Wear-resistant AR coating film for optical element and preparation method of wear-resistant AR coating film

Abstract

The invention discloses a wear-resistant AR coating film for an optical element and a preparation method of the wear-resistant AR coating film, and belongs to the technical field of optical elements, and the preparation method comprises the steps of substrate pretreatment, bottom layer deposition, hardness layer preparation, interference layer deposition, antifouling layer deposition and post-treatment. By optimizing the structural design of the multi-layer film and the preparation process of each layer, the coating film has high hardness and high light transmittance, the thickness of the film layer is in a suitable range, the problems of overlarge internal stress and film layer cracking caused by purely increasing the thickness of the hardness layer are avoided, the defect of insufficient hardness when the thickness of the film layer is controlled is overcome, and the service life of the film layer is prolonged. And good balance of high hardness, high light transmission and proper film thickness is realized.

Description

Technical Field

[0001] This invention relates to the field of optical element technology, and more specifically to a wear-resistant AR coating for optical elements and its preparation method. Background Technology

[0002] Anti-reflective (AR) coating is a key technology for improving the light transmission performance of optical components. Its core function is to reduce the proportion of reflected light on the optical surface and improve the transmission efficiency of incident light. Therefore, it is widely used in many technical fields such as consumer electronics, optical imaging, and precision instruments.

[0003] However, in the process of optimizing the performance of traditional antireflective coatings, if the film density is increased or high-hardness components are introduced to enhance the film hardness, the reflectivity in the visible light band will increase, which in turn will reduce the transmittance. If the core goal is to improve the transmittance, the film hardness is difficult to meet the standard due to the film structure or the characteristics of the material itself, and scratches are easy to occur during actual use.

[0004] To address the aforementioned contradictions, Chinese patent CN120794375A attempted to achieve a balance between hardness and light transmittance through a multilayer film structure design. However, the weak interfacial bonding between film layers still presents challenges, making it difficult to simultaneously achieve a balance between high light transmittance, high hardness, and suitable film thickness. When increasing the thickness of the hardening layer to enhance hardness, excessive stress can easily be generated within the film layer, leading to cracking. Conversely, when controlling the film thickness to prevent cracking, the film hardness cannot meet the requirements of practical application scenarios. These shortcomings limit the widespread application of anti-reflective coatings in applications requiring high durability (such as display cover plates that require frequent contact).

[0005] Based on this, the present invention designs a wear-resistant AR coating for optical components and a method for preparing the same to solve the above problems. Summary of the Invention

[0006] To address the aforementioned shortcomings of existing technologies, this invention provides a method for preparing a wear-resistant AR coating for optical components, comprising the following steps: S1: Substrate pretreatment; Select a substrate, rinse and dry it, introduce Ar, activate it with plasma, immerse it in a silane coupling agent solution, and cure it to obtain a pretreated substrate; S2: Drilling the bottom layer of sediment; The pretreated substrate is placed in the vacuum chamber of the magnetron sputtering equipment, evacuated and heated to 200-250℃ and kept at that temperature, O2 is introduced, and Si targets and Ti targets are sputtered alternately until the underlayer thickness is ≥0.2μm. S3: Hardness layer preparation; Keeping the substrate temperature constant, the working gas is adjusted to an Ar / O2 / N2 mixed gas. High-energy pulsed magnetron sputtering technology is used to sputter the AlSi target, and Ar ion source-assisted bombardment is turned on to continuously deposit until the hard layer thickness is ≥0.6μm. S4: Interference layer deposition; Keeping the vacuum level and substrate temperature constant in S3, switch to alternating deposition of SiO2 target and TiO2 target, set a total of 4-6 deposition cycles, and the total thickness of the interference layer is ≥0.2μm; S5: Anti-fouling layer deposition; Maintain the S4 vacuum chamber environment, use a molybdenum boat electrode, pass current to evaporate the AF antifouling liquid, and deposit an antifouling layer with a thickness ≥0.3μm; S6: Post-processing; Turn off the ion source and sputtering power supply, maintain the vacuum chamber environment, and allow the substrate to cool to room temperature. After cooling, remove the substrate and UV cure it to form a wear-resistant AR coating for optical components on the substrate surface.

