.050 - 2.100; and / or,

[0022] The thickness of the third antireflective layer is 130nm-135nm.

[0023] In one or more embodiments of the present invention, the refractive index n4 of the fourth antireflection layer is 1.850-1.880; and / or,

[0024] The thickness of the fourth antireflective layer is 3nm-8nm.

[0025] In one or more embodiments of the present invention, the refractive index n5 of the fifth antireflection layer is 1.410-1.430; and / or,

[0026] The thickness of the fifth antireflective layer is 88nm-94nm.

[0027] In one or more embodiments of the present invention, the thickness of the flexible transition layer is 0.5 nm-1.5 nm; and / or,

[0028] The substrate layer is made of either PET or CPI; and / or

[0029] The thickness of the substrate layer is 23μm-50μm.

[0030] Another specific embodiment of the present invention provides the following technical solution:

[0031] A process for preparing an antireflective and anti-reflective membrane includes the following steps:

[0032] Provide base materials;

[0033] A flexible transition layer, a first antireflection layer, a second antireflection layer, a third antireflection layer, a fourth antireflection layer, and a fifth antireflection layer are sequentially formed on the substrate by magnetron sputtering.

[0034] In one or more embodiments of the present invention, in the process of forming the flexible transition layer by magnetron sputtering, the target material is a silicon carbide target, and the sputtering gas includes argon and nitrogen, with a flow rate ratio of argon to nitrogen of 9:1 to 8.5:1.5; and / or,

[0035] In the process of forming the first antireflection layer by magnetron sputtering, the target materials include silicon targets and aluminum targets, and the target power ratio of the silicon targets and aluminum targets is 9.5:0.5-9:1. The sputtering gases include oxygen, argon, and nitrogen, and the flow rate ratio of oxygen, argon, and nitrogen is 6:3:1-6:2.5:1.5; and / or,

[0036] In the process of forming the second antireflection layer by magnetron sputtering, the target materials include silicon targets and niobium targets, and the target power ratio of the silicon targets and niobium targets is 7.5:2.5-7:3. The sputtering gases include oxygen, argon, and nitrogen, and the flow rate ratio of oxygen, argon, and nitrogen is 9:4:2-8.5:3.5:3; and / or,

[0037] In the process of forming the third antireflection layer by magnetron sputtering, the target materials include silicon targets, niobium targets, and yttrium targets, with a target power ratio of 3:7:0.1-3.5:6.5:0.2. The sputtering gases include oxygen, argon, and nitrogen, with a flow rate ratio of 10:3:2-9:2.5:3.5; and / or,

[0038] In the process of forming the fourth antireflection layer by magnetron sputtering, the target materials include silicon targets and zirconium targets, and the target power ratio of the silicon targets and zirconium targets is 4.5:5.5-5:5. The sputtering gases include oxygen, argon, and nitrogen, and the flow rate ratio of oxygen, argon, and nitrogen is 4:4:1-3.5:3.5:2; and / or,

[0039] In the process of forming the fifth antireflection layer by magnetron sputtering, the target material is a silicon target, and the sputtering gas includes oxygen, argon, and nitrogen, with a flow rate ratio of oxygen, argon, and nitrogen of 8:3:1 to 8:2.5:1.5; and / or,

[0040] The temperature of the substrate is controlled to be below 50°C.

[0041] In one or more embodiments of the present invention, in the process of forming the flexible transition layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or,

[0042] In the process of forming the first antireflection layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or,

[0043] In the process of forming the second antireflection layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or,

[0044] In the process of forming the third antireflection layer by magnetron sputtering, the bias voltage is -100V to -150V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or,

[0045] In the process of forming the fourth antireflection layer by magnetron sputtering, the bias voltage is -50V to -100V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or,

[0046] In the process of forming the fifth antireflection layer by magnetron sputtering, the bias voltage is -30V to -80V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%.

[0047] In one or more embodiments of the present invention, during the magnetron sputtering process, ICP-assisted magnetron sputtering is used, wherein the power of the ICP is 2kW-4kW.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] (1) Design of gradient refractive index composite materials:

[0050] Film structure: A five-layer asymmetric film system (low-medium-low-high-medium-high-low refractive index) is adopted, and the material of each layer is a gradient mixed oxide (such as SiAlO). x NbSiO x By adjusting the proportion of metallic elements, a continuous transition of refractive index is achieved, eliminating abrupt stress at the interface.

