An electronic screen tempered glass film with anti-glare function and a preparation method thereof
By integrally molding a nanoscale concave-convex anti-glare structure on the surface of a glass substrate, the problems of coating peeling and chemical etching damage in anti-glare tempered glass films have been solved, achieving a balance between anti-glare effect and mechanical properties, simplifying the production process and improving product stability.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHENZHEN RUIGUAN PHOTOELECTRIC GLASS CO LTD
- Filing Date
- 2026-03-30
- Publication Date
- 2026-05-29
AI Technical Summary
Existing anti-glare tempered glass films suffer from problems such as coating peeling, yellowing, and chemical etching damage when trying to balance anti-glare effects with the mechanical protection performance of the glass substrate. In addition, the production process is cumbersome and the environmental control costs are high.
A matrix formulation employing phase-separation induced composite components and phase-separation regulated fluxing composite components, combined with a gradient quenching process that synchronizes tempering and phase separation, is used to integrally form a nanoscale concave-convex anti-glare structure on the surface of a glass substrate. Through staged batch feeding, atmosphere control, and electric field-assisted treatment, the anti-glare structure and the glass substrate are prepared simultaneously.
It achieves compatibility between anti-glare function and glass substrate performance, simplifies the production process, improves mechanical properties and mass production stability, avoids interface peeling and structural damage, and adapts to high-definition display requirements.
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Figure CN122102514A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of glass manufacturing technology, and more specifically, to a tempered glass film for electronic screens with anti-glare function and a method for preparing the same. Background Technology
[0002] Tempered glass screen protectors are widely used protective components for screens in consumer electronics, automotive displays, and industrial control terminals. Their core function is to provide impact and scratch resistance for various flat panel display screens. Tempered glass screen protectors with anti-glare functions can also reduce specular reflections and glare interference from ambient light by regulating the reflection of light on the glass surface, effectively improving screen visibility and visual comfort in strong light environments. With the rapid popularization of high-resolution display technology and the continuous improvement in screen protection requirements for various terminal products, the industry has placed higher demands on the comprehensive performance of anti-glare tempered glass screen protectors. Products must simultaneously meet the needs of high-definition displays, possess stable mechanical protection capabilities, and offer excellent anti-glare effects.
[0003] Currently, most mainstream anti-glare tempered glass screen protectors in the industry are prepared by chemical etching with hydrofluoric acid or by applying organic functional coatings. Chemical etching can easily damage the surface stress layer of tempered glass to varying degrees, leading to a certain degree of reduction in the glass's impact resistance. Coating, on the other hand, has stability issues such as coating peeling and yellowing after long-term use. Neither of these conventional preparation methods can achieve a stable anti-glare effect while also taking into account the mechanical protection properties of the glass substrate and the optical display compatibility with high-resolution screens. This is a core technical problem that the industry urgently needs to solve. At the same time, existing processes also have industry pain points such as long production processes and high environmental control costs. Summary of the Invention
[0004] To address the problem that existing anti-glare tempered glass films cannot simultaneously achieve both anti-glare performance and overall glass substrate properties, this application provides an electronic screen tempered glass film with anti-glare function and its preparation method.
[0005] In a first aspect, this application provides a tempered glass film for electronic screens with anti-glare function, employing the following technical solution: An anti-glare tempered glass film for electronic screens, the tempered glass film comprising a tempered glass substrate, the tempered glass substrate being prepared from the following raw materials in parts by weight: 65-72 parts silicon dioxide, 12-16 parts sodium oxide, 6-9 parts calcium oxide, 1.5-3.5 parts aluminum oxide, 3.5-7 parts phase separation inducing composite component, 0.4-1.0 parts phase separation regulating fluxing composite component, 0.2-0.5 parts composite clarifying agent, and 0.3-0.8 parts lithium carbonate; The tempered glass substrate has a nanoscale concave-convex anti-glare structure integrally formed on one side surface. The nanoscale concave-convex anti-glare structure is formed by metastable phase separation of the glass substrate, with the phase separation region size being 100-300nm and the structure depth being 0.5-1μm.
[0006] By adopting the above technical solution, phase separation induction composite components and phase separation regulation fluxing composite components are introduced into the sodium-calcium-silicon glass base system. This provides a nucleation basis and controllable conditions for controllable metastable phase separation in the glass during subsequent heat treatment. The glass matrix can form a two-phase homogeneous structure with different chemical properties, namely a silicon-rich phase and an alkali-boron-rich phase, through metastable phase separation. After subsequent selective acid etching, a nanoscale concave-convex anti-glare structure is integrally formed on the surface of the glass matrix. There is no need for additional surface etching or coating on the finished glass product. This allows the anti-glare structure to form a complete and continuous phase with the glass matrix, without a two-phase interface. Structurally, this avoids the problems of anti-glare structure detachment and interface failure, while also preventing damage to the internal structure of the glass matrix during subsequent processing.
[0007] Preferably, the phase-separation regulating fluxing composite component is composed of strontium oxide, sodium fluorosilicate, and phosphorus pentoxide in a mass ratio of (2.8-3.2):(1.8-2.2):(0.8-1.2). The phase separation-induced composite component is composed of boron oxide, magnesium fluoride, and zirconium oxide in a mass ratio of (3.8-4.2):(1.8-2.2):(0.8-1.2). The mass ratio of the phase separation-controlled fluxing composite component to the phase separation-induced composite component is (0.8-1.2):6.
[0008] By employing the above technical solutions, boron oxide, as a glass network forger, can break the continuity of the silicon-oxygen network, regulate the degree of polymerization of the glass network, and lower the critical temperature for phase separation, providing a structural basis for metastable phase separation. Magnesium fluoride can reduce the activation energy for glass phase separation, promote uniform nucleation during the phase separation process, and avoid localized phase separation anomalies. Zirconia can regulate the growth rate of the phase separation region, limit the maximum size of the phase separation region, and prevent excessive growth of the phase separation region leading to deterioration of optical performance. The three components, when combined in a specific ratio, can achieve precise control of phase separation nucleation and growth. Strontium oxide can regulate the viscosity and surface tension of the glass melt, optimizing the dispersion of the phase separation components in the melt. Sodium fluorosilicate can help reduce the activation energy for phase separation and accelerate the phase separation kinetics. Phosphorus pentoxide can serve as a nucleation site for phase separation, optimizing the uniformity of the size distribution of the phase separation region. When these three components are combined with the phase separation-inducing composite component in a specific ratio, the glass phase separation temperature range can be well matched with the subsequent heat treatment process window, ensuring that the phase separation process is completed uniformly and controllably in a short time.
[0009] Preferably, the composite clarifying agent is composed of cerium oxide and sodium chloride in a mass ratio of (0.9-1.1):1.
[0010] By adopting the above technical solution, cerium oxide can release oxygen through a variable valence reaction in the high-temperature molten state, promoting the aggregation, growth, and floating out of the microbubbles in the glass melt. At low temperatures, it can absorb oxygen and will not form new bubble defects during the glass cooling process. Sodium chloride can reduce the high-temperature viscosity and surface tension of the glass melt, and help improve the fluidity and clarification and homogenization effect of the melt. When the two are compounded in a specific ratio, they can efficiently eliminate bubbles, streaks, and stone defects in the melt during the glass melting process, improve the optical uniformity of the glass matrix, and provide a homogeneous and defect-free glass foundation for subsequent uniform phase separation.