[0007] Furthermore, S1 specifically involves: selecting high-transmittance optical glass as the substrate, ultrasonically cleaning it with 5-10wt% washing solution at 70-90kHz for 15-25 minutes, rinsing it with deionized water at 38-42℃ for 200-300 seconds, drying it at 40-60℃ for 20-30 minutes, then introducing Ar and performing plasma activation at 280-320W for 4-8 minutes, immersing it in a 0.8-1.5% silane coupling agent solution, soaking it at room temperature for 15-25 minutes, and curing it at 120-140℃ for 25-35 minutes to obtain the pretreated substrate.

[0008] Furthermore, the silane coupling agent is silane coupling agent N3112, silane coupling agent KH-550, or B-201 silane coupling agent.

[0009] Furthermore, S2 specifically involves: placing the pretreated substrate into the vacuum chamber of the magnetron sputtering equipment and evacuating it to a vacuum level of 5 × 10⁻⁶. - 4 Below Pa, heat to 200-250℃ and hold for 15-25 minutes, then introduce O2 at a flow rate of 18-22 sccm, adjust the oxygen partial pressure to 0.13-0.17 Pa, and set the sputtering power density to 3-5 W / cm. 2 The Si and Ti targets are sputtered alternately, and the interlayer period is controlled to be 8-12nm by controlling the sputtering time of each target, and the deposition continues until the bottom layer thickness is ≥0.2μm.

[0010] Furthermore, S3 specifically involves: maintaining a constant substrate temperature, adjusting the working gas to an Ar / O2 / N2 mixture, and increasing the sputtering power density to 4-6 W / cm². 2High-energy pulsed magnetron sputtering technology was used to sputter AlSi targets with a pulse frequency of 450-550Hz and a duty cycle of 8-12%. Ar ion source was turned on to assist in bombardment, and the ion energy was controlled at 70-90eV. The deposition continued until the hard layer thickness was ≥0.6μm.

[0011] Furthermore, the Si content in the AlSi target is 20-30 at%.

[0012] Furthermore, in the working gas, Ar is the carrier gas, and the volume ratio of O2 / N2 is 1:2.5-3.5.

[0013] Furthermore, in S4, the sealing layer is a SiO2 layer with a thickness of 10-15 nm.

[0014] A wear-resistant AR coating for optical components prepared according to the preparation method described above.

[0015] Compared with the prior art, the beneficial effects of this invention are as follows: 1. This invention optimizes the design of the multilayer film structure and the preparation process of each layer, so that the coating has both high hardness and high light transmittance, and the film thickness is within a suitable range. This avoids the problems of excessive internal stress and film cracking caused by simply increasing the thickness of the hardness layer, and also solves the defect of insufficient hardness when controlling the film thickness. It achieves a good balance between high hardness, high light transmittance and suitable film thickness.

[0016] 2. This invention significantly improves the interfacial bonding between the film layer and the substrate, and between the film layers, by alternately sputtering Si and Ti targets in the bottom layer, optimizing the substrate pretreatment process and UV curing posttreatment steps. This effectively enhances the structural stability of the film layer, making the coating less prone to peeling or damage when subjected to external forces such as friction and corrosion, thus meeting the usage requirements of application scenarios with high durability requirements such as display cover plates.

[0017] 3. The wear-resistant AR coating prepared by this invention not only exhibits excellent performance in hardness and light transmittance, but also possesses good resistance to alkaline sweat corrosion and UV aging, as well as low haze, small color difference, and stable optical performance. This comprehensively improves the overall performance of the coating and broadens its application range in multiple fields such as consumer electronics, optical imaging, and precision instruments, demonstrating significant practical value. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the accompanying drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are merely some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without any creative effort.

[0019] Figure 1 This is a schematic diagram of the structure of a wear-resistant AR coating for optical components according to the present invention.