[0051] Flexible transition layer: An ultrathin (0.5nm-1.5nm) amorphous silicon carbide (a-SiC) layer is introduced between the substrate and the first layer to improve the interface adhesion and buffer bending stress.

[0052] (2) Optimization of magnetron sputtering process:

[0053] Composite target sputtering: Hybrid target co-sputtering is used, and the composition of the film is controlled by adjusting the ratio of reactive gases (O2 / Ar / N2);

[0054] Pulse bias technology: Apply bidirectional pulse bias to reduce the internal stress of the film to <200MPa (traditional process >500MPa), and improve the bending life (reflectivity change <0.1% after 100,000 bends with a radius of 3 mm).

[0055] Low-temperature deposition: The substrate temperature is controlled below 50°C. ICP-assisted ionization (power 2kW-4kW) is used to improve the film density and avoid deformation of the flexible substrate caused by high temperature. Attached Figure Description

[0056] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments recorded in the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0057] Figure 1 It is a schematic structural diagram of an antireflection and antireflection film in an embodiment of the present invention.

[0058] Main reference numerals description:

[0059] 1, substrate layer; 2, flexible transition layer; 3, first antireflection layer; 4, second antireflection layer; 5, third antireflection layer; 6, fourth antireflection layer; 7, fifth antireflection layer. Specific embodiments

[0060] In order to enable those skilled in the art to better understand the technical solutions in this disclosure, the technical solutions in the embodiments of this disclosure will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of this disclosure, rather than all the embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those of ordinary skill in the art without creative efforts should fall within the scope of protection of this disclosure.

[0061] A specific embodiment of the present invention provides an antireflection and antireflection film, as Figure 1 shown, including a substrate layer 1, a flexible transition layer 2, a first antireflection layer 3, a second antireflection layer 4, a third antireflection layer 5, a fourth antireflection layer 6, and a fifth antireflection layer 7 that are sequentially stacked; wherein, the refractive index of the first antireflection layer 3 is n1, the refractive index of the second antireflection layer 4 is n2, the refractive index of the third antireflection layer 5 is n3, the refractive index of the fourth antireflection layer 6 is n4, and the refractive index of the fifth antireflection layer 7 is n5, satisfying: n1 < n2 < n3, and n5 < n4 < n3.

[0062] Specifically, n1 is 1.440 - 1.460, n2 is 1.650 - 1.680, n3 is 2.050 - 2.100, n4 is 1.8500 - 1.880, and n5 is 1.410 - 1.430. The present invention sets a five-layer film structure on the flexible transition layer and adjusts the refractive indices of each film layer to make the refractive indices of the five-layer film structure show a continuous transition: low refractive index, medium-low refractive index, high refractive index, medium-high refractive index, and low refractive index, eliminating the interfacial mutation stress, reducing the interference of light with different wavelengths, reducing the appearance of rainbow-like stripes, reducing the reflected light, and increasing the transmitted light.

[0063] The flexible transition layer can improve the adhesion of the membrane interface and buffer bending stress. Combined with the membrane design of the first, second, third, fourth and fifth anti-reflective layers, the membrane material has excellent bending resistance.

[0064] Furthermore, the substrate layer is made of either PET (polyethylene terephthalate) or CPI (polyimide), with a thickness of 23μm-50μm.

[0065] Furthermore, the flexible transition layer material is amorphous silicon carbide (a-SiC) with a thickness of 0.5nm-1.5nm. By introducing the flexible transition layer, chemical bonds are formed between Si-C bonds and carboxyl groups on the PET surface, buffering bending stress and improving film adhesion.

[0066] Furthermore, the material of the first antireflective layer is a mixed oxide of silicon and aluminum, SiAlO. x (SiO2-Al2O3), with a thickness of 38nm-41nm. Using co-sputtering with Si and Al targets, a solid solution of SiO2 and Al2O3 is formed in a mixed atmosphere of oxygen, nitrogen, and argon, resulting in a predominantly amorphous state with Al... 3+ Partially replaces Si 4+ The continuous network structure with low defect density at the sites has a low refractive index.

