A method for preparing anti-glare glass

Abstract

The application discloses a preparation method of anti-dazzle glass, which comprises the following steps: surface cleaning treatment of a glass substrate; coating a film layer on the surface of the glass substrate; coating photoresist on the film layer; performing exposure, development and film layer etching treatment; through dry etching, the longitudinal depth of the glass is directionally etched, and then through wet etching, the longitudinal and transverse directions are etched at the same time, so that a certain depth-width ratio is obtained, the anti-dazzle area is increased, or the surface of the glass is preliminarily shaped through wet etching, and then the dry etching is used to realize accurate depth control and feature shaping in a specific area. The anti-dazzle performance can be effectively improved and is close to the disorder diffusion effect of frosting; the surface texture distribution is more uniform, and the defects that the flash points are different and the surface microstructure is difficult to accurately control in the traditional frosting process are overcome; the microstructure is directly formed on the glass substrate through the etching process, and the reliability requirement in various harsh use environments can be met.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of anti-dazzle glass, in particular to a preparation method of anti-dazzle glass. BACKGROUND

[0002] With the rapid development of display technology, anti-glare (AG) glass as a key optical component to improve display effect, its preparation process has undergone continuous innovation and evolution. Currently, the preparation methods of AG glass mainly include chemical frosting process, yellow light exposure and development process and spraying AG process. These methods have their own advantages and limitations in practical application.

[0003] The traditional chemical frosting process uses frosting powder and other chemical reagents to wet etch the glass surface to form a random distribution of micron-level rough structure. Although this process has the characteristics of low cost and simple operation, due to the randomness of chemical reaction, the size and distribution of the surface microstructure are difficult to control accurately, which affects the optical performance and batch consistency of the product. At the same time, the rough surface formed by the frosting process is easy to accumulate dirt and has certain defects.

[0004] The yellow light exposure and development process borrows from the photolithography technology in semiconductor manufacturing, which coats photoresist on the glass surface, uses a mask (MASK) for selective exposure and development, and finally uses wet etching to transfer the microstructure pattern to the glass substrate. This method can achieve precise control of microstructure size, shape and arrangement, but the traditional wet etching process has obvious limitations in forming high aspect ratio microstructures due to its isotropic characteristics, which directly affects the anti-glare effect and flash point control of AG glass.

[0005] The spraying AG process forms a functional layer with scattering effect by spraying coating containing specific components on the glass surface. This method is simple and efficient, but the adhesion and durability of the coating often cannot meet the requirements of high-end display products, and it is easy to age or peel off in some application environments, limiting the service life.

[0006] With the development of display technology towards high definition and large size, the performance requirements of AG glass are continuously improved. Especially in the fields of medical display, professional image processing and other fields, higher requirements are put forward for anti-glare effect and flash point control. However, the existing pure wet etching process encounters a bottleneck in improving the performance of microstructure, and it is difficult to achieve excellent anti-glare performance and low flash point characteristics at the same time.

[0007] With the rapid development of display technology, AG glass plays an increasingly important role in improving display effects. However, the existing AG glass preparation technology still has obvious shortcomings in optical performance, display effect, etc., and it is difficult to meet the increasing performance requirements of high-end display field. The current mainstream preparation methods such as sandblasting etching method, yellow light exposure development etching method and spraying method all face technical bottlenecks that are difficult to break through; the existing technology has the following defects:

[0008] 1. The sandblasting etching method uses sandblasting powder with disordered particle size distribution to etch the glass surface, which has random distribution characteristics, and therefore has excellent anti-glare performance. However, due to the different particle sizes of sandblasting powder and the difficulty in accurate control, the etching process inevitably brings problems such as uneven flash points and unstable surface roughness. Especially in the environment of high brightness, the uneven distribution will produce local strong reflection or glare points, affecting the consistency and aesthetics of the overall product. In addition, the sandblasting powder from different batches or different suppliers may have differences in particle morphology and chemical properties, further amplifying the volatility of the production process. The fluctuations of process parameters such as temperature, concentration and time during preparation will cause significant differences in product quality, restricting the realization of large-scale production.

[0009] 2. The yellow light exposure development etching method borrows from the photolithography technology of semiconductor industry, and realizes precise control of microstructure through MASK pattern. This method can form microstructures with uniform size and controllable distribution, so it performs well in flash point control. However, due to the regularity of MASK pattern, the arrangement of microstructures formed is relatively orderly, lacking sufficient randomness, resulting in anti-glare performance inferior to sandblasting process. Especially when observed at a large viewing angle, the regularly arranged microstructures may produce optical interference, affecting the display quality. At the same time, the traditional wet etching process is isotropic in nature, making it difficult to form an ideal aspect ratio, which further limits the improvement of anti-glare performance.

[0010] 3. The spraying method uses spraying of materials containing specific particles on the glass surface to form a functional layer. Although this additive process is simple to operate, it has serious reliability problems. The most prominent defect is that its wear resistance is much lower than that of subtractive processes such as sandblasting and yellow light exposure development etching. This is because the sprayed layer, as a functional coating added to the glass surface, has a weaker bond with the substrate than the microstructures formed by chemical reaction or physical etching. In practical applications, the sprayed layer is easily damaged or peeled off due to mechanical effects such as friction and impact, resulting in a significant reduction in product service life. In addition, the uniformity and repeatability of the spraying process are difficult to guarantee, affecting the stability of product quality.

[0011] As disclosed in a kind of AG anti-glare glass preparation method of patent CN119143400A, comprising the following steps: surface treatment is carried out to glass substrate;Uniformly coat a layer of functional coating on the surface of glass substrate;Uniformly coat photoresist on the surface of functional coating, carry out soft baking treatment after coating;High-precision MASK is used to carry out pattern design and exposure, and the microstructure pattern designed accurately is transferred to photoresist layer;After exposure, development treatment is carried out, and the part of photoresist not exposed is removed, and predetermined pattern is formed on glass substrate;The photoresist pattern after development is cured, to ensure that it has enough etching resistance and stability in subsequent etching process;Etching treatment is carried out, and the functional coating and glass substrate not protected are removed, and accurate microstructure pattern is formed;Using photoresist removal technology, residual photoresist is removed, and the final microstructure pattern is obtained;The surface of microstructure pattern is functionalized by fluorination treatment;Anti-glare effect needs to be improved. SUMMARY

[0012] In view of the deficiencies in the prior art, the present application provides an anti-glare glass preparation method to achieve better anti-glare effect and flash point.