[0020] The annotations in the attached figures are explained as follows: 1. Substrate; 2. Underlayer; 3. Hardening layer; 4. Interference layer; 5. Anti-fouling layer. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] Example 1: This example provides a method for preparing a wear-resistant AR coating for optical components, including the following steps: S1: Pretreatment of substrate 1; High-transparency optical glass substrate 1 was selected and ultrasonically cleaned for 15 min at 70 kHz with 5 wt% detergent (Shenzhen Huijie Detergent Products Co., Ltd., product specification HJ-B303, the same below), rinsed with 38℃ deionized water for 200 s, dried at 40℃ for 20 min, Ar was introduced and plasma activated at 280 W for 4 min, and then immersed in 0.8% silane coupling agent solution (solvent is ethanol and deionized water in a volume ratio of 4:1) for 15 min at room temperature and cured at 120℃ for 25 min to obtain pretreated substrate 1; The silane coupling agent is silane coupling agent N3112; S2: Drilling the bottom layer of sedimentation; The pretreated substrate 1 is placed in the vacuum chamber of the magnetron sputtering equipment, and the vacuum is evacuated to 5×10⁻⁶. -4 Below Pa, heat to 200℃ and hold for 15 min, then introduce O2 at a flow rate of 18 sccm, adjust the oxygen partial pressure to 0.13 Pa, and set the sputtering power density to 3 W / cm². 2 Alternately sputter Si and Ti targets, and control the interlayer period to 8nm by controlling the sputtering time of each target, and continue to deposit until the thickness of the bottom layer 2 is ≥0.2μm; S3: Preparation of hardness layer 3; Keeping the substrate 1 temperature constant, the working gas was adjusted to an Ar / O2 / N2 mixture (Ar as the carrier gas), with an O2 / N2 volume ratio of 1:2.5, and the sputtering power density was increased to 4 W / cm². 2High-energy pulsed magnetron sputtering technology was used to sputter an AlSi target (Si content 20 at%) with a pulse frequency of 450 Hz and a duty cycle of 8%. Ar ion source was turned on to assist in bombardment, and the ion energy was controlled at 70-90 eV. The deposition continued until the thickness of the hard layer 3 was ≥0.6 μm. S4: Interference layer 4 deposition; Keeping the vacuum level of S3 and the temperature of substrate 1 constant, the deposition was switched to alternating SiO2 target and TiO2 target, with a total of 4 deposition cycles. The sealing layer was a 10nm thick SiO2, and the total thickness of the interference layer 4 was ≥0.2μm. S5: Anti-fouling layer 5 deposition; Maintain the S4 vacuum chamber environment, use a molybdenum boat electrode, apply a current of 70mA, evaporate the AF antifouling liquid (Shenzhen Zhongfu Technology Co., Ltd., model UD120, the same below), deposit for 3 minutes, and form an antifouling layer with a thickness ≥0.3μm. S6: Post-processing; Turn off the ion source and sputtering power supply, maintain the vacuum chamber environment, and cool substrate 1 to room temperature at a cooling rate of ≤5℃ / min. After cooling, remove substrate 1 and irradiate it at a wavelength of 365nm and an irradiation intensity of 500mW / cm². 2 UV curing for 10 minutes forms a wear-resistant AR coating for optical components on the surface of substrate 1.