[0067] Furthermore, the second antireflective layer is made of a mixed oxide of silicon and niobium, NbSiO. x (Nb2O5-SiO2), with a thickness of 115nm-120nm. Using co-sputtering with Si and Nb targets, a mixed phase of high-refractive-index Nb2O5 and SiO2 is preferentially generated under high O2 flow rate. Nb2O5 provides a transition between medium and low refractive indices, while the Nb-O bond energy is high (about 590kJ / mol), which can enhance the mechanical strength of the film.

[0068] Furthermore, the third antireflection layer is a mixed oxide of silicon, niobium, and yttrium, Nb₂O₅-SiO₂-Y₂O₃, with a thickness of 130 nm-135 nm. Y₂O₃ is introduced using Y-target co-sputtering or a pre-alloyed target. 3+ Ions occupy interstitial sites in the Nb₂O₅ lattice, forming an amorphous-nanocrystalline composite structure. 3+ The absorption peaks of ions in the 520nm-650nm range can offset the phase error of the film system, reducing the color difference ΔE to below 1.2 and decreasing the appearance of rainbow stripes.

[0069] Furthermore, the fourth antireflective layer is made of a mixed oxide of silicon and zirconium, ZrSiO. xThe thickness is 3nm-8nm. The thermal expansion mismatch between ZrSiO4 and PET substrate is only 15% (the mismatch between traditional oxides and PET substrate is >60%). The interfacial shear stress decreases by about 40% during bending, avoiding the risk of delamination and thus improving bending resistance.

[0070] Furthermore, the fifth antireflective layer is made of silicon dioxide (SiO2) with a thickness of 88nm-94nm. The fifth antireflective layer is formed by sputtering using a Si target, where the Si target is sputtered in O2 to generate dense amorphous SiO2, which serves as the outermost layer to provide scratch resistance and environmental stability.

[0071] Another specific embodiment of the present invention provides a process for preparing an antireflective coating, comprising the following steps: providing a substrate; and sequentially forming a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer on the substrate by magnetron sputtering.

[0072] Specifically, during magnetron sputtering, relevant parameters such as target power, sputtering gas, power supply parameters, and substrate temperature are optimized. Target power affects the density, adhesion, and refractive index of the film. This invention sets different target powers for the target used in each film layer, so that each film layer reaches a predetermined refractive index and the adhesion between film layers is high, which can improve the bending resistance of the film material.

[0073] The sputtering gases selected are oxygen, argon, and nitrogen. By adjusting the gas ratios and the type of target material, the composition of the film can be controlled. Specifically, the addition of nitrogen enhances amorphization: nitrogen doping inhibits oxide crystallization, forming a dense amorphous structure, reducing internal stress from 500 MPa in pure oxides to <200 MPa; and refines grain size: nitrogen dissociates into active N atoms in the plasma, adsorbing onto the substrate surface and hindering the longitudinal growth of oxide grains (columnar crystals), promoting the formation of equiaxed or amorphous structures. These factors ultimately improve the bending resistance of the film material.

[0074] The power supply in this invention uses a pulsed DC power supply. By adjusting the power supply parameters, stress can be reduced by 20%-30%. The specific principles are as follows: Grain refinement: High-frequency pulses (50kHz) increase the ion bombardment frequency, interrupting the longitudinal growth of columnar crystals and forming a nanocrystalline / amorphous hybrid structure (grain size <20nm), reducing grain boundary stress concentration; Thermal stress suppression: Low duty cycle (20%-40%) shortens the duration of ion bombardment, reducing local temperature rise (0T <50%℃), and reducing thermal expansion mismatch stress; Defect repair: The pulse interval (60%-80% of the time) allows for atomic rearrangement in the film layer, repairing microcracks and pores, and reducing residual stress. By reducing stress, the microstructure of the film layer is improved, the rainbow-like stripes caused by optical mixing interference are suppressed, and the bending resistance of the film material is enhanced.

[0075] The substrate temperature is controlled below 50℃ to avoid deformation of the flexible substrate caused by high temperature and to improve the density of the film layer.