[0011] Preferably, the thickness of the tempered glass substrate is 0.2-0.4 mm, and a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure, the thickness of the monolayer silicon dioxide passivation film being 1-5 nm.
[0012] By adopting the above technical solution, a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure. This film can seal the micro-defects and micropores formed on the glass surface by phase separation acid etching, block the contact path between the external corrosive medium and the glass substrate, and improve the chemical stability and scratch resistance of the glass surface. The substrate thickness of 0.2-0.4mm is suitable for the assembly requirements of mainstream electronic screens such as mobile phones, tablets, and automotive screens. At the same time, it ensures that the glass substrate has sufficient mechanical strength and processing performance, and is suitable for subsequent cutting, bonding, coating and other processing steps, avoiding the risk of glass breakage caused by thin processing.
[0013] Secondly, this application provides a method for preparing a tempered glass film for electronic screens with anti-glare function, using the following technical solution: A method for preparing a tempered glass film for electronic screens with anti-glare function includes the following steps: S1. Batching and Melting: Weigh each raw material for preparing the tempered glass substrate, and use a staged batch feeding method to complete high-temperature melting, clarification and homogenization. Then, use the overflow pull-down method to form the glass sheet. S2. Preheating and Homogenization and Atmosphere Control: After cleaning and drying, the glass sheet is sent to the preheating section of the tempering furnace to complete the preheating and homogenization treatment under a protective atmosphere. S3, Tempering-Phase Separation Synchronous Gradient Quenching and Electric Field Assisted Coupling: The preheated glass sheet is sent into the tempering furnace quenching section. A two-stage gradient air cooling quenching process including hot air quenching and cold air quenching is adopted. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied to the glass sheet for auxiliary treatment, so as to achieve controllable metastable phase separation on the glass surface while completing physical tempering. S4. Integrated rinsing-passivation treatment: The tempered glass sheet is first rinsed with a weak acid solution of citric acid, and then soaked in a sodium silicate solution for in-situ passivation treatment, forming a nano-level concave-convex anti-glare structure on the glass surface and completing the size locking. S5. Drying and post-processing cutting: Rinse and dry the processed glass sheet, and complete the functional layer coating and size cutting according to the requirements to obtain the finished tempered glass film.
[0014] By adopting the above technical solution, the phased and batch feeding melting process, combined with subsequent atmosphere control, tempering-phase separation synchronous treatment, and rinsing-passivation integrated process, can form a complete continuous process flow for the preparation of the glass substrate, the construction of the phase separation structure, and the completion of physical tempering. The two independent heat treatment processes of glass phase separation and physical tempering are coupled and completed in the same quenching process. There is no need to add an additional anti-glare structure preparation process after tempering, which simplifies the production process. At the same time, the construction process of the anti-glare structure is precisely matched with the tempering process of the glass substrate, avoiding the damage to the tempering stress layer caused by the anti-glare treatment in the existing step-by-step process, and achieving a balance between anti-glare function and tempering mechanical properties.
[0015] Preferably, in step S1, the specific process of high-temperature melting with staged and batch feeding is as follows: In the first stage, silicon dioxide, sodium oxide, calcium oxide, aluminum oxide and lithium carbonate are weighed according to the weight parts, and mixed evenly to obtain the basic batch material. The basic batch material is melted at 1450-1500℃ for 2-3 hours, and the mixture is continuously stirred during the melting process to form a glass base melt. In the second stage, while maintaining a melting temperature of 1450-1500℃, a composite clarifying agent is added to the glass base melt, and stirring is continued for 30-60 minutes to complete the clarification and homogenization. In the third stage, the glass melt is cooled to 1250-1300℃, and phase separation induction composite components and phase separation regulation fluxing composite components are added to the melt. After stirring continuously for 40-80 minutes, the temperature is lowered to 1200-1250℃, and the glass sheet with a thickness of 0.2-0.4mm is formed by overflow pull-down method. After cutting, it is naturally cooled to room temperature.
[0016] By adopting the above technical solution, the feeding and temperature settings in the three stages correspond to the optimal operating temperature windows of each component. The high-temperature melting in the first stage allows high-melting-point skeleton materials such as silica to fully melt, forming a continuous and uniform silica glass network. Lithium carbonate, as a flux, can effectively reduce the melting temperature of the skeleton material and shorten the melting cycle. The isothermal range in the second stage is the state where the glass melt viscosity is the lowest. At this time, the addition of composite clarifying agent can maximize the clarifying effect and achieve the homogenization of the melt. The cooling range in the third stage can ensure that the phase-separated functional components are uniformly dispersed in the melt and avoid excessive loss of volatile components such as boron and fluorine at high temperatures. At the same time, during the stirring and cooling process of the melt, the phase-separated components can spontaneously migrate to the surface of the glass melt, forming a concentration gradient enriched on the surface, laying the foundation for surface-oriented phase separation in the subsequent heat treatment process.
[0017] Preferably, in step S2, the protective atmosphere is nitrogen, the purity of the nitrogen is ≥99.99%, the oxygen content in the furnace is controlled to be ≤50ppm, the furnace is maintained at a slight positive pressure of 50-100Pa, and the atmosphere control continues until the end of the hot air quenching stage in step S3; the preheating temperature is 620-650℃, and the preheating time is 80-120s.
[0018] By adopting the above technical solutions, high-purity nitrogen is introduced throughout the preheating and hot air quenching stages, and the oxygen content in the furnace is controlled. This prevents surface oxidation of the glass at high temperatures and inhibits the volatilization of boron and fluorine components related to phase separation at high temperatures, ensuring stable concentrations of phase-separation-related components on the glass surface. This ensures consistent phase separation behavior across different batches of glass and improves performance stability during mass production. The slightly positive pressure environment inside the furnace prevents outside air from entering, further reducing the impact of oxygen content on the glass surface. The continuous nitrogen flow can promptly remove trace volatilized components, preventing them from depositing and contaminating the glass surface. The preheating process eliminates internal stress generated during the cooling and cutting of the glass sheet, ensuring a uniform overall glass temperature close to the glass transition temperature. This provides a uniform temperature base for tempering and phase separation during subsequent quenching, avoiding inconsistencies in phase separation and uneven distribution of tempering stress caused by localized temperature unevenness.
[0019] Preferably, in step S3, the two-stage gradient air cooling quenching process is as follows: first, the first stage of hot air quenching and electric field assisted treatment is performed, and then the second stage of cold air quenching and tempering is performed. The parameters for the first stage of hot air quenching and electric field assisted treatment are as follows: hot air quenching with a wind pressure of 0.3-0.5MPa and a wind temperature of 180-220℃ is used for 15-25s. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied. The electric field parameters are AC voltage of 500-800V and frequency of 15-25Hz. After treatment, the glass surface temperature drops to 580-600℃. The parameters for the second stage of cold air quenching and tempering are as follows: stop applying the electric field, switch to cold air quenching with a wind pressure of 0.8-1.2MPa and a wind temperature of 20-30℃, and continue for 30-40 seconds to form a compressive stress layer on the glass surface.