[0023] Example 2: This example provides a method for preparing a wear-resistant AR coating for optical components, including the following steps: S1: Pretreatment of substrate 1; High-transparency optical glass substrate 1 was selected, ultrasonically cleaned with 10wt% washing solution at 90kHz for 25min, rinsed with 42℃ deionized water for 300s, dried at 60℃ for 30min, Ar was introduced, and plasma activation was performed at 320W for 8min. Then, it was immersed in 1.5% silane coupling agent solution (solvent is ethanol and deionized water in a volume ratio of 4:1), soaked at room temperature for 25min, and cured at 140℃ for 35min to obtain pretreated substrate 1. The silane coupling agent is silane coupling agent KH-550; S2: Drilling the bottom layer of sedimentation; The pretreated substrate 1 is placed in the vacuum chamber of the magnetron sputtering equipment, and the vacuum is evacuated to 5×10⁻⁶. -4 Below Pa, heat to 250℃ and hold for 25 min, then introduce O2 at a flow rate of 22 sccm, adjust the oxygen partial pressure to 0.17 Pa, and set the sputtering power density to 5 W / cm². 2 Alternately sputter Si and Ti targets, and control the interlayer period to 12nm by controlling the sputtering time of each target, and continue to deposit until the thickness of the bottom layer 2 is ≥0.2μm; S3: Preparation of hardness layer 3; Keeping the substrate 1 temperature constant, the working gas was adjusted to an Ar / O2 / N2 mixture (Ar as the carrier gas), with an O2 / N2 volume ratio of 1:3.5, and the sputtering power density was increased to 6 W / cm². 2 High-energy pulsed magnetron sputtering technology was used to sputter an AlSi target (Si content 30 at%) with a pulse frequency of 550 Hz and a duty cycle of 12%. Ar ion source was turned on to assist in bombardment, and the ion energy was controlled at 90 eV. The deposition continued until the thickness of the hard layer 3 was ≥0.6 μm. S4: Interference layer 4 deposition; Keeping the vacuum level of S3 and the temperature of substrate 1 constant, the deposition was switched to alternating SiO2 target and TiO2 target, with a total of 6 deposition cycles. The sealing layer was a 15nm thick SiO2 layer, and the total thickness of the interference layer 4 was ≥0.2μm. S5: Anti-fouling layer 5 deposition; Maintain the S4 vacuum chamber environment, use a molybdenum boat electrode, apply a current of 150mA, evaporate the AF antifouling liquid, deposit for 5 minutes, and form an antifouling layer with a thickness ≥0.3μm. S6: Post-processing; Turn off the ion source and sputtering power supply, maintain the vacuum chamber environment, and cool substrate 1 to room temperature at a cooling rate of ≤5℃ / min. After cooling, remove substrate 1 and irradiate it at a wavelength of 365nm and an irradiation intensity of 500mW / cm². 2 UV curing for 10 minutes forms a wear-resistant AR coating for optical components on the surface of substrate 1.

[0024] Example 3: This example provides a method for preparing a wear-resistant AR coating for optical components, including the following steps: S1: Pretreatment of substrate 1; High-transparency optical glass substrate 1 was selected, ultrasonically cleaned with 8wt% detergent at 75kHz for 22min, rinsed with 39℃ deionized water for 240s, dried at 46℃ for 25min, Ar was introduced, and plasma activation was performed at 305W for 5min. Then, it was immersed in a 1.2% silane coupling agent solution (solvent is ethanol and deionized water in a volume ratio of 4:1), soaked at room temperature for 20min, and cured at 128℃ for 32min to obtain pretreated substrate 1. The silane coupling agent is B-201 silane coupling agent; S2: Drilling the bottom layer of sedimentation; The pretreated substrate 1 is placed in the vacuum chamber of the magnetron sputtering equipment, and the vacuum is evacuated to 5×10⁻⁶. -4 Below Pa, heat to 230℃ and hold for 22 min, then introduce O2 at a flow rate of 20 sccm, adjust the oxygen partial pressure to 0.14 Pa, and set the sputtering power density to 4.5 W / cm². 2Alternately sputter Si and Ti targets, and control the interlayer period to 10nm by controlling the sputtering time of each target, and continue to deposit until the thickness of the bottom layer 2 is ≥0.2μm; S3: Preparation of hardness layer 3; Keeping the substrate temperature constant, the working gas was adjusted to an Ar / O2 / N2 mixture (Ar as the carrier gas), with an O2 / N2 volume ratio of 1:3, and the sputtering power density was increased to 5 W / cm². 2 High-energy pulsed magnetron sputtering technology was used to sputter an AlSi target (Si content 28 at%) with a pulse frequency of 520 Hz and a duty cycle of 11%. Ar ion source was turned on to assist in bombardment, and the ion energy was controlled at 75 eV. The deposition continued until the thickness of the hard layer 3 was ≥0.6 μm. S4: Interference layer 4 deposition; Keeping the vacuum level of S3 and the temperature of substrate 1 constant, the deposition was switched to alternating SiO2 target and TiO2 target, with a total of 5 deposition cycles. The sealing layer was a 12nm thick SiO2, and the total thickness of the interference layer 4 was ≥0.2μm. S5: Anti-fouling layer 5 deposition; Maintain the S4 vacuum chamber environment, use a molybdenum boat electrode, apply a current of 120mA, evaporate the AF antifouling liquid, deposit for 5 minutes, and form an antifouling layer with a thickness ≥0.3μm. S6: Post-processing; Turn off the ion source and sputtering power supply, maintain the vacuum chamber environment, and cool substrate 1 to room temperature at a cooling rate of ≤5℃ / min. After cooling, remove substrate 1 and irradiate it at a wavelength of 365nm and an irradiation intensity of 500mW / cm². 2 UV curing for 10 minutes forms a wear-resistant AR coating for optical components on the surface of substrate 1.