[0013] To solve the above technical problems, the technical scheme adopted by the present application is as follows:

[0014] The anti-glare glass preparation method comprises the following steps:

[0015] Step 1: surface cleaning treatment of glass substrate;

[0016] Step 2: coating a film layer on the surface of glass substrate;

[0017] Step 3: coating photoresist on the film layer;

[0018] Step 4: exposure, development and film layer etching treatment;

[0019] Step 5: by dry etching, directional etching longitudinal depth of glass, then by wet etching method, etching longitudinal and transverse at the same time, to obtain a certain depth-width ratio, increase anti-glare area; or, first, wet method is used to construct the morphology of glass surface, then dry etching is used to realize accurate depth control and feature shaping in specific area.

[0020] Further or preferably:

[0021] The process flow in step 5 is:

[0022] Dry etching glass→photoresist removal→wet etching glass 1→film layer removal→wet etching glass 2;

[0023] Or, dry etching glass→wet etching glass 1→photoresist removal→film layer removal→wet etching glass 2;

[0024] Or, stripping photoresist→dry etching glass→wet etching glass 1→stripping film layer→wet etching glass 2;

[0025] Or, stripping photoresist→wet etching glass 1→dry etching glass→stripping film layer→wet etching glass 2;

[0026] Or, wet etching glass 1→stripping photoresist→dry etching glass→stripping film layer→wet etching glass 2;

[0027] Or, wet etching glass 1→dry etching glass→stripping photoresist→stripping film layer→wet etching glass 2.

[0028] In the step 1, the substrate surface is first rinsed with deionized water, and dust and organic impurities are removed by soft brush or ultrasonic means; or, a cleaning agent or solvent is added for degreasing and oil removal treatment, the treatment temperature is in the range of 20-100℃, and the treatment time is 1-10min.

[0029] In the step 2, the thickness of the film layer is in the range of 50-3000A, and the film layer is generated by vacuum coating or evaporation.

[0030] In the step 3, the thickness of the photoresist is in the range of 0.5-20μm; the coating method is slot coating, the coating speed is controlled between 10-200mm / s, and the spraying pressure is controlled between 0.03-0.98MPa; after coating, soft baking is performed, the soft baking temperature is controlled between 50-200℃, and the time is 30-300 seconds.

[0031] In the step 4, in the exposure process, according to the batch quantity and resolution requirement, a contact, near or projection exposure machine is selected; the exposure energy is between 50-500mJ / cm 2 .

[0032] In the step 4, the developing time is about 30-90s, and the temperature is maintained at 20-30℃; the conductivity of the developing solution should be maintained in the range of 1-80mS / cm; after developing, post-baking is performed, the temperature is in the range of 50-300℃, and the duration is 1-20min.

[0033] In the step 4, before etching the film layer, the photoresist pattern needs to be cured, heat curing or UV curing is performed in the temperature range of 50-500℃ for 1-60min, so as to enhance the etching resistance and mechanical strength of the photoresist pattern, and prevent deformation or delamination during etching.

[0034] In the step 5, the dry etching process is as follows:

[0035] The dry etching step uses an inductively coupled plasma technology to realize precise microstructure processing of the anti-dazzle glass; the dry etching is directional etching of the glass by using a plasma etching technology;

[0036] In terms of process parameter setting, the vacuum system needs to be maintained in a vacuum state of 0.1-10 Torr to ensure the stability of the plasma and the sufficient dissociation of the gas; in terms of gas flow, the flow of the main etching gas (C4F6 and SF6) is controlled in the range of 50-200 sccm, the flow of the inert gas (such as Ar or He) is set to 50-150 sccm, and if O2 is added, it is controlled in the range of 5-20 sccm.

[0037] In step 5, the wet etching stage, chemical reagents are used for all-around etching of the microstructure, realizing a key transition from a simple longitudinal recess to a complex three-dimensional structure, and the wet etching is performed in the horizontal and vertical directions at the same time.

[0038] Compared with the prior art, the present application has the following advantages:

[0039] The dry and wet etching combined AG glass preparation method provided by the present application innovatively combines dry etching and wet etching processes, and has made a significant breakthrough in anti-glare performance, flash point control and wear resistance, etc., providing a new technical solution for the high-end display field. The specific embodiments are as follows:

[0040] In terms of anti-glare performance, the present application fully utilizes the process advantages of dry and wet etching. First, a basic structure with a high aspect ratio is formed by dry etching, and then fine adjustment is performed by wet etching with an optimized ratio, finally realizing an anti-glare effect comparable to that of the traditional sandblasting process. This composite process not only provides a larger scattering area, but also ensures the stability and repeatability of product performance through accurate parameter control, solving the problem of uncontrollable microstructure in the traditional sandblasting process.

[0041] In terms of flash point control, the present application uses the same photolithography technology as the yellow light exposure and development process as the pattern transfer means, realizes the uniform distribution of the microstructure through the accurate design and transfer of the MASK pattern. Combined with the synergistic effect of dry and wet etching, the flash phenomenon is effectively suppressed while maintaining excellent anti-glare performance. This precisely controllable preparation method enables the product to maintain excellent display effect in a high-brightness display environment, significantly improving the user experience.

[0042] In terms of wear resistance, the application is completely based on subtractive process, which overcomes the inherent defects of insufficient coating adhesion in spray coating. In particular, the high aspect ratio structure formed by dry etching provides an ideal basis for subsequent wet etching, making the final microstructure firmly combined with the glass substrate. Experiments show that the AG glass prepared by the application performs best in wear resistance test, far superior to traditional spray coating process, and also better than products prepared by single frosting or yellow light process.