[0076] Furthermore, in the process of forming the flexible transition layer by magnetron sputtering, the target material is a silicon carbide target, the sputtering gas includes argon and nitrogen, the flow ratio of argon and nitrogen is 9:1-8.5:1.5, the bias voltage is -80V to -120V, the pulse frequency is 30kHz-80kHz, and the duty cycle is 20%-40%.

[0077] The first antireflection layer is formed by sputtering using silicon and aluminum targets, with a target power ratio of 9.5:0.5-9:1. The parameters for sputtering the first antireflection layer satisfy the following: sputtering gases include oxygen, argon, and nitrogen, with a flow rate ratio of 6:3:1-6:2.5:1.5; bias voltage is -80V to -120V; pulse frequency is 30kHz-80kHz; and duty cycle is 20%-40%.

[0078] A second antireflection layer was formed by sputtering using silicon and niobium targets, with a target power ratio of 7.5:2.5-7:3. The parameters for sputtering the second antireflection layer met the following requirements: sputtering gases included oxygen, argon, and nitrogen, with a flow rate ratio of 9:4:2-8.5:3.5:3; bias voltage of -80V to -120V; pulse frequency of 30kHz-80kHz; and duty cycle of 20%-40%.

[0079] A third antireflection layer was formed by sputtering using silicon, niobium, and yttrium targets, with a target power ratio of 3:7:0.1-3.5:6.5:0.2. The parameters for sputtering the third antireflection layer met the following requirements: sputtering gases included oxygen, argon, and nitrogen, with a flow rate ratio of 10:3:2-9:2.5:3.5; bias voltage of -100V to -150V; pulse frequency of 30kHz-80kHz; and duty cycle of 20%-40%.

[0080] A fourth antireflection layer was formed by sputtering using silicon and zirconium targets, with a target power ratio of 4.5:5.5-5:5. The parameters for sputtering the fourth antireflection layer met the following requirements: sputtering gases included oxygen, argon, and nitrogen, with a flow rate ratio of 4:4:1-3.5:3.5:2; bias voltage of -50V to -100V; pulse frequency of 30kHz-80kHz; and duty cycle of 20%-40%.

[0081] The fifth antireflection layer is formed by sputtering with a silicon target. The sputtering gases include oxygen, argon and nitrogen, with a flow rate ratio of 8:3:1 to 8:2.5:1.5. The bias voltage is -30V to -80V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%.

[0082] Furthermore, during the magnetron sputtering process, ICP (inductively coupled plasma) is used to assist magnetron sputtering, with an ICP power of 2kW-4kW. ICP-assisted ionization is used to improve film density and prevent deformation of the flexible substrate caused by high temperatures.

[0083] The present invention will be further described in detail below with reference to specific embodiments.

[0084] Example 1

[0085] The antireflective coating in this embodiment includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 1.

[0086] Table 1. Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 1

[0087]

[0088] Example 2

[0089] The antireflective coating in this embodiment includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 38μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 2.

[0090] Table 2. Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 2

[0091]

[0092] Example 3

[0093] The antireflective coating in this embodiment includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of PET with a thickness of 23 μm. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 3.

[0094] Table 3. Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 3

[0095]

[0096] Example 4

[0097] The antireflective coating in this embodiment includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 4.

[0098] Table 4. Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 4

[0099]

[0100] Example 5

[0101] The antireflective coating in this embodiment includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 5.

[0102] Table 5. Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 5.

[0103]

[0104] Comparative Example 1

[0105] The antireflective coating in this comparative example includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 6.

[0106] Table 6 Comparative Example 1: Magnetron sputtering parameters, refractive index, and thickness of each layer

[0107]

[0108] Comparative Example 2

[0109] The antireflective coating in this comparative example includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 7.

[0110] Table 7 Comparative Example 2: Magnetron sputtering parameters, refractive index, and thickness of each layer

[0111]

[0112] Comparative Example 3

[0113] The antireflective coating in this comparative example includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 8.

[0114] Table 8 Comparative Example 3: Magnetron sputtering parameters, refractive index, and thickness of each layer

[0115]

[0116] Comparative Example 4

[0117] The antireflective coating in this comparative example includes a substrate layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The first, second, third, fourth, and fifth antireflective layers are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 9.