[0025] Comparative Example 1: The difference between this comparative example and Example 3 is that in the bottom layer 2, only the Si target is sputtered, and there is no Ti target.

[0026] Comparative Example 2: The difference between this comparative example and Example 3 is that in S3, the volume ratio of O2 / N2 is 1:1.

[0027] Comparative Example 3: The difference between this comparative example and Example 3 is that in S4, the sealing layer is a 20nm thick TiO2.

[0028] Comparative Example 4: The difference between this comparative example and Example 3 is that UV curing was not performed in S6.

[0029] Experiment Example 1: Pencil Hardness Test; Using a 7H Mitsubishi test pencil lead, apply 750gf pressure, with the pencil lead at a 45° angle to the surface to be tested, and make 5 strokes at the test location, each stroke being 20mm long. Acceptance criteria: After testing, no permanent indentations are allowed on the surface of the abrasion-resistant AR coating, and no visible scratches or abrasions are allowed on the surface of the abrasion-resistant AR coating in other locations.

[0030] The results are shown in Table 1: Table 1 Sample number Test Results Surface scratches after testing Test Conclusion Example 1 9H No scratches qualified Example 2 9H No scratches qualified Example 3 9H No scratches qualified Comparative Example 1 8H No scratches qualified Comparative Example 2 8H Minor scratches Unqualified Comparative Example 3 8H Minor scratches Unqualified Comparative Example 4 7H Scratches Unqualified Experiment Example 2: Friction Resistance Test; Using a Minoan eraser and a 1000g weight, at a speed of 40 cycles / min and a test stroke of 40mm, the test was repeated 7500 times on the coated surface of the Coverglass.

[0031] Criteria for passing the test: Initial water droplet angle ≥110°, 5 test points on the sample; 3 test points within the test stroke, water droplet angle >100° after friction; no coating peeling is observed in the appearance.

[0032] The results are shown in Table 2: Table 2 Sample number Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Angle of water droplet before friction 1 115.24 116.18 116.62 112.66 105.77 111.67 112.66 Angle of water droplet before friction 2 117.15 115.49 115.70 112.71 105.84 112.08 111.73 Angle of water droplet before friction 3 116.24 116.05 116.30 112.89 106.21 112.22 111.95 Angle of water droplet before friction 4 116.65 115.21 116.68 113.62 107.07 113.05 112.04 Water droplet angle before friction 5 115.99 115.31 116.67 110.55 105.99 110.24 111.91 Angle of water droplet after friction 1 105.98 106.82 106.08 102.33 96.44 99.67 97.86 Angle of water droplet after friction 2 105.30 106.41 105.77 101.97 99.27 97.35 96.43 Water droplet angle 3 after friction 105.53 106.43 105.34 102.21 99.88 97.88 96.21 Appearance after friction No damage No damage No damage No damage Damaged Damaged Damaged Test Conclusion qualified qualified qualified qualified Unqualified Unqualified Unqualified Experiment Example 3: Alkaline Sweat Test; The CG was wrapped in ISO alkaline sweat and placed in an incubator for 24 hours before being removed and the water droplet angle was measured.