[0043] In addition, the application has obvious advantages in process controllability. By accurately controlling the process parameters of dry and wet etching, the aspect ratio, morphology and distribution density of the microstructure can be flexibly adjusted to meet the needs of different application scenarios for optical performance; at the same time, the process has good repeatability and high stability, which is beneficial to the large-scale production of products. BRIEF DESCRIPTION OF DRAWINGS

[0044] The content expressed by each figure in the specification and the marks in the figures are briefly described as follows:

[0045] Figure 1 Figure 1 is a schematic diagram of the preparation process of the application.

[0046] Figure 2 Figure 2 is a schematic diagram of the preparation process of the application.

[0047] Figure 3 Figure 3 is a schematic diagram of the preparation process of the application.

[0048] Figure 4 Figure 4 is a schematic diagram of the preparation process of the application.

[0049] Figure 5 Figure 5 is a schematic diagram of the preparation process of the application.

[0050] Figure 6 Figure 6 is a schematic diagram of the preparation process of the application.

[0051] Figure 7 Figure 7 is a schematic diagram of the yellow light AG preparation process of the application.

[0052] Figure 8 Figure 8 is a schematic diagram before dry etching of the application.

[0053] Figure 9 Figure 9 is a schematic diagram after dry etching of the application.

[0054] Figure 10 Figure 10 is a schematic diagram after dry etching + wet etching of the application.

[0055] Figure 11 Figure 11 is a schematic diagram of Figure 10 Figure 12 is a schematic diagram of removing photoresist.

[0056] Figure 12Schematic diagram of the present application after removing the blocking layer.

[0057] Figure 13 Schematic diagram of the present application for comparison between dry and wet etching structures. DETAILED DESCRIPTION

[0058] The specific embodiments of the present application will be further described in detail with reference to the accompanying drawings.

[0059] The preparation method of the anti-glare glass comprises the following steps:

[0060] Step 1: surface cleaning treatment of the glass substrate;

[0061] Step 2: coating a film layer on the surface of the glass substrate;

[0062] Step 3: coating photoresist on the film layer;

[0063] Step 4: exposure, development and film layer etching treatment;

[0064] Step 5: through dry etching, directional etching of the longitudinal depth of the glass, and then through wet etching, etching of the longitudinal and transverse directions at the same time, to obtain a certain aspect ratio and increase the anti-glare area; or, first, through wet etching, preliminary topography construction on the glass surface, and then using dry etching to realize precise depth control and feature shaping in a specific area.

[0065] The present application makes key improvements on the basis of the traditional photoexposure, development and etching method. In the first process route, the glass is first directional etched longitudinally by dry etching, so as to pre-shape the structure features with a certain depth on the glass surface. The subsequent wet etching can continue to etch in the longitudinal and transverse directions at the same time, expand the existing vertical grooves in the transverse direction and further deepen them, so as to obtain a relatively large aspect ratio. Through this "dry first and then wet" composite etching process, both the transverse and longitudinal directions are taken into account.

[0066] The present application also innovatively proposes a second process route, that is, first, using wet etching to construct the preliminary topography on the glass surface to form a basic microstructure with a certain opening width, and then using dry etching technology to accurately etch the longitudinal direction of the microstructure bottom to form a multi-level structure of pit-in-pit. This "wet first and then dry" process sequence can maintain the advantage of transverse expansion of wet etching, and further increase the longitudinal depth through the high directionality of dry etching, to realize fine regulation of the microstructure bottom area.

[0067] The following effects are finally achieved: ① at a deep level, the grooves and structures are more obvious, the overall surface area is increased, and the anti-glare performance can be effectively improved and is close to the disorder diffusion effect of sandblasting; ② the surface texture ensures that the microstructure distribution is more uniform under the synergistic action of mask exposure, and overcomes the defects that the flash points are not the same and the surface microstructure is difficult to accurately control in the traditional sandblasting process; ③ compared with the spraying method which only covers a functional coating on the surface of the glass, the etching process is adopted in the present application to directly form microstructures on the glass substrate, and the surface texture derived from the material body has the natural wear resistance advantage, which can meet the reliability requirements in various harsh environments.

[0068] The preferred specific examples of the present application are:

[0069] The present application proposes an innovative dry-wet etching combined process. The method combines the directionality advantage of dry etching and the uniformity characteristics of wet etching, and realizes accurate control of the microstructure morphology through multi-step synergistic action. That is, on the basis of the traditional yellow light exposure development etching method, the process performance is broken through by introducing a dry etching step. According to the cooperation mode of the film layer and the photoresist and the sequence of dry and wet etching, six main process routes are divided (as shown in Figures 1 to 6 Fig. 1-6):

[0070] Process 1: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→dry etching glass→photoresist stripping→wet etching glass 1→film layer stripping→wet etching glass 2

[0071] Process 2: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→dry etching glass→wet etching glass 1→photoresist stripping→film layer stripping→wet etching glass 2

[0072] Process 3: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→photoresist stripping→dry etching glass→wet etching glass 1→film layer stripping→wet etching glass 2

[0073] Process 4: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→photoresist stripping→wet etching glass 1→dry etching glass→film layer stripping→wet etching glass 2

[0074] Process 5: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→wet etching glass 1→photoresist stripping→dry etching glass→film layer stripping→wet etching glass 2

[0075] Process 6: glass substrate→coating film layer→coating photoresist→exposure→development→film layer etching→wet etching glass 1→dry etching glass→photoresist stripping→film layer stripping→wet etching glass 2

[0076] The common feature of Process 1 and Process 2 is to retain the film layer and the photoresist simultaneously in the dry etching stage to form a double protection structure, that is, the film layer is first deposited on the glass substrate, and then the photoresist is coated and patterned thereon, and then the microstructure is accurately transferred by using dry etching. This route fully plays the advantages of double protection of photoresist and film layer, and guarantees the high fidelity and morphology stability of the microstructure after dry etching. The difference between the two processes lies in the timing of removing the photoresist: the photoresist is removed immediately after dry etching in Process 1, while the photoresist is removed after completing dry etching and the first wet etching in Process 2.