[0020] By adopting the above technical solution, 580-600℃ is the metastable phase separation critical temperature range of this glass system. Within this temperature range, the glass system has the kinetic conditions for phase separation, but has not reached the softening point of the glass, so it will not affect the stress formation in the subsequent tempering process. First, the glass temperature is stabilized in this phase separation temperature range by hot air quenching, providing a suitable temperature and time window for the phase separation process on the glass surface. The low-frequency alternating electric field applied simultaneously can, on the one hand, drive the alkali metal ions and boron ions in the glass to migrate directionally to the glass surface, promoting the phase separation process to be concentrated in the 0.5-1μm depth range on the glass surface. On the other hand, it can reduce the phase separation activation energy and accelerate the phase separation rate, so that the phase separation process can be completed in a short time of 15-25s, which is suitable for the time window of the tempering process. Then, the glass temperature is rapidly reduced to room temperature by cold air quenching. On the one hand, a uniform permanent compressive stress layer is formed on the glass surface through rapid temperature change, completing physical tempering. On the other hand, the phase separation structure on the glass surface is quickly locked, preventing the phase separation region from continuing to grow during the cooling process and causing structural runaway. Finally, the tempering and phase separation are completed simultaneously.
[0021] Preferably, in step S4, the citric acid aqueous solution has a mass fraction of 0.5-1.0% and a rinsing time of 10-15s, the sodium silicate aqueous solution has a mass fraction of 0.2-0.5% and a soaking time of 8-12s; after soaking, the glass slide is rinsed with deionized water until the pH of the rinsing solution is neutral.
[0022] By adopting the above technical solution, the solubility of the alkali-rich boron phase formed by phase separation on the glass surface is much higher than that of the silicon-rich phase in a weak acid environment. Therefore, the citric acid aqueous solution can selectively dissolve the alkali-rich boron phase, accurately forming a nanoscale concave-convex structure corresponding to the size of the phase separation region. The weak acidity of citric acid can avoid excessive corrosion of the silicon-rich phase of the glass, ensuring the dimensional accuracy and uniformity of the concave-convex structure. After rinsing, passivation treatment is carried out directly without intermediate water washing, which can avoid the acid residue on the glass surface after rinsing from continuing to cause uneven corrosion before water washing, ensuring the batch consistency of the anti-glare structure size. Sodium silicate can be hydrolyzed in the weak acid environment of the glass surface, generating silicon dioxide in situ and forming a chemical bond with the silicon-oxygen network of the glass matrix, forming a continuous passivation film on the surface of the concave-convex structure. This can not only quickly terminate the acid etching reaction and lock the size and morphology of the anti-glare structure, but also seal surface micro-defects and improve the chemical stability of the glass surface.
[0023] Preferably, in step S5, the hot air temperature for drying is 100-120℃, and the drying time is 15-20 minutes, to obtain an anti-glare tempered glass substrate; after the glass substrate is treated with a functional layer, it is cut and trimmed according to a preset size to obtain a finished electronic screen tempered glass film with anti-glare function.
[0024] By adopting the above technical solution, a drying temperature of 100-120℃ can completely remove residual moisture from the glass surface and micropores of the uneven structure without changing the internal stress distribution of the glass. This avoids defects such as bubbles and pinholes in the subsequent functional layer coating caused by residual moisture. After drying, the functional layer coating and size cutting can be carried out according to the usage requirements, so that the product can be adapted to the assembly and usage requirements of different types of electronic screens. Laser cutting and trimming can avoid defects such as edge chipping and micro-cracks caused by mechanical cutting, ensuring the edge strength and appearance yield of the product, and improving the applicability and processing adaptability of the product.
[0025] In summary, this application has the following beneficial effects: 1. This application adopts a matrix formulation containing phase separation inducing composite components and phase separation regulating fluxing composite components, combined with a tempering-phase separation synchronous gradient quenching process. Through the synergistic effect of the formulation and process, a nanoscale anti-glare structure can be integrally formed on the surface of the glass matrix without the need for additional surface etching or coating treatment. This helps to avoid structural damage to the glass matrix caused by anti-glare treatment and achieves compatibility between anti-glare function and basic glass performance.
[0026] 2. The preparation method of this application uses a two-stage gradient air-cooling quenching process to couple the physical tempering of glass with the controllable metastable phase separation of the surface in the same process. This breaks the fixed process route of the existing technology that involves step-by-step processing, which can effectively shorten the production process and reduce the adverse effects of step-by-step processes on the tempered stress layer, thus better ensuring the mechanical properties of the glass.
[0027] 3. In this application, the preferred process design is to apply a low-frequency alternating electric field simultaneously with hot air quenching. This can drive the directional migration of functional ions in the glass through the electric field, which helps to limit the phase separation process within a set depth range on the glass surface, reduce the adverse effects of phase separation on optical performance, and achieve anti-glare effect while better taking into account the screen display performance.
[0028] 4. The preparation method of this application, through a high-temperature melting process of phased and batch feeding, allows different functional components to be added to the glass system at an appropriate temperature window, which helps to ensure the uniform formation of the basic glass network, while reducing the high-temperature volatilization loss of phase-separated functional components, and providing a homogeneous and stable glass matrix for controllable phase separation in the subsequent tempering process.
[0029] 5. In this application, the preferred treatment process is an integrated process of citric acid weak acid rinsing and sodium silicate in-situ passivation. After rinsing, there is no need for intermediate water washing before passivation. This process can precisely control the acid etching process and lock the anti-glare structure size. At the same time, it can seal micro-defects on the surface, which helps to improve the chemical stability of the glass surface and optimize the long-term reliability of the product in complex environments. Attached Figure Description
[0030] Figure 1 This is a flowchart of the manufacturing process of an electronic screen tempered glass film with anti-glare function provided in this application. Detailed Implementation
[0031] The present application will be further described in detail below with reference to embodiments and comparative examples. Unless otherwise specified, the experimental methods used below are conventional methods. Unless otherwise specified, the materials, reagents, methods and instruments used are all conventional materials, reagents, methods and instruments in the art, which can be obtained by those skilled in the art through commercial channels or prepared according to literature methods.
[0032] Technical Concept: In related technologies, the anti-glare structure of tempered glass anti-glare films for electronic screens is mostly prepared through surface coating or chemical etching processes, and tempering and anti-glare treatment are often carried out in separate steps. This approach has significant drawbacks. The core reason is that there is an interface gap between the coating and the glass substrate, which is prone to peeling and wear. Chemical etching can damage the stress layer on the glass surface, leading to a decrease in mechanical properties. In the step-by-step process, subsequent anti-glare processing can disturb the stress distribution of tempering, making it difficult to achieve a synergistic balance between anti-glare effect and tempering mechanical properties. At the same time, the process is cumbersome and affects the stability of mass production.