[0033] The preparation method for ISO alkaline sweat is as follows: Add 20.00±0.01g of sodium chloride (analytical grade), 17.50±0.01g of NH4Cl (analytical grade), 5.00±0.01g of urea (analytical grade), 15ml of 85% lactic acid (analytical grade), and 2.5ml of anhydrous acetic acid (analytical grade) to a 1000ml glass beaker. Add pure water to 1000ml and stir thoroughly to completely dissolve the solid powder. Calibrate the pH meter and measure the pH value of the liquid. Carefully add NaOH solution dropwise to the mixed solution using a pipette to bring the pH value to 9.5. Acceptance criteria: Initial water droplet angle ≥110°, 5 test points on the sample; water droplet angle ≥100° after alkaline sweat corrosion; no coating peeling on the surface.

[0034] The results are shown in Table 3: Table 3 Sample number Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Water droplet angle 1 before testing 115.13 115.51 116.72 111.33 106.87 113.85 114.66 Water droplet angle 2 before testing 118.24 117.42 114.10 111.29 106.55 113.54 113.72 Water droplet angle 3 before testing 117.87 117.79 117.40 112.06 105.82 112.27 115.88 Water droplet angle 4 before testing 118.48 118.18 115.68 112.41 110.65 112.94 113.21 Water droplet angle 5 before test 118.25 115.91 114.48 111.98 110.24 112.21 112.62 Water droplet angle 1 after testing 113.52 114.46 112.51 95.77 102.21 108.55 105.42 Water droplet angle 2 after testing 113.76 112.72 112.89 96.23 101.89 106.71 106.11 Water droplet angle 3 after testing 113.77 114.52 113.32 94.88 101.43 102.98 105.75 Water droplet angle 4 after testing 112.19 114.07 113.39 97.61 101.59 101.73 105.82 Water droplet angle 5 after testing 114.29 114.24 112.60 97.62 97.68 105.99 106.04 Appearance after testing No damage No damage No damage Damaged Damaged No damage No damage Test Conclusion qualified qualified qualified Unqualified Unqualified qualified qualified Experiment Example 4: Mohs Hardness Test; Standard Mohs hardness pen (such as Mineralab), automatic hardness tester, 750gf pressure, test at a 90° angle between the pen tip and the sample; Acceptance criteria: S standard ≥ 7, A standard ≥ 5, B standard ≥ 4.

[0035] The results are shown in Table 4: Table 4 Sample number Test Results Surface scratches after testing Test Conclusion Example 1 6 No scratches qualified Example 2 6 No scratches qualified Example 3 6 No scratches qualified Comparative Example 1 5 No scratches qualified Comparative Example 2 5 No scratches qualified Comparative Example 3 5 No scratches qualified Comparative Example 4 4 Scratches Unqualified Experiment Example 5: UV Aging Test; 12 cycles, each lasting 8 hours, including 4 hours of UV light irradiation (UV-A, 340nm, 0.63W / m²). 2 / nm and 60°C) and 4 hours (50°C) of humidity exposure; Acceptance criteria: Initial water droplet angle ≥111°, tested at 3 points; Water droplet angle after UV treatment >100°, tested at 3 points; No coating peeling is observed in appearance; General principles for color difference control (visual inspection + digital quantification using a colorimeter): 4. If the color does not change visually after the test and the color difference value is within the control range, it is deemed qualified; 5. After the test, if the color does not change visually and the color difference value exceeds the control range, it is deemed qualified; 6. If the color changes visually after the test, but the color difference value is within the control range, it is deemed qualified; 7. If the color changes visually after the test and the color difference value exceeds the control range, it is deemed unqualified; Color difference control range: delta E≤3.