[0077] The significant feature of Process 3 is to remove the photoresist before dry etching, and only use the film layer as an etching mask. This process route simplifies the process and reduces the adverse effects of the photoresist in the dry etching environment, such as thermal deformation or degradation. By using only the film layer to protect the selected area, the required morphology requirements can also be obtained in the dry etching.

[0078] Processes 4, 5 and 6 are to perform dry etching after wet etching. These routes first use wet etching to preliminarily construct the morphology of the glass surface, and then use dry etching technology to realize precise depth control and feature shaping in specific areas. This "reverse" processing method provides new possibilities for the regulation of microstructure morphology. By forming an initial profile through wet etching, and then using the directional characteristics of dry etching for fine regulation, special surface topography that is difficult to achieve by conventional processes can be obtained.

[0079] The step of removing the photoresist has certain flexibility in the above processes, and the photoresist can be removed at any time according to actual needs to adapt to the optical and mechanical performance requirements at each stage, which is within the scope of protection of the patent.

[0080] The present application preferably uses a dry-wet composite etching process; based on the photoexposure and development, the dry etching with strong directionality is first used to improve the aspect ratio of the microstructure, and then the wet etching is used to optimize the surface morphology, realizing the precise regulation of the geometric characteristics of the microstructure, so as to obtain high-performance AG (anti-glare) glass.

[0081] The dry-wet etching combined AG glass preparation method proposed by the present application innovatively combines dry etching and wet etching processes, and has made significant breakthroughs in anti-glare performance, flash point control and wear resistance, etc., providing a new technical solution for the high-end display field. The specific embodiments are as follows:

[0082] 1. In terms of anti-glare performance, the present application fully utilizes the process advantages of dry and wet etching combination. First, a basic structure with high aspect ratio is formed by dry etching, and then fine adjustment is made by wet etching with optimized ratio, finally achieving anti-glare effect comparable to traditional sandblasting process. This composite process not only provides a larger scattering area, but also ensures the stability and repeatability of product performance through precise parameter control, solving the problem of uncontrollable microstructure in traditional sandblasting process.

[0083] 2. In terms of flash point control, the present application uses the same photolithography technology as the photoexposure and development process as the pattern transfer means, and realizes the uniform distribution of microstructure through precise design and transfer of MASK pattern. Combined with the synergistic effect of dry and wet etching, the flash phenomenon is effectively suppressed while maintaining excellent anti-glare performance. This precisely controllable preparation method enables the product to maintain excellent display effect in high brightness display environment, significantly improving user experience.

[0084] 3. In terms of wear resistance, the present application is completely based on subtractive process, overcoming the inherent defect of insufficient coating adhesion in spraying method. In particular, the high aspect ratio structure formed by dry etching provides an ideal foundation for subsequent wet etching, making the final microstructure firmly combined with the glass substrate. Experiments show that the AG glass prepared by the present application performs best in wear resistance test, far superior to traditional spraying process, and also better than products prepared by single sandblasting or photo process.

[0085] In addition, the present application also has obvious advantages in process controllability. By precisely controlling the process parameters of dry and wet etching, the aspect ratio, topography and distribution density of microstructure can be flexibly adjusted to meet the needs of different application scenarios for optical performance. At the same time, the process has good repeatability and high stability, which is beneficial to the large-scale production of products.

[0086] As shown in Figures 7 to 13 , the specific process of dry and wet etching combination is as follows (the process details and technical parameters of each step will be described in detail below to facilitate understanding of the implementation details of the entire process and its impact on the performance of the final product):

[0087] A. Glass substrate treatment

[0088] First, deionized water is used for preliminary rinsing, and soft brush or ultrasonic means are used to remove dust and organic impurities on the surface of the substrate; if necessary, low-concentration cleaning agents or solvents can be added for degreasing and oil removal treatment. The treatment temperature range is 20-100℃, and the treatment time is 1-10min.

[0089] B. Coating layer

[0090] The film layer plays a crucial role in the present application, as it serves as both a mask for subsequent dry etching and a key element for precise control of microstructure morphology in wet etching processes. The material selection for the film layer can include ITO (Indium Tin Oxide), Cr (Chromium), Mo (Molybdenum), SiO2 (Silicon Dioxide), and Si3N4 (Silicon Nitride), among others. These materials have different characteristics, allowing for flexible selection based on actual process requirements and cost considerations, ensuring that the film layer provides the necessary protection and performance support during etching.

[0091] The thickness of the film layer is typically controlled within the range of 100-2000 (angstroms), with the specific value depending on the process conditions of subsequent dry etching and the requirements for microstructure aspect ratio. A film layer that is too thick may provide better protection but increases etching difficulty and material cost; a film layer that is too thin may be damaged during etching, affecting the integrity of the microstructure.

[0092] The preparation method for the film layer mainly uses vacuum coating or evaporation technology, including but not limited to physical vapor deposition (PVD), chemical vapor deposition (CVD), and sputtering coating, among others. These technologies can form a uniform, dense film on the surface of the glass substrate with good adhesion.

[0093] Specifically, the key parameters for each film layer are as follows: for ITO, argon gas (Ar) is typically used for deposition, with a gas flow of 320-400 sccm, a vacuum degree of 0.5 Pa, a coating temperature range of 150-300°C, a power of 6-8 kW, and a gas supply ratio of 1:0.3. For Cr film layer, the same gas is used, with a flow of 320-400 sccm, a vacuum degree of 0.5 Pa, a temperature range of 200-300°C, a power setting of 5-15 kW, and a gas ratio of 1:0. The preparation of Mo film layer requires a vacuum degree of 0.65 Pa, an Ar gas flow of 350-600 sccm, and an O2 gas flow of 10-40 sccm, with a temperature control of 150-200°C and a power of 6-12 kW, and a ratio of 10-40 sccm. For SiO2 film layer, Ar gas is used, with a gas flow of 100-180 sccm, a vacuum degree of 0.5 Pa, a coating temperature range of 200-300°C, and a power of 10-20 kW. Finally, for Si3N4 preparation, 200-320 sccm of N2 gas and 100-150 sccm of Ar gas are introduced, with a vacuum degree of 0.6 Pa, a temperature range of 200-300°C, a power of 20-45 kW, and a gas ratio of 25-60 sccm.