[0033] To address the aforementioned issues, this technical solution achieves a breakthrough through synergistic optimization of formulation and process: the formulation introduces a composite component for phase separation induction and phase separation regulation, providing nucleation and regulation conditions for metastable phase separation in the glass matrix; the preparation process employs staged batch feeding and melting to ensure uniform dispersion of raw materials, followed by preheating and homogenization in a protective atmosphere to eliminate internal stress, and then simultaneous tempering and controllable metastable phase separation on the surface through a two-stage gradient air-cooling quenching coupled with an electric field; finally, the anti-glare structure is locked in through integrated rinsing and passivation treatment, making the anti-glare structure integrally formed with the glass matrix, fundamentally solving the problems of interface detachment and damage to mechanical properties, while simplifying the process and improving the overall performance and mass production reliability of the product.
[0034] Example 1: This example provides an electronic screen tempered glass film with anti-glare function. The tempered glass film uses tempered glass substrate as the core functional carrier and contains the following raw materials in parts by weight: 68.5 parts of silicon dioxide, 14 parts of sodium oxide, 7.5 parts of calcium oxide, 2.5 parts of aluminum oxide, 5.25 parts of phase separation inducing composite component, 0.875 parts of phase separation regulating fluxing composite component, 0.35 parts of composite clarifying agent, and 0.55 parts of lithium carbonate. The phase-separation regulating flux composite component is composed of strontium oxide, sodium fluorosilicate, and phosphorus pentoxide in a mass ratio of 3:2:1; the phase-separation inducing composite component is composed of boron oxide, magnesium fluoride, and zirconium oxide in a mass ratio of 4:2:1; the mass ratio of the phase-separation regulating flux composite component to the phase-separation inducing composite component is 1:6; the composite clarifying agent is composed of cerium oxide and sodium chloride in a mass ratio of 1:1; the thickness of the tempered glass substrate is 0.3 mm, and a nanoscale concave-convex anti-glare structure is integrally formed on one side of the tempered glass substrate. This nanoscale concave-convex anti-glare structure is formed by metastable phase separation of the glass substrate, with a phase separation region size of 200 nm and a structural depth of 0.75 μm; a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure, with a thickness of 3 nm, which can seal surface micro-defects and improve the chemical stability of the glass.
[0035] The preparation method of the above-mentioned tempered glass film for electronic screens with anti-glare function includes the following steps: S1. Batching and Melting: Weigh the raw materials for preparing the tempered glass substrate according to the weight proportions, and complete the high-temperature melting and clarification and homogenization by feeding in stages and batches. Then, use the overflow and downward pulling method to form the glass sheet. The specific process of high-temperature melting with phased and batch feeding is as follows: In the first stage, silicon dioxide, sodium oxide, calcium oxide, aluminum oxide, and lithium carbonate were weighed according to their weight proportions and added to a horizontal high-speed mixer. The mixture was stirred at 400 r / min for 17.5 min. After mixing, the mixture was passed through a 200-mesh standard sieve to remove agglomerated particles, resulting in a uniform basic batch. The basic batch was placed in a 5L high-purity platinum crucible and then placed in a silicon molybdenum rod high-temperature box furnace. The furnace was melted at 1475℃ for 2.5 h. During the melting process, a high-purity quartz stirring rod was used to continuously and uniformly stir the melt at 100 r / min to eliminate local component inhomogeneity and form a homogeneous and transparent glass base melt. In the second stage, while maintaining a melting temperature of 1475℃ and continuous stirring, a composite clarifying agent is added to the glass base melt at a uniform rate. After the addition is completed, stirring is continued for 45 minutes to complete the clarification and homogenization. The high-temperature oxidation-reduction reaction of cerium oxide eliminates bubbles, streaks and stone defects in the glass melt. In the third stage, the furnace temperature is uniformly reduced to 1275℃, and the phase separation induction composite component and the phase separation regulation flux composite component are uniformly added to the melt. The mixture is stirred continuously for 60 minutes to ensure that the two components are uniformly dispersed in the glass melt network and to form a concentration gradient enriched on the surface. After stirring, the melt temperature is uniformly reduced to 1225℃, and the mixture is formed by an overflow pull-down device with a pull-down rate controlled at 8m / min to form a continuous glass ribbon with a thickness of 0.3mm. The ribbon is then cut into glass sheets of a preset size of 100mm×150mm by a diamond wheel and allowed to cool naturally to room temperature in a dust-free environment.
[0036] S2. Preheating and Homogenization and Atmosphere Control: After cleaning and drying, the glass sheet is sent to the preheating section of the tempering furnace to complete the preheating and homogenization treatment under a protective atmosphere. The process involves first placing the cooled glass sheet into a multi-tank ultrasonic cleaner, where it is ultrasonically cleaned sequentially with neutral glass cleaner and deionized water at a frequency of 40kHz and a cleaning time of 3 minutes per tank. After cleaning, the glass sheet is dried with clean hot air at 60℃ for 10 minutes to remove surface moisture and impurities. The dried glass sheet is then placed in the preheating section of a continuous horizontal tempering furnace. High-purity nitrogen is introduced throughout the preheating section to establish a protective atmosphere, with nitrogen purity controlled at ≥99.99% and oxygen content in the furnace ≤50ppm. A slight positive pressure of 75Pa is maintained inside the furnace to prevent oxidation of the glass surface and volatilization of phase-separated components at high temperatures. Atmosphere control continues until the end of the hot air quenching stage in step S3. The preheating section has three gradient temperature zones, with the final constant temperature zone stabilizing at 635℃. The total residence time of the glass sheet in the preheating section is 100s, ensuring that the overall glass temperature reaches a uniform range of ±10℃ from the glass transition temperature, eliminating internal stress in the glass, and providing a uniform temperature basis for subsequent tempering and phase separation treatment.
[0037] S3, Tempering-Phase Separation Synchronous Gradient Quenching and Electric Field Assisted Coupling: The preheated glass sheet is sent into the tempering furnace quenching section. A two-stage gradient air cooling quenching process including hot air quenching and cold air quenching is adopted. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied to the glass sheet for auxiliary treatment, so as to achieve controllable metastable phase separation on the glass surface while completing physical tempering. The two-stage gradient air cooling quenching process is as follows: first, the first stage of hot air quenching and electric field assisted treatment is performed, and then the second stage of cold air quenching and tempering is performed. The two stages are completed continuously in the same quenching section without intermediate stops. The parameters for the first stage of hot air quenching and electric field-assisted treatment are as follows: hot air is output using nozzles arranged symmetrically at the top and bottom, with a wind pressure of 0.4 MPa, a wind temperature of 200℃, a distance of 15 mm between the nozzles and the glass surface, and hot air quenching lasts for 20 seconds; during the quenching process, a low-frequency alternating electric field perpendicular to the glass surface is simultaneously applied to the original glass sheet through parallel flat electrodes set at the top and bottom of the quenching section. The electric field parameters are AC voltage of 650V and frequency of 20Hz, and the duration of electric field application is exactly the same as the duration of hot air quenching; the glass surface temperature is precisely reduced to the range of 580-600℃ by hot air temperature control, and with the electric field driving the directional migration of alkali metal ions, controllable metastable phase separation is completed within a depth of 0.5-1μm on the glass surface, forming a uniform silicon-rich phase and an alkali-boron-rich phase; The parameters for the second stage of cold air quenching tempering and shaping are as follows: After the hot air quenching and electric field application are completed, the electric field output is immediately stopped, and the air path is simultaneously switched to room temperature clean compressed air. Cold air with a wind pressure of 1.0 MPa and a wind temperature of 25°C is used for rapid quenching. The distance between the air nozzle and the glass surface is kept at 15 mm. The cold air quenching lasts for 35 seconds, so that the overall temperature of the glass drops sharply to below 200°C within 10 seconds, and finally cools to room temperature. A uniform compressive stress layer of 700 MPa is formed on the glass surface through rapid temperature change, which completes the physical tempering. At the same time, the phase separation structure on the glass surface is quickly locked to prevent the excessive growth of the phase separation region from damaging the optical performance.