[0036] The results are shown in Table 5: Table 5 Sample number Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Initial teardrop angle position 1 115.83 114.90 117.52 113.53 116.63 114.82 102.42 Initial teardrop angle position 2 114.25 115.42 115.68 114.42 118.38 115.61 103.21 Initial teardrop angle position 3 115.60 115.32 118.18 113.65 117.23 114.73 102.64 Initial teardrop angle position 4 116.27 115.61 115.42 115.61 116.25 114.55 103.01 Initial teardrop angle position 5 118.36 118.83 117.56 114.77 118.46 115.28 102.73 UV-treated water droplet angle position 1 112.19 112.57 112.62 108.55 111.78 98.92 92.84 UV-treated water droplet position 2 114.36 114.26 114.97 109.67 112.25 102.44 93.26 UV-treated water droplet angle position 3 111.77 112.94 114.28 108.72 111.97 101.68 94.20 UV-treated water droplet angle position 4 109.62 112.09 113.52 109.41 109.25 103.5 93.87 UV-treated water droplet position 5 110.65 111.63 113.22 108.92 106.33 102.71 93.61 Color difference value delta E≤3 0.12 0.15 0.20 0.57 0.64 0.81 3.4 Test Conclusion qualified qualified qualified qualified qualified Unqualified Unqualified Experiment Example 6: Optical Testing of the Visible Zone; The test was conducted in a darkroom. The measuring instrument used was a Konica CM3600A test device with a D65 light source, an observation angle of 10°, a spot diameter of 25.4 mm, a xenon lamp, and a test wavelength of 360-740 nm. Transmittance of the VA region, at a wavelength of 550nm, the test area is selected as the VA region on the front of the sample; VA region reflectivity, 550nm wavelength, the test area is selected as the VA region on the front of the sample; For the haze test, refer to ASTM 1003 A or B standard, and select the VA area on the front of the sample for testing. Acceptance criteria: transmittance ≥ 90.5%, reflectance ≤ 9%, haze ≤ 0.18, a value = 0 ± 1, b value = 0.4 ± 0.4.

[0037] The results are shown in Table 6: Table 6 project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 value of a -0.09 -0.09 -0.06 -0.17 -0.14 -0.4 -0.2 b value 0.81 0.85 0.9 0.84 0.82 1.7 0.88 transmittance % 94.49 94.44 94.42 91.33 92.21 89.87 90.58 Haze 0.08 0.09 0.09 0.12 0.13 0.22 0.15 Reflectivity % 4.97 4.96 4.98 5.89 5.64 5.66 6.73 Test Conclusion qualified qualified qualified qualified qualified Unqualified qualified As shown in Tables 1-6, the wear-resistant AR coating prepared in the embodiments of the present invention performs excellently in hardness-related tests, meeting the requirements for high light transmittance and high hardness, and the surface is not easily scratched; it has good abrasion resistance, maintaining good surface characteristics after friction, with no coating peeling; in alkaline sweat environment, the coating has strong stability, and its appearance and key performance are not significantly affected; the Mohs hardness reaches the qualified standard, providing a reliable abrasion resistance basis; after UV aging test, the water droplet angle, appearance, and color difference of the coating all meet the requirements, demonstrating excellent anti-aging ability; in terms of optical performance, the transmittance, reflectance, haze, and color difference values ​​all meet the qualification criteria; Comparative Example 1, due to the lack of Ti target and the sputtering of only Si target in the bottom layer, has insufficient resistance to alkaline sweat corrosion and the coating is damaged. This shows that the addition of Ti target is crucial to improving the bonding stability between the film and the substrate and enhancing corrosion resistance. In Comparative Example 2, the O2 / N2 volume ratio in the preparation of the hardness layer was adjusted to 1:1, which deviated from the ratio range specified in this invention, resulting in a decrease in pencil hardness, coating damage in the abrasion resistance test, and failure to meet the alkaline sweat corrosion resistance standard. Comparative Example 3 replaced the SiO2 sealing layer of the interference layer with a 20nm thick TiO2. Not only did the transmittance, haze and color difference values ​​fail to meet the requirements in the optical test, but the abrasion resistance and UV aging tests also failed. This shows that the material and thickness of the SiO2 sealing layer are crucial to maintaining the optical performance and protective stability of the coating. Comparative Example 4 omitted the UV curing step in the post-processing, resulting in the pencil hardness and Mohs hardness not meeting the standards, surface scratches, and a significant decrease in abrasion resistance and UV aging resistance. This fully demonstrates that UV curing can effectively improve the overall adhesion and structural stability of the film.