[0094] Note: The ratio range is determined according to the characteristics of the film layer

[0095] C. Coating photoresist

[0096] The selection of photoresist can be based on the actual process requirements, using positive or negative photoresist material. Positive photoresist increases solubility in the exposed area, and is removed after development; negative photoresist is the opposite, the exposed area is cross-linked and solidified, and is retained after development. Its thickness is usually controlled within the range of 0.5-20 μm to ensure the resolution and accuracy of subsequent pattern transfer.

[0097] The coating method uses slot coating, which is suitable for rapid coating of large-area glass. The coating speed is usually controlled between 10-200 mm / s to ensure uniform coverage. The GAP (gap between the glue layer and the substrate) during coating is kept within the range of 50-300 μm, and the spraying pressure is controlled within the range of 0.03-0.98 MPa. After coating, soft baking is usually required to remove the solvent in the photoresist and improve the adhesion and stability of the photoresist. The soft baking temperature is generally controlled at 50-200°C, and the time is 30-300 seconds. After coating, the photoresist thickness and uniformity can be detected by film thickness tester or optical microscope to ensure that it meets the requirements of subsequent photolithography process.

[0098] D. MASK pattern design and exposure

[0099] In the dry and wet etching combined process of the present application, the MASK pattern design and exposure plays a crucial role in the size accuracy and distribution uniformity of the final microstructure. First, according to the optical requirements of the target AG glass, various patterns such as dot array, line array, honeycomb or polygon can be selected when designing the MASK pattern, and the aperture is usually limited within the range of 1-200 μm. According to the arrangement of patterns of different sizes, various arrangement methods such as normal distribution, exponential distribution, bimodal distribution or random distribution can be realized, so as to realize specific scattering and optical effects for different application scenarios.

[0100] In the exposure process, contact, proximity or projection exposure machines are selected according to the batch size and resolution requirements. The exposure energy is usually between 50-500 mJ / cm 2 , which is determined by the characteristics of the photoresist, the wavelength of the light source and the resolution level. The commonly used UV wavelengths are i-line (365 nm), h-line (405 nm) and g-line (436 nm), and the selection of appropriate wavelength should be based on the specific application requirements and the photosensitivity matching of the photoresist. If multiple layers of exposure are required, the alignment error is controlled within ±0.5-1 μm through a double-sided alignment system to ensure the accurate matching of multiple layers of patterns.

[0101] E. Development

[0102] The developing solution used in the development process is of a specific concentration (such as TMAH tetramethylammonium hydroxide or potassium hydroxide KOH solution), and the development time is generally about 30-90 s, and the temperature is maintained at 20-30°C to obtain a stable development rate and reliable pattern fidelity. In addition, the conductivity of the developing solution should be maintained within the range of 1-80 mS / cm to ensure uniform chemical reactions during the development process. After development is complete, post-baking treatment is also required, with a temperature range of 50-300°C and a duration of 1-20 min to further enhance the etch resistance of the photoresist and stabilize the pattern.

[0103] In actual operation, both immersion and spraying can be used for development. Immersion improves development uniformity by slow stirring, making it easier to control the overall rate; while spraying shortens the development cycle, but places higher requirements on flow rate and nozzle precision. After development is complete, the pattern edges and line width are usually checked using an optical system, online monitoring, or offline CD-SEM (critical dimension scanning electron microscope) to ensure that the development is sufficient and there is no over-etching. After multiple rinsing with deionized water and rapid drying, post-baking at 50-300°C for 1-20 min can be performed as needed to further enhance the etch resistance of the photoresist pattern. Through the above development process, the photoresist layer can accurately reproduce the MASK pattern.

[0104] F. Film layer etching

[0105] Before film layer etching, the photoresist pattern usually needs to be cured. Specifically, thermal curing or UV curing can be performed at a temperature range of 50-500°C for 1-60 min to enhance the etch resistance and mechanical strength of the photoresist pattern, preventing deformation or delamination during etching. After completing the pattern curing, the film layer can be etched.

[0106] The material selection for the film layer can include ITO, Cr, Mo, SiO2, and Si3N4. For different types of film layers, corresponding etching solutions are used for processing: for ITO, Cr, and Mo film layers, a mixed solution of nitric acid or hydrochloric acid is mainly used, with a concentration controlled between 1-10%; for SiO2 film layers, hydrofluoric acid is used, with a concentration usually between 5-20%; and for Si3N4 film layers, phosphoric acid is used, with a concentration range of 10-30%. The specific etching time depends on the film layer thickness (usually ) and the required pattern depth and sidewall precision.

[0107] The etching process needs to be observed and measured in time to ensure that the film pattern is completely transferred but avoid over-etching damage to the substrate. Optical microscopy can be used for rapid detection to evaluate the critical dimensions and pattern edges. After etching, multiple cleaning steps should be performed immediately using deionized water or corresponding cleaning agents to remove etching residues, and finally dried in a clean environment or low-temperature dried. Through the above steps, a film pattern consistent with the photoresist pattern can be obtained on the glass surface, providing accurate area protection and guidance for subsequent dry etching or wet etching steps.

[0108] G. Dry etching process

[0109] The dry etching step uses inductively coupled plasma (ICP) technology to achieve precise microstructure processing of AG glass. This process is particularly suitable for high aspect ratio microstructure requirements based on traditional glass etching technology. The etching process is carried out in a dry etching machine such as a reactive ion etching machine (RIE) or an inductively coupled plasma etching machine (ICP), in which the ICP etching machine generates high-density plasma through inductive coupling, enabling high-selectivity etching of materials such as silicon, silicon dioxide, and metals.