[0038] S4. Integrated rinsing-passivation treatment: The tempered glass sheet is first rinsed with a weak acid solution of citric acid, and then soaked in a sodium silicate solution for in-situ passivation treatment, forming a nano-level concave-convex anti-glare structure on the glass surface and completing the size locking. The tempered glass sheet is fed into a continuous roller washing tank. First, a 0.75% (w / w) food-grade citric acid aqueous solution is used at a constant temperature of 27.5℃ to immerse and rinse one side of the glass after the phase separation treatment in step S3 for 12.5 seconds. This selectively removes the alkali-rich boron phase formed on the glass surface, creating a uniform nanoscale anti-glare structure. After rinsing, no further water washing is required. The glass sheet is immediately placed into a constant-temperature passivation tank at 42.5℃ and immersed in a 0.35% (w / w) sodium silicate aqueous solution for 10 seconds. This forms a monolayer silica passivation film in situ on the nanoscale surface, precisely terminating the acid etching reaction and locking in the size and morphology of the anti-glare structure. After immersion, the glass sheet is rinsed with 0.3MPa high-pressure deionized water on both sides until the pH of the rinsing solution is neutral, thoroughly removing any residual reaction solution from the surface.
[0039] S5. Drying and post-processing cutting: Rinse and dry the processed glass sheet, and complete the functional layer coating and size cutting according to the requirements to obtain the finished tempered glass film. The process involves first rinsing the original glass sheet and then placing it in a Class 100 cleanroom hot air circulating oven. The sheet is dried at a constant temperature of 110℃ for 17.5 minutes to thoroughly remove surface moisture, resulting in a clean, anti-glare tempered glass substrate. On the non-anti-glare side of the glass substrate, a slit coating process is used to apply a 25μm thick acrylic optical pressure-sensitive adhesive. After coating, the adhesive is cured at 50℃ for 5 minutes, and then a 75μm thick PET release film is laminated. A UV nanosecond laser cutting machine is used to cut the film to the preset dimensions of the mobile phone screen, with the laser power set to 12W and the cutting speed at 200mm / s. After cutting, a full inspection of the appearance and optical performance is performed, and defective products are removed to obtain the finished anti-glare tempered glass film for electronic screens.
[0040] Example 2: This example provides an electronic screen tempered glass film with anti-glare function. The tempered glass film uses tempered glass substrate as the core functional carrier and contains the following raw materials in parts by weight: 65 parts of silicon dioxide, 12 parts of sodium oxide, 6 parts of calcium oxide, 1.5 parts of aluminum oxide, 3.5 parts of phase separation inducing composite component, 0.47 parts of phase separation regulating fluxing composite component, 0.2 parts of composite clarifying agent, and 0.3 parts of lithium carbonate. The phase-separation regulating flux composite component is composed of strontium oxide, sodium fluorosilicate, and phosphorus pentoxide in a mass ratio of 2.8:1.8:0.8; the phase-separation inducing composite component is composed of boron oxide, magnesium fluoride, and zirconium oxide in a mass ratio of 3.8:1.8:0.8; the mass ratio of the phase-separation regulating flux composite component to the phase-separation inducing composite component is 0.8:6; the composite clarifying agent is composed of cerium oxide and sodium chloride in a mass ratio of 0.9:1; the thickness of the tempered glass substrate is 0.2 mm, and a nanoscale concave-convex anti-glare structure is integrally formed on one side of the tempered glass substrate. This nanoscale concave-convex anti-glare structure is formed by metastable phase separation of the glass substrate, with a phase separation region size of 100 nm and a structural depth of 0.5 μm; a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure, with a thickness of 1 nm, which can seal surface micro-defects and improve the chemical stability of the glass.
[0041] The preparation method of the above-mentioned tempered glass film for electronic screens with anti-glare function includes the following steps: S1. Batching and Melting: Weigh the raw materials for preparing the tempered glass substrate according to the weight proportions, and complete the high-temperature melting and clarification and homogenization by feeding in stages and batches. Then, use the overflow and downward pulling method to form the glass sheet. The specific process of high-temperature melting with phased and batch feeding is as follows: In the first stage, silicon dioxide, sodium oxide, calcium oxide, aluminum oxide, and lithium carbonate were weighed according to their weight proportions and added to a horizontal high-speed mixer. The mixture was stirred at 300 r / min for 15 min. After mixing, the mixture was passed through a 200-mesh standard sieve to remove agglomerated particles, resulting in a uniform basic batch. The basic batch was placed in a 5L high-purity platinum crucible and then placed in a silicon molybdenum rod high-temperature box furnace. The furnace was melted at 1450℃ for 2 h. During the melting process, a high-purity quartz stirring rod was used to continuously and uniformly stir the melt at 100 r / min to eliminate local component inhomogeneity and form a homogeneous and transparent glass base melt. In the second stage, while maintaining a melting temperature of 1450℃ and continuous stirring, a composite clarifying agent is added to the glass base melt at a uniform rate. After the addition is completed, stirring is continued for 30 minutes to complete the clarification and homogenization. The high-temperature oxidation-reduction reaction of cerium oxide eliminates bubbles, streaks and stone defects in the glass melt. In the third stage, the furnace temperature is uniformly reduced to 1250℃, and the phase separation induction composite component and the phase separation regulation flux composite component are uniformly added to the melt. The mixture is stirred continuously for 40 minutes to ensure that the two components are uniformly dispersed in the glass melt network and to form a concentration gradient enriched on the surface. After stirring, the melt temperature is uniformly reduced to 1200℃, and the mixture is formed by an overflow pull-down device with a pull-down rate controlled at 10m / min to form a continuous glass ribbon with a thickness of 0.2mm. The ribbon is then cut into glass sheets of a preset size of 100mm×150mm by a diamond wheel and allowed to cool naturally to room temperature in a dust-free environment.
[0042] S2. Preheating and Homogenization and Atmosphere Control: After cleaning and drying, the glass sheet is sent to the preheating section of the tempering furnace to complete the preheating and homogenization treatment under a protective atmosphere. The process involves first placing the cooled glass sheet into a multi-tank ultrasonic cleaner, where it is ultrasonically cleaned sequentially with neutral glass cleaner and deionized water at a frequency of 40kHz. Each tank is cleaned for 2 minutes. After cleaning, the glass sheet is dried with clean hot air at 55℃ for 8 minutes to remove surface moisture and impurities. The dried glass sheet is then placed in the preheating section of a continuous horizontal tempering furnace. High-purity nitrogen is continuously introduced into the preheating section to create a protective atmosphere, with nitrogen purity controlled at ≥99.99%, oxygen content ≤50ppm, and a slight positive pressure of 50Pa maintained inside the furnace to prevent oxidation of the glass surface and volatilization of phase-separated components at high temperatures. This atmosphere control continues until the end of the hot air quenching stage in step S3. The preheating section has three temperature gradient zones, with the final constant temperature zone stabilizing at 620℃. The total residence time of the glass sheet in the preheating section is 80 seconds, ensuring a uniform overall glass temperature within the glass transition temperature range of ±10℃. This eliminates internal stress in the glass and provides a uniform temperature basis for subsequent tempering and phase separation processes.