[0118] Table 9 Comparative Example 4: Magnetron sputtering parameters, refractive index, and thickness of each layer.

[0119]

[0120] Comparative Example 5

[0121] The antireflective coating in this comparative example includes a substrate layer, a flexible transition layer, a first antireflective layer, a second antireflective layer, a third antireflective layer, a fourth antireflective layer, and a fifth antireflective layer stacked sequentially. The substrate layer is made of 50 μm thick PET. The flexible transition layer, the first antireflective layer, the second antireflective layer, the third antireflective layer, the fourth antireflective layer, and the fifth antireflective layer are all formed by magnetron sputtering. The specific parameters of magnetron sputtering and the thickness and refractive index of each layer are shown in Table 10.

[0122] Table 10 Magnetron sputtering parameters, refractive index, and thickness of each layer in Example 1

[0123]

[0124] The following tests were conducted on the membrane materials used in each embodiment and comparative example: Adhesion test: cross-cut adhesion test according to ASTM D3359; Transmittance test: ASTM D1003; Reflectance test: ISO 13468-1; ΔE test: ASTM E308; Bending resistance test: GB / T 38001.11; Internal stress test: GB / T 44517-2024. The test results are shown in Table 11.

[0125] Table 11 Performance Test Results

[0126]

[0127] As can be seen from Table 11, the antireflective and anti-reflective film in the embodiments of the present invention exhibits excellent bending resistance. At the same time, the ∆E (color difference) value is small. Generally speaking, the smaller the ∆E value, the fainter the rainbow stripes and the better the optical performance of the film material.

[0128] In Comparative Example 1, the nitrogen gas was removed during sputtering of the membrane material, leading to increased internal stress and decreased bending resistance. In Comparative Example 2, the yttrium target was removed during the formation of the third antireflection layer, and the absence of Y element in the membrane layer resulted in an increased ΔE value, making the membrane material prone to rainbow-like stripes. In Comparative Example 3, the power supply parameters were adjusted during preparation, with no bias voltage and no adjustment to the output power and duty cycle, leading to increased internal stress, decreased bending resistance, and reduced membrane adhesion. In Comparative Example 4, the flexible transition layer was removed, resulting in decreased membrane adhesion and decreased bending resistance. In Comparative Example 5, the ICP power was turned off during preparation, leading to decreased bending resistance, reduced adhesion, and increased internal stress.

[0129] In summary, by optimizing the film layer design, target material usage, sputtering gas ratio, and power supply parameters, this invention solves the problems of existing films being unresistant to bending and having rainbow-like stripes. The resulting antireflective and anti-reflective film not only has excellent bending resistance, low reflectivity, and high transmittance, but also has small color difference and does not have the rainbow stripe problem.

[0130] It will be apparent to those skilled in the art that this disclosure is not limited to the details of the exemplary embodiments described above, and that this disclosure can be implemented in other specific forms without departing from the spirit or essential characteristics of this disclosure. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of this disclosure is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within this disclosure.

[0131] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider 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. An antireflective and anti-reflective membrane, characterized in that, It includes a substrate layer, a flexible transition layer, a first antireflection layer, a second antireflection layer, a third antireflection layer, a fourth antireflection layer, and a fifth antireflection layer that are sequentially stacked. Among them, the refractive index of the first antireflection layer is n1, the refractive index of the second antireflection layer is n2, the refractive index of the third antireflection layer is n3, the refractive index of the fourth antireflection layer is n4, and the refractive index of the fifth antireflection layer is n5, satisfying: n1 < n2 < n3, and n5 < n4 < n3; The material of the flexible transition layer is amorphous silicon carbide; The material of the first antireflection layer is a mixed oxide of silicon and aluminum; The material of the second antireflection layer is a mixed oxide of silicon and niobium; The material of the third antireflection layer is a mixed oxide of silicon, niobium, and yttrium; The material of the fourth antireflection layer is a mixed oxide of silicon and zirconium; The material of the fifth antireflection layer is silicon dioxide.

2. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The refractive index n1 of the first antireflection layer is 1.440 - 1.460; and / or, The thickness of the first antireflection layer is 38 nm - 41 nm.

3. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The refractive index n2 of the second antireflection layer is 1.650 - 1.680; and / or, The thickness of the second antireflection layer is 115 nm - 120 nm.

4. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The refractive index n3 of the third antireflection layer is 2.050 - 2.100; and / or, The thickness of the third antireflection layer is 130 nm - 135 nm.

5. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The refractive index n4 of the fourth antireflection layer is 1.850 - 1.880; and / or, The thickness of the fourth antireflection layer is 3 nm - 8 nm.

6. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The refractive index n5 of the fifth antireflection layer is 1.410 - 1.430; and / or, The thickness of the fifth antireflection layer is 88 nm - 94 nm.

7. The antireflective and anti-reflective membrane according to claim 1, characterized in that, The thickness of the flexible transition layer is 0.5 nm - 1.5 nm; and / or, The material of the substrate layer is any one of PET and CPI; and / or, The thickness of the substrate layer is 23 μm - 50 μm.

8. A process for preparing the antireflective and anti-reflective membrane according to any one of claims 1-7, characterized in that, It includes the following steps: Provide a substrate; On the substrate, a flexible transition layer, a first antireflection layer, a second antireflection layer, a third antireflection layer, a fourth antireflection layer, and a fifth antireflection layer are sequentially formed by magnetron sputtering.

9. According to the preparation process of the antireflection and antireflection enhancement film described in claim 8, the characteristics are as follows, In the process of forming the flexible transition layer by magnetron sputtering, the target is a silicon carbide target, the sputtering gas includes argon and nitrogen, and the flow ratio of argon and nitrogen is 9:1 - 8.5:1.5; and / or, In the process of forming the first antireflection layer by magnetron sputtering, the targets include a silicon target and an aluminum target, the target power ratio of the silicon target and the aluminum target is 9.5:0.5 - 9:1, the sputtering gas includes oxygen, argon, and nitrogen, and the flow ratio of oxygen, argon, and nitrogen is 6:3:1 - 6:2.5:1.5; and / or, In the process of forming the second antireflection layer by magnetron sputtering, the targets include a silicon target and a niobium target, the target power ratio of the silicon target and the niobium target is 7.5:2.5 - 7:3, the sputtering gas includes oxygen, argon, and nitrogen, and the flow ratio of oxygen, argon, and nitrogen is 9:4:2 - 8.5:3.5:3; and / or, In the process of forming the third antireflection layer by magnetron sputtering, the target materials include silicon targets, niobium targets, and yttrium targets, with a target power ratio of 3:7:0.1-3.5:6.5:0.

2. The sputtering gases include oxygen, argon, and nitrogen, with a flow rate ratio of 10:3:2-9:2.5:3.5; and / or, In the process of forming the fourth antireflection layer by magnetron sputtering, the target materials include silicon targets and zirconium targets, and the target power ratio of the silicon targets and zirconium targets is 4.5:5.5-5:

5. The sputtering gases include oxygen, argon, and nitrogen, and the flow rate ratio of oxygen, argon, and nitrogen is 4:4:1-3.5:3.5:2; and / or, In the process of forming the fifth antireflection layer by magnetron sputtering, the target material is a silicon target, and the sputtering gas includes oxygen, argon, and nitrogen, with a flow rate ratio of oxygen, argon, and nitrogen of 8:3:1 to 8:2.5:1.5; and / or, The temperature of the substrate is controlled to be below 50°C.

10. The preparation process of the antireflective and anti-reflective membrane according to claim 8, characterized in that, In the process of forming the flexible transition layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or, In the process of forming the first antireflection layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or, In the process of forming the second antireflection layer by magnetron sputtering, the bias voltage is -80V to -120V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or, In the process of forming the third antireflection layer by magnetron sputtering, the bias voltage is -100V to -150V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or, In the process of forming the fourth antireflection layer by magnetron sputtering, the bias voltage is -50V to -100V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%; and / or, In the process of forming the fifth antireflection layer by magnetron sputtering, the bias voltage is -30V to -80V, the pulse frequency is 30kHz to 80kHz, and the duty cycle is 20% to 40%.

11. The preparation process of the antireflective and anti-reflective membrane according to claim 8, characterized in that, During the magnetron sputtering process, ICP-assisted magnetron sputtering is used, and the power of the ICP is 2kW-4kW.

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