[0110] The core of dry etching is to use plasma etching technology to etch glass directionally. Fluorine-based gases (CF4, C4F8, SF6, etc.) are usually combined with inert gases (Ar, He). C4F6+H2+Ar or C4F6+CH2F2+Ar mixed gas is usually used as the etching gas. Among them, C4F6 serves as the CF X group supply source, ensuring stable supply of CFX groups during etching, generating CF X responsible for chemical reaction with SiO2 on the glass surface; H2 and CH2F2 act as F - removal agents, generating HF gas by combining with free F - ions, effectively controlling the selectivity of the etching reaction, thereby directionally controlling the longitudinal etching depth of the glass; Ar mainly plays a physical bombardment role, using ion bombardment to promote the reaction of CF X groups with SiO2 to improve the etching rate.

[0111] In terms of process parameter settings, the vacuum system needs to be maintained at a vacuum state of 0.1-10 Torr to ensure the stability of the plasma and the sufficient dissociation of the gas. In terms of gas flow, the flow of the main etching gas (C4F6 and SF6) is controlled in the range of 50-200 sccm, the flow of the inert gas (such as Ar or He) is set at 50-150 sccm, and the flow of O2, if added, is controlled at 5-20 sccm. Precise control of these parameters is crucial for etching rate and quality. Too low a flow will result in insufficient supply of reactants, limiting the etching rate, while too high a flow will cause active particles to be discharged without sufficient reaction, reducing the etching effect. Therefore, the flow settings need to be optimized through experiments to find the appropriate optimal range. Power settings are also critical. The ICP source power is usually between 2000-5000 W, which can effectively increase the plasma density and directly affect the etching rate. The RF bias power is adjusted in the range of 1000-3000 W to enhance the dynamics of ion bombardment for better anisotropy. Excessive power may cause damage to the photoresist or film layer, which requires a balance between etching efficiency and material integrity when adjusting the power.

[0112] In the dry etching step of the present application, after the pre-MASK pattern transfer and film layer opening treatment, the surface only forms a hole diameter "a" at the film layer position, as shown in Figure 8 The glass body has not yet been directly etched. By using plasma technology for directional longitudinal etching of the glass, a certain depth "h" can be excavated inside the glass while the hole diameter "a" remains substantially unchanged, as shown in Figure 9 From "a" to "h", the most essential change brought about by dry etching is realized, which is the transition from simple "opening" to actual "recessed structure", and the area originally only with film layer opening gradually evolves into a longitudinal channel or concave area with a controllable depth in the glass body.

[0113] As can be seen from the comparison of Figure 8 and Figure 9 , the microstructure after dry etching is not simply expanded in the "a" direction, but a certain depth (h) is excavated longitudinally into the glass while ensuring that the hole width (a) remains substantially unchanged. The technical principle behind this is that dry etching utilizes the synergistic effect of the components in the C4F6+H2+Ar (or C4F6+CH2F2+Ar) plasma:

[0114] ① C4F6 is ionized and decomposed into CF X groups after being excited by high-energy plasma. These CF X radicals are the main active species that chemically react with SiO2 on the glass surface and chemically combine or bond with SiO2.

[0115] ②H2 or CH2F2 as F - "ion quenchers" that consume free radicals, generate HF volatiles at the etch region, and weaken F - corrosion to non-target areas, thus achieving "directional" etching.

[0116] ③Ar ions vertically bombard the etching region under the acceleration of the electric field, which can not only strip the reaction products but also enhance the anisotropic etching effect of the sidewall, allowing the etching path to be more vertically deepened.

[0117] The synergistic effect of directional etching allows the aperture "a" to maintain its original size, avoiding excessive lateral expansion, but forms a vertical cavity with high depth in the sub-micron to micron range (etching depth h can reach 0.1-10 μm, or even deeper). The high aspect ratio structure formed by dry etching provides an ideal topography for subsequent wet etching. This etching strategy, which prioritizes vertical depth, not only significantly expands the effective scattering area but also provides ample space for fine-tuning of the microstructure later, thereby achieving improved anti-glare performance and effective suppression of the sparkle point.

[0118] From a microscopic perspective, the structural characteristics after dry etching mainly manifest in the sidewall and the bottom: the sidewall presents a relatively flat profile with obvious anisotropic characteristics. Due to the synergistic effect of Ar ion bombardment and CFX free radicals, a micron-scale step may be formed, and the bottom will exhibit a nanoscale microscopic roughness, mainly due to ion bombardment effects and local reaction rate differences during plasma etching. By adjusting parameters such as etching temperature (20-300℃), gas flow ratio, RF power, and working gas pressure, the sidewall angle and bottom morphology can be controlled to some extent.

[0119] H. Wet etching 1

[0120] As shown in Figure 10 , after dry etching, the present invention enters the wet etching stage, which utilizes chemical reagents for all-around etching of the microstructure, achieving a key transition from simple vertical recess to a complex three-dimensional structure. The "b" parameter in the figure represents the etching width and depth in both the lateral and vertical directions during wet etching. This simultaneous expansion is a direct manifestation of the isotropic characteristics of wet etching.

[0121] In the final etching topography, by comparing the morphology after dry etching ( Figure 9 ) with the structure after wet etching ( Figure 10The following significant changes can be observed: ① The microstructure opening width expands from the original "a" to "a+2b", the lateral dimension increases significantly; ② The depth further increases from the dry etching "h" to "h+b", which strengthens the overall aspect ratio; ③ The originally relatively flat sidewall presents a smooth transition after wet etching, and the overall profile of the microstructure is more smooth and continuous. This morphology evolution lays the foundation for subsequent optical performance optimization (Note: In the figure, straight lines are used directly for easy display, but it does not affect the actual etched morphology).

[0122] The wet etching solution is prepared using a single acid or a mixed acid system. It includes but is not limited to HF (hydrofluoric acid) or NH4F (ammonium fluoride) as the main etchant, and can optionally add hydrochloric acid, nitric acid, sulfuric acid, acetic acid, etc. inorganic or organic acids as auxiliary acidic components, such as HF / NH4HF2 mainly providing basic etching capability for silicate structure (mainly SiO2), HCl / HNO3 / H2SO4 / HAc etc. mainly used to adjust the etching rate, buffer reaction byproducts and fine-tune surface roughness, helping to obtain more uniform etching morphology. The process temperature is controlled in the range of 20-50℃, which can ensure sufficient reaction activity and avoid reaction runaway and bubble generation caused by high temperature. The wet etching equipment can be selected as a tank or horizontal etching machine according to the demand.