[0043] S3, Tempering-Phase Separation Synchronous Gradient Quenching and Electric Field Assisted Coupling: The preheated glass sheet is sent into the tempering furnace quenching section. A two-stage gradient air cooling quenching process including hot air quenching and cold air quenching is adopted. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied to the glass sheet for auxiliary treatment, so as to achieve controllable metastable phase separation on the glass surface while completing physical tempering. The two-stage gradient air cooling quenching process is as follows: first, the first stage of hot air quenching and electric field assisted treatment is performed, and then the second stage of cold air quenching and tempering is performed. The two stages are completed continuously in the same quenching section without intermediate stops. The parameters for the first stage of hot air quenching and electric field-assisted treatment are as follows: hot air is output using nozzles arranged symmetrically at the top and bottom, with a wind pressure of 0.3 MPa, a wind temperature of 180℃, a distance of 15 mm between the nozzles and the glass surface, and hot air quenching lasts for 15 seconds; during the quenching process, a low-frequency alternating electric field perpendicular to the glass surface is simultaneously applied to the glass sheet through parallel plate electrodes set at the top and bottom of the quenching section. The electric field parameters are AC voltage of 500V and frequency of 15Hz, and the duration of electric field application is exactly the same as the duration of hot air quenching; the glass surface temperature is precisely reduced to 580℃ by hot air temperature control, and with the electric field driving the directional migration of alkali metal ions, controllable metastable phase separation is completed within a depth of 0.5 μm on the glass surface, forming a uniform silicon-rich phase and an alkali-boron-rich phase; The parameters for the second stage of cold air quenching tempering and shaping are as follows: After the hot air quenching and electric field application are completed, the electric field output is immediately stopped, and the air path is simultaneously switched to room temperature clean compressed air. Cold air with a pressure of 0.8MPa and a temperature of 20℃ is used for rapid quenching. The distance between the air nozzle and the glass surface is kept at 15mm. The cold air quenching lasts for 30s, so that the overall temperature of the glass drops sharply to below 200℃ within 10s, and finally cools to room temperature. A uniform compressive stress layer of 600MPa is formed on the glass surface through rapid temperature change, which completes the physical tempering. At the same time, the phase separation structure on the glass surface is quickly locked to prevent the excessive growth of the phase separation region from damaging the optical performance.
[0044] S4. Integrated rinsing-passivation treatment: The tempered glass sheet is first rinsed with a weak acid solution of citric acid, and then soaked in a sodium silicate solution for in-situ passivation treatment, forming a nano-level concave-convex anti-glare structure on the glass surface and completing the size locking. The tempered glass sheet is fed into a continuous roller washing tank. First, a 0.5% (w / w) food-grade citric acid aqueous solution is used at a constant temperature of 25°C to immerse and rinse one side of the glass after the phase separation treatment in step S3 for 10 seconds. This selectively removes the alkali-rich boron phase formed on the glass surface, creating a uniform nanoscale anti-glare structure. After rinsing, no further water washing is required. The glass sheet is immediately placed into a constant-temperature passivation tank at 40°C and immersed in a 0.2% (w / w) sodium silicate aqueous solution for 8 seconds. This forms a monolayer silica passivation film in situ on the nanoscale surface, precisely terminating the acid etching reaction and locking in the size and morphology of the anti-glare structure. After immersion, the glass sheet is rinsed with 0.3 MPa high-pressure deionized water on both sides until the pH of the rinsing solution is neutral, thoroughly removing any residual reaction solution from the surface.
[0045] S5. Drying and post-processing cutting: Rinse and dry the processed glass sheet, and complete the functional layer coating and size cutting according to the requirements to obtain the finished tempered glass film. The process involves sending the rinsed glass substrate into a Class 100 cleanroom hot air circulating oven and drying it at a constant temperature of 100℃ for 15 minutes to completely remove surface moisture, resulting in a clean anti-glare tempered glass substrate. An electron beam vacuum evaporation coating process is then used on the anti-glare surface to sequentially deposit a 120nm thick silica antireflective film and a 10nm thick fluoride waterproof and oleophobic layer, with the coating vacuum controlled at 5×10⁻³Pa. A UV nanosecond laser cutting machine is then used to cut and round the corners according to the preset dimensions of the tablet / watch screen, with the laser power set to 10W and the cutting speed at 250mm / s. After cutting, a full inspection of appearance and optical performance is performed, and defective products are removed to obtain the finished electronic screen tempered glass film with anti-glare function.
[0046] Example 3: This example provides an electronic screen tempered glass film with anti-glare function. The tempered glass film uses tempered glass substrate as the core functional carrier and contains the following raw materials in parts by weight: 72 parts of silicon dioxide, 16 parts of sodium oxide, 9 parts of calcium oxide, 3.5 parts of aluminum oxide, 7 parts of phase separation inducing composite component, 1.4 parts of phase separation regulating fluxing composite component, 0.5 parts of composite clarifying agent, and 0.8 parts of lithium carbonate. The phase-separation regulating flux composite component is composed of strontium oxide, sodium fluorosilicate, and phosphorus pentoxide in a mass ratio of 3.2:2.2:1.2; the phase-separation inducing composite component is composed of boron oxide, magnesium fluoride, and zirconium oxide in a mass ratio of 4.2:2.2:1.2; the mass ratio of the phase-separation regulating flux composite component to the phase-separation inducing composite component is 1.2:6; the composite clarifying agent is composed of cerium oxide and sodium chloride in a mass ratio of 1.1:1; the thickness of the tempered glass substrate is 0.4 mm, and a nanoscale concave-convex anti-glare structure is integrally formed on one side of the tempered glass substrate. This nanoscale concave-convex anti-glare structure is formed by metastable phase separation of the glass substrate, with a phase separation region size of 300 nm and a structural depth of 1 μm; a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure, with a thickness of 5 nm, which can seal surface micro-defects and improve the chemical stability of the glass.