[0038] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing a wear-resistant AR coating for optical components, characterized in that, Includes the following steps: S1: Substrate pretreatment; Select a substrate, rinse and dry it, introduce Ar, activate it with plasma, immerse it in a silane coupling agent solution, and cure it to obtain a pretreated substrate; S2: Drilling the bottom layer of sediment; The pretreated substrate is placed in the vacuum chamber of the magnetron sputtering equipment, evacuated and heated to 200-250℃ and kept at that temperature, O2 is introduced, and Si targets and Ti targets are sputtered alternately until the underlayer thickness is ≥0.2μm. S3: Hardness layer preparation; Keeping the substrate temperature constant, the working gas is adjusted to an Ar / O2 / N2 mixed gas. High-energy pulsed magnetron sputtering technology is used to sputter the AlSi target, and Ar ion source-assisted bombardment is turned on to continuously deposit until the hard layer thickness is ≥0.6μm. S4: Interference layer deposition; Keeping the vacuum level and substrate temperature constant in S3, switch to alternating deposition of SiO2 target and TiO2 target, set a total of 4-6 deposition cycles, and the total thickness of the interference layer is ≥0.2μm; S5: Anti-fouling layer deposition; Maintain the S4 vacuum chamber environment, use a molybdenum boat electrode, pass current to evaporate the AF antifouling liquid, and deposit an antifouling layer with a thickness ≥0.3μm; S6: Post-processing; Turn off the ion source and sputtering power supply, maintain the vacuum chamber environment, and allow the substrate to cool to room temperature. After cooling, remove the substrate and UV cure it to form a wear-resistant AR coating for optical components on the substrate surface.

2. The method for preparing a wear-resistant AR coating for optical components according to claim 1, characterized in that, S1 specifically involves: ultrasonically cleaning the substrate with a 5-10 wt% washing solution at 70-90 kHz for 15-25 min, rinsing with deionized water at 38-42℃ for 200-300 s, drying at 40-60℃ for 20-30 min, then introducing Ar and performing plasma activation at 280-320 W for 4-8 min, immersing in a 0.8-1.5% silane coupling agent solution at room temperature for 15-25 min, and curing at 120-140℃ for 25-35 min to obtain the pretreated substrate.

3. The method for preparing a wear-resistant AR coating for optical components according to claim 1, characterized in that, The silane coupling agent is silane coupling agent N3112, silane coupling agent KH-550, or B-201 silane coupling agent.

4. The method for preparing a wear-resistant AR coating for optical components according to claim 1, characterized in that, S2 specifically involves placing the pretreated substrate into the vacuum chamber of the magnetron sputtering equipment and evacuating it to a vacuum level of 5 × 10⁻⁶. -4 Below Pa, heat to 200-250℃ and hold for 15-25 minutes, then introduce O2 at a flow rate of 18-22 sccm, adjust the oxygen partial pressure to 0.13-0.17 Pa, and set the sputtering power density to 3-5 W / cm. 2 The Si and Ti targets are sputtered alternately, and the interlayer period is controlled to be 8-12nm by controlling the sputtering time of each target, and the deposition continues until the bottom layer thickness is ≥0.2μm.

5. The method for preparing a wear-resistant AR coating for optical components according to claim 1, characterized in that, S3 specifically involves maintaining a constant substrate temperature, adjusting the working gas to an Ar / O2 / N2 mixture, and increasing the sputtering power density to 4-6 W / cm². 2 High-energy pulsed magnetron sputtering technology was used to sputter AlSi targets with a pulse frequency of 450-550Hz and a duty cycle of 8-12%. Ar ion source was turned on to assist in bombardment, and the ion energy was controlled at 70-90eV. The deposition continued until the hard layer thickness was ≥0.6μm.

6. The method for preparing a wear-resistant AR coating for optical components according to claim 5, characterized in that, The AlSi target contains 20-30 at of Si.

7. The method for preparing a wear-resistant AR coating for optical components according to claim 5, characterized in that, In the working gas, Ar is the carrier gas, and the volume ratio of O2 / N2 is 1:2.5-3.

5.

8. The method for preparing a wear-resistant AR coating for optical components according to claim 1, characterized in that, In S4, the sealing layer is SiO2 with a thickness of 10-15nm.

9. An abrasion-resistant AR coating for optical components prepared by the preparation method according to any one of claims 1-8.

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