[0123] I. Photoresist stripping

[0124] Using photoresist removal technology, the remaining photoresist is removed to obtain the final microstructure pattern. The method of removing photoresist can adopt wet removal or dry removal, and the removal time is 1-15min. This step ensures that the surface is free of residual substances to prepare for subsequent processing.

[0125] As shown in Figure 11 , after completing the dry etching and the first wet etching, the photoresist has been completely removed. It needs to be specially pointed out that the photoresist removal step in the present application has high process flexibility, which can adjust its position in the process flow according to the actual demand. The example in the picture only presents one situation, for example, the process steps of stripping photoresist→wet etching glass→stripping membrane layer can also be used. This flexibility makes the process more adaptable, regardless of the sequence used, it belongs to the protection scope of the patent.

[0126] J. Stripping membrane layer

[0127] For the removal of the film layer, the corresponding wet etching solution can be selected according to the properties of the film layer. For ITO, Cr and Mo film layers, a mixed solution of nitric acid or hydrochloric acid is mainly used, with a concentration controlled between 1-10%; for SiO2 film layers, hydrofluoric acid is used, with a concentration usually between 5-20%; and for Si3N4 film layers, phosphoric acid is used, with a concentration ranging from 10-30%. The equipment can be selected according to the production scale, using a tank or horizontal etching machine. The specific etching parameters (such as temperature, time) depend on the film layer material, thickness and the properties of the etching solution used. Generally, the etching temperature is controlled between 20-50°C, and the etching time is adjusted according to the actual situation until the film layer is completely removed. In order to avoid damage to the glass surface caused by excessive etching, the etching process needs to be monitored in real time, and the reaction needs to be stopped in time.

[0128] As shown in Figure 12 , after the removal of the film layer, a specific microstructure morphology is formed on the surface of the glass substrate. The longitudinal depth "h" of the microstructure and the lateral width "a" and "b" together constitute the aspect ratio of the entire structure, and the calculation formula is: aspect ratio = (h+b) / (a+2b). This formula shows that by increasing the longitudinal depth (h), the overall aspect ratio can be effectively improved, thereby expanding the effective area of anti-glare.

[0129] After this series of processes, the microstructure formed finally has excellent anti-glare performance, reaching a similar effect to the traditional sandblasting method, but with better flash control than the sandblasting process.

[0130] As shown in Figure 13 , the dry etching + wet etching (after removing the photoresist and film layer) structure diagram is shown in Figure I : dry etching + wet etching (after removing the photoresist and film layer) structure diagram; Figure II : wet etching (after removing the photoresist and film layer) structure diagram.

[0131] As shown in the figure, there is a significant difference in microstructure morphology between the dry and wet etching combined process (Figure I) and the simple wet etching (Figure II). For the dry and wet etching combined process, a relatively deep etching depth is first formed in the longitudinal direction by dry etching, and then wet etching is used to expand in both the lateral and longitudinal directions. The planar visual area of the microstructure obtained finally can be represented as (a+2b)*(h+b), where "a+2b" represents the final aperture in the lateral direction, and "h+b" represents the superposition of the longitudinal depth and the lateral wall expansion. In contrast, the planar visual area of the microstructure obtained by ordinary wet etching is (a+2b)*b, i.e. a pit with a depth of b and a total lateral width of a+2b is formed on the glass surface, and the effective scattering area is relatively reduced.

[0132] In terms of anti-glare performance, the microstructure etched by the dry-wet combined process is deeper in the longitudinal direction, and its surface area increases approximately exponentially with the etching depth. The larger surface area means that the incident light will experience more scattering and attenuation inside the pits and on the sidewalls under strong light, effectively reducing the intensity of direct light and lowering glare. Such geometric expansion plays a crucial role. The wide and deep pit structure not only disperses light in multiple directions, but also disrupts the coherent path of light to some extent, making the glare sufficiently weakened.

[0133] In addition to the process of first dry etching and then wet etching, the attached Figures 4 to 6 The flow chart of first wet etching 1 and then dry etching is shown. This process shows significant differences in microstructure morphology control and optical performance adjustment:

[0134] In terms of morphology, in the process of first wet etching and then dry etching, the initial wet etching uses its isotropic characteristics to form initial pits with wide openings and flat profiles on the glass surface. At this time, the microstructure already has basic scattering function, but the aspect ratio is relatively limited. The subsequent dry etching further increases the depth of the central region based on these pre-formed pits through highly directional plasma action, forming a "wide mouth and deep bottom" composite structure. This structure combines the large-area scattering characteristics of wet etching and the high aspect ratio characteristics of dry etching. In contrast, the traditional dry-first process first forms deep and narrow vertical pores through plasma directional etching, and then the wet etching expands the width of these pores, finally forming a "narrow mouth and gradually wide" conical or funnel-shaped structure. These two different morphology evolution paths lead to essential differences in the scattering characteristics of the final microstructure.

[0135] From the perspective of optical performance, the microstructure formed by the process of first wet etching and then dry etching has multi-level scattering characteristics. The shallow microstructure formed by the initial wet etching provides preliminary surface scattering ability, which is suitable for processing of large-angle incident light; while the deep structure increased by the subsequent dry etching enhances the scattering ability of small-angle incident light. This hierarchical scattering mechanism enables the final AG glass to maintain excellent anti-glare performance under different lighting conditions.

[0136] K. Wet etching 2

[0137] The wet etching 2 stage is an important step to realize the optimization of the final microstructure morphology and performance. This process aims to further adjust the formed microstructure to achieve the final required haze requirement.

[0138] Similar to wet etching 1, the etching solution used in wet etching 2 includes but is not limited to single acid or mixed acid such as HF, NH4HF2, etc., and inorganic or organic acid such as hydrochloric acid, nitric acid, sulfuric acid, acetic acid, etc. can be selectively added as auxiliary acidic component. During the etching process, the liquid concentration, temperature and etching rate need to be checked regularly in order to adjust the process parameters according to the real-time data. By keeping proper agitation of the liquid, the accumulation of reaction products can be avoided, further improving the etching uniformity and efficiency.