[0047] The preparation method of the above-mentioned tempered glass film for electronic screens with anti-glare function includes the following steps: S1. Batching and Melting: Weigh the raw materials for preparing the tempered glass substrate according to the weight proportions, and complete the high-temperature melting and clarification and homogenization by feeding in stages and batches. Then, use the overflow and downward pulling method to form the glass sheet. The specific process of high-temperature melting with phased and batch feeding is as follows: In the first stage, silicon dioxide, sodium oxide, calcium oxide, aluminum oxide, and lithium carbonate were weighed according to their weight proportions and added to a horizontal high-speed mixer. The mixture was stirred at 500 r / min for 20 minutes. After mixing, the mixture was passed through a 200-mesh standard sieve to remove agglomerated particles, resulting in a uniform basic batch. The basic batch was placed in a 5L high-purity platinum crucible and then placed in a silicon molybdenum rod high-temperature box furnace. The mixture was melted at 1500℃ for 3 hours. During the melting process, a high-purity quartz stirring rod was used to continuously and uniformly stir the mixture at 100 r / min to eliminate local component inhomogeneity and form a homogeneous and transparent glass base melt. In the second stage, while maintaining a melting temperature of 1500℃ and continuous stirring, a composite clarifying agent is added to the glass base melt at a uniform rate. After the addition is completed, stirring is continued for 60 minutes to complete the clarification and homogenization. The high-temperature oxidation-reduction reaction of cerium oxide eliminates bubbles, streaks and stone defects in the glass melt. In the third stage, the furnace temperature is uniformly reduced to 1300℃, and the phase separation induction composite component and the phase separation regulation fluxing composite component are uniformly added to the melt. The mixture is stirred continuously for 80 minutes to ensure that the two components are uniformly dispersed in the glass melt network and to form a concentration gradient enriched on the surface. After stirring, the melt temperature is uniformly reduced to 1250℃, and the mixture is formed by an overflow pull-down device with a pull-down rate controlled at 6m / min to form a continuous glass ribbon with a thickness of 0.4mm. The ribbon is then cut into glass sheets of a preset size of 100mm×150mm by a diamond wheel and allowed to cool naturally to room temperature in a dust-free environment.
[0048] S2. Preheating and Homogenization and Atmosphere Control: After cleaning and drying, the glass sheet is sent to the preheating section of the tempering furnace to complete the preheating and homogenization treatment under a protective atmosphere. The process involves first placing the cooled glass sheet into a multi-tank ultrasonic cleaner, where it is ultrasonically cleaned sequentially with neutral glass cleaner and deionized water at a frequency of 40kHz and a cleaning time of 4 minutes per tank. After cleaning, the glass sheet is dried with clean hot air at 65℃ for 12 minutes to remove surface moisture and impurities. The dried glass sheet is then placed in the preheating section of a continuous horizontal tempering furnace. High-purity nitrogen is introduced throughout the preheating section to establish a protective atmosphere, with nitrogen purity controlled at ≥99.99% and oxygen content ≤50ppm. A slight positive pressure of 100Pa is maintained inside the furnace to prevent oxidation of the glass surface and volatilization of phase-separated components at high temperatures. Atmosphere control continues until the end of the hot air quenching stage in step S3. The preheating section has three gradient temperature zones, with the final constant temperature zone stabilizing at 650℃. The total residence time of the glass sheet in the preheating section is 120s, ensuring that the overall glass temperature reaches a uniform range of ±10℃ from the glass transition temperature, eliminating internal stress and providing a uniform temperature basis for subsequent tempering and phase separation treatment.
[0049] S3, Tempering-Phase Separation Synchronous Gradient Quenching and Electric Field Assisted Coupling: The preheated glass sheet is sent into the tempering furnace quenching section. A two-stage gradient air cooling quenching process including hot air quenching and cold air quenching is adopted. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied to the glass sheet for auxiliary treatment, so as to achieve controllable metastable phase separation on the glass surface while completing physical tempering. The two-stage gradient air cooling quenching process is as follows: first, the first stage of hot air quenching and electric field assisted treatment is performed, and then the second stage of cold air quenching and tempering is performed. The two stages are completed continuously in the same quenching section without intermediate stops. The parameters for the first stage of hot air quenching and electric field-assisted treatment are as follows: hot air is output using nozzles arranged symmetrically at the top and bottom, with a wind pressure of 0.5 MPa, a wind temperature of 220℃, a distance of 15 mm between the nozzles and the glass surface, and hot air quenching lasts for 25 seconds; during the quenching process, a low-frequency alternating electric field perpendicular to the glass surface is simultaneously applied to the original glass sheet through parallel flat electrodes set at the top and bottom of the quenching section. The electric field parameters are AC voltage of 800V and frequency of 25Hz, and the duration of electric field application is exactly the same as the duration of hot air quenching; the glass surface temperature is precisely reduced to 600℃ by hot air temperature control, and with the electric field driving the directional migration of alkali metal ions, controllable metastable phase separation is completed within a depth of 1 μm on the glass surface, forming a uniform silicon-rich phase and an alkali-rich boron phase; The parameters for the second stage of cold air quenching tempering and shaping are as follows: After the hot air quenching and electric field application are completed, the electric field output is immediately stopped, and the air path is simultaneously switched to room temperature clean compressed air. Cold air with a pressure of 1.2 MPa and a temperature of 30°C is used for rapid quenching. The distance between the air nozzle and the glass surface is maintained at 15 mm. The cold air quenching lasts for 40 seconds, so that the overall temperature of the glass drops sharply to below 200°C within 10 seconds, and finally cools to room temperature. A uniform compressive stress layer of 800 MPa is formed on the glass surface through rapid temperature change, completing the physical tempering. At the same time, the phase separation structure on the glass surface is quickly locked to prevent excessive growth of the phase separation region from damaging the optical performance.
[0050] S4. Integrated rinsing-passivation treatment: The tempered glass sheet is first rinsed with a weak acid solution of citric acid, and then soaked in a sodium silicate solution for in-situ passivation treatment, forming a nano-level concave-convex anti-glare structure on the glass surface and completing the size locking. The tempered glass sheet is fed into a continuous roller washing tank. First, a 1.0% (w / w) food-grade citric acid aqueous solution is used at a constant temperature of 30°C to immerse and rinse one side of the glass after the phase separation treatment in step S3 for 15 seconds. This selectively removes the alkali-rich boron phase formed on the glass surface, creating a uniform nanoscale anti-glare structure. After rinsing, no further water washing is required. The glass sheet is immediately placed in a constant-temperature passivation tank at 45°C and immersed in a 0.5% (w / w) sodium silicate aqueous solution for 12 seconds. This forms a monolayer silica passivation film in situ on the nanoscale surface, precisely terminating the acid etching reaction and locking in the size and morphology of the anti-glare structure. After immersion, the glass sheet is rinsed with 0.3 MPa high-pressure deionized water on both sides until the pH of the rinsing solution is neutral, thoroughly removing any residual reaction solution from the surface.
[0051] S5. Drying and post-processing cutting: Rinse and dry the processed glass sheet, and complete the functional layer coating and size cutting according to the requirements to obtain the finished tempered glass film. The rinsed glass substrate is placed in a Class 100 cleanroom hot air circulating oven and dried at a constant temperature of 120℃ for 20 minutes to completely remove surface moisture, resulting in a clean anti-glare tempered glass substrate. First, an electron beam vacuum evaporation coating process is used to deposit a 150nm thick silicon dioxide antireflective film and a 15nm thick fluoride waterproof and oleophobic layer onto the anti-glare surface. The coating vacuum degree is controlled at 5×10⁻⁶. -3 Pa; then, a slit coating process is used on the non-anti-glare surface of the glass substrate to coat an acrylic optical pressure-sensitive adhesive with a thickness of 30μm. After coating, it is cured at 50℃ for 5 minutes, and then a 75μm thick PET release film is laminated; a UV nanosecond laser cutting machine is used to cut and round the corners according to the preset size of the flat panel / vehicle screen. The laser power is set to 15W and the cutting speed is 150mm / s; after cutting, a full inspection of appearance and optical performance is carried out, and defective products are rejected to obtain the finished product of electronic screen tempered glass film with anti-glare function.