[0139] The present application proposes an innovative dry-wet etching combined process in the technical field of AG glass preparation, and the core technical features and protection points mainly lie in the following aspects:

[0140] Firstly, the fundamental innovation of the present application lies in the preparation method combining dry etching with wet etching. This composite process breaks through the limitations of traditional single etching process and initiates a new preparation approach for AG glass. Therefore, any method using dry etching technology in the preparation process of AG glass, regardless of its specific process parameters or equipment selection, falls within the protection scope of the present patent.

[0141] Secondly, the present application innovatively breaks through the fixed sequence limitation of dry etching and wet etching in traditional process, and clearly includes both the process of performing dry etching before wet etching and the process of performing dry etching after wet etching into the protection scope. This flexible process layout provides a wider technical path for precise control of microstructure morphology, and can select the optimal etching sequence according to the performance requirements of different application scenarios. Whether it is the traditional "dry first, wet later" process route or the innovative "wet first, dry later" process route, as long as it embodies the core idea of combining dry and wet etching, it falls within the protection scope of the present patent.

[0142] Thirdly, the present application particularly emphasizes the precise control scheme of microstructure aspect ratio. Specifically, it first forms an initial structure with a depth of 0.1-10 μm in the longitudinal direction through dry etching, and then realizes two-way three-dimensional etching in the longitudinal and transverse (5-100 μm) directions using wet etching. This technical scheme of enhancing anti-glare effect by increasing aspect ratio is an important protection content of the present application. All preparation methods using similar parameter ranges and process ideas fall within the protection scope of the present patent.

[0143] Fourthly, the present application extends the selection of film layer materials. In the dry-wet etching combined process, all technical schemes using ITO, Cr, Mo, SiO2 and Si3N4, etc. as film layers and combining with dry etching process fall within the protection scope of the present application. Whether it is the use of a single material mentioned above or the use of multiple materials to construct a film layer structure, as long as it is combined with dry etching process to prepare AG glass, it falls within the core protection scope of the present application.

[0144] The above four key technical features are interrelated and indispensable, and jointly constitute the complete technical solution of the present application. These features not only embody the innovativeness of the present application, but also provide a basis for subsequent technical development. By comprehensively protecting these key points, the technical advantages and patent value of the present application in the field of AG glass preparation are ensured.

[0145] The above only describes the preferred embodiments of the present application, and the above technical features can be arbitrarily combined to form multiple embodiment schemes of the present application.

[0146] The present application has been described above in conjunction with the drawings, and it is obvious that the specific implementation of the present application is not limited by the above manner. Any non-essential improvement using the concept and technical solution of the present application, or direct application of the concept and technical solution of the present application to other occasions without improvement, are all within the protection scope of the present application.

Claims

1. A method for producing an anti-glare glass, characterized by: It comprises the following steps: Step 1: surface cleaning treatment of the glass substrate; Step 2: coating a film layer on the surface of the glass substrate; Step 3: coating photoresist on the film layer; Step 4: exposure, development and film layer etching treatment; Step 5: through dry etching, etching the longitudinal depth of the glass, and then through wet etching, etching the longitudinal and transverse directions at the same time, to obtain a certain aspect ratio, increase the anti-glare area; or, first, through wet etching, to construct the surface of the glass, and then through dry etching, to realize precise depth control and feature shaping in a specific area; In the step 5, the process flow is: dry etching of glass→removal of photoresist→wet etching of glass 1→removal of film layer→wet etching of glass 2; In the step 2, the thickness of the film layer is 50-3000A, and the film layer is generated by vacuum coating or evaporation; in the step 3, the thickness of the photoresist is 0.5-20μm; the coating method is slot coating, the coating speed is controlled between 10-200mm / s, and the spraying pressure is controlled between 0.03-0.98 MPa; after coating, soft baking is performed, the soft baking temperature is controlled between 50-200℃, and the time is 30-300 seconds; In the step 4, in the exposure process, according to the batch and resolution requirements, a contact, near or projection exposure machine is selected; the exposure energy is between 50-500mJ / cm²; In the step 4, the development time is 30-90s, and the temperature is maintained at 20-30℃; the conductivity of the developer should be maintained within the range of 1-80 mS / cm; after development, post-baking is performed, the temperature range is 50-300℃, and the duration is 1-20 min; before film layer etching, the photoresist pattern needs to be cured, heat curing or UV curing is performed at a temperature range of 50-500℃ for 1-60 min, to enhance the etching resistance and mechanical strength of the photoresist pattern, and prevent deformation or delamination during etching; In the step 5, in the wet etching stage, the microstructure is etched in all directions by using chemical reagents, realizing the key transition from simple longitudinal depression to complex three-dimensional structure; the wet etching is performed in the transverse and longitudinal directions at the same time, to improve the etching width and depth, and enhance the anti-glare effect. In the step 1, first, deionized water is used for preliminary rinsing, and soft brush or ultrasonic means is used to remove dust and organic impurities on the surface of the substrate; or, cleaning agent or solvent is added for degreasing and oil removal treatment, the treatment temperature range is 20-100℃, and the treatment time is 1-10 min. ​ 2. The method of claim 1, wherein the anti-glare glass is prepared by: ​ 3. The method of claim 1, wherein the anti-glare glass is prepared by: The dry etching process in step 5 is: The dry etching step uses inductively coupled plasma technology to achieve precise microstructure processing of anti-glare glass; dry etching involves using plasma etching technology to directionally etch glass; In terms of process parameter settings, the vacuum system needs to be maintained at a vacuum state of 0.1-10 Torr to ensure the stability of the plasma and the complete dissociation of the gas; in terms of gas flow, the flow of the main etching gas is controlled within the range of 50-200 sccm, the flow of the inert gas is set at 50-150 sccm, and if O2 is added, it is controlled at 5-20 sccm.

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