[0052] Comparative Example 1: The only difference between this comparative example and Example 1 is that the phase separation-induced composite component in the formula is removed, the missing weight parts are made up with an equal proportion of silica, and all other raw material ratios, preparation processes and parameters are completely consistent with Example 1.
[0053] Comparative Example 2: The only difference between this comparative example and Example 1 is that the phase separation control fluxing composite component in the formula is removed, and the missing weight parts are made up with an equal proportion of silicon dioxide. All other raw material ratios, preparation processes, and parameters are completely consistent with Example 1.
[0054] Comparative Example 3: The only difference between this comparative example and Example 1 is that the first stage of hot air quenching in the two-stage gradient air cooling quenching process is omitted in step S3. Instead, the preheated glass sheet is directly subjected to one-step cold air quenching using the second stage cold air quenching parameters. All other raw material ratios, preparation processes, and parameters are completely consistent with Example 1.
[0055] Comparative Example 4: The only difference between this comparative example and Example 1 is that a low-frequency alternating electric field is not applied during the first stage of hot air quenching in step S3. All other raw material ratios, preparation processes, and parameters are completely consistent with Example 1.
[0056] Comparative Example 5: The only difference between this comparative example and Example 1 is that the anti-glare structure is prepared using the industry-standard tempering followed by hydrofluoric acid chemical etching process. Specifically, the phase separation induction composite component and phase separation regulation flux composite component in the formula are removed, and the missing weight parts are supplemented with an equal proportion of silicon dioxide. All raw materials are mixed and melted at one time and formed into a glass sheet by overflow pull-down method. After conventional physical tempering, the glass sheet is etched for 120s using a hydrofluoric acid frosting solution to form an anti-glare structure, followed by polishing and cleaning. The subsequent coating and cutting steps are completely consistent with Example 1, and all other parameters are consistent with Example 1.
[0057] I. Comprehensive Optical Performance Testing of Anti-Glare Tempered Glass Film: The testing standards were GB / T31831-2015 "Tempered Glass Protective Film for Flat Panel Display Devices" and GB / T2680-2021 "Determination of Visible Light Transmittance, Direct Solar Transmittance, Total Solar Transmittance, Ultraviolet Transmittance and Related Window Glass Parameters of Architectural Glass". Parallel tests were conducted on samples from Examples 1-3 and Comparative Examples 1-5 using an ultraviolet-visible-near-infrared spectrophotometer, haze meter, sharpness tester, and specular reflectance meter. All samples were cut to a standard size of 100mm × 100mm, with 10 parallel samples prepared for each group. The testing environment was 23℃±2℃ and 50%±5% relative humidity. First, the average visible light transmittance of the samples in the 380nm to 780nm visible light band was measured using an ultraviolet-visible-near-infrared spectrophotometer. The test results were as follows: First, the transmittance was measured at 5nm intervals, and the average value of 10 parallel samples was taken as the final test result. Second, a haze meter was used to test the haze value of the samples according to the standard integrating sphere method. Before testing, the instrument was calibrated using a standard calibration plate. Each group of samples was tested 3 times and the average value was taken. Then, a sharpness meter was used to test the image sharpness of the samples. During the test, the sample was placed close to the surface of the standard test image, and the image was acquired and the sharpness value was calculated through the instrument's built-in optical system. Finally, a specular reflectance meter was used to test the specular reflectance of the samples at a 60° incident angle. Five different points were tested for each group of samples and the average value was taken. All test procedures strictly followed the corresponding standard operating procedures, and the four core optical parameters of visible light transmittance, haze, sharpness, and specular reflectance of all samples were fully recorded to comprehensively evaluate the anti-glare effect and high-resolution screen display adaptation performance of the samples.
[0058] II. Mechanical Performance Testing of Anti-Glare Tempered Glass Film: The testing standard was GB / T31831-2015 "Tempered Glass Protective Film for Flat Panel Display Devices". A glass surface stress meter and a falling ball impact tester were used to test the mechanical properties of samples from Examples 1-3 and Comparative Examples 1-5. All samples were cut to the standard size of a 150mm × 75mm mobile phone screen. Twenty parallel samples were prepared for each group. The testing environment was a temperature of 23℃±2℃ and a relative humidity of 50%±5%. First, the surface compressive stress value and compressive stress layer depth of the samples were tested using a glass surface stress meter. A immersion solution with the corresponding refractive index was used during the test. Ten samples were tested in each group, and the average value was taken from three different points on each sample. Strict adherence to the test criteria was maintained. The operation was completed according to the standard testing procedure. Subsequently, the impact resistance performance was tested using a falling ball impact tester. The sample was fixed horizontally on a standard test fixture with an inner frame size of 140mm × 65mm. A standard steel ball with a mass of 32g was dropped freely from a height of 1.5m to impact the center of the sample. All 20 samples in each group were tested. The number of qualified samples that did not break was recorded, and the impact pass rate was calculated. At the same time, the breakage state of the broken samples was recorded to evaluate the tempering safety performance of the samples. By using two indicators, surface compressive stress and falling ball impact performance, the mechanical properties of the tempering of the samples were comprehensively verified to see whether they were affected by the preparation process of the anti-glare structure, and to verify the effect of balancing anti-glare function and tempering mechanical properties.
[0059] III. Long-term reliability test of anti-glare tempered glass film under constant humidity and heat environment. The test standard is GB / T2423.3-2006 "Environmental testing for electrical and electronic products - Part 2: Test methods - Test Cab: Constant humidity and heat test". The samples of Examples 1-3 and Comparative Examples 1-5 were divided into optical test group and mechanical test group. Twenty parallel samples were prepared for each group. All samples first completed the initial optical performance and initial mechanical performance tests according to the standards and methods of the above two tests, and the initial values were recorded completely. Then all samples were placed in a constant temperature and humidity test chamber. The test conditions were set according to the standard requirements: temperature 85℃, relative humidity 85%, and test duration 1000h. During the test, the environment inside the test chamber was maintained. With stable parameters, samples were kept at a distance of more than 5 mm to avoid mutual obstruction affecting the test results. After the test, the samples were taken out and left to stand for 24 hours in a normal temperature and humidity environment. Then, the optical and mechanical properties of the aged samples were tested according to the aforementioned test standards and methods. The performance retention rate of visible light transmittance, clarity, and surface compressive stress of each sample, as well as the change of drop ball impact pass rate, were calculated. At the same time, the structural integrity of the sample surface was observed using a high-magnification optical microscope, and the presence of defects such as coating peeling, surface corrosion, and microcracks was recorded. The long-term reliability of the samples under high temperature and high humidity harsh environments was comprehensively evaluated, and the performance advantages of the integrated design of the anti-glare structure and glass substrate were verified.
[0060] Table 1: Comprehensive Test Results of Optical Performance of Anti-Glare Tempered Glass Film Sample number Visible light transmittance (%) Haze (%) Image sharpness (%) 60° specular reflectance (%) Example 1 94.2 2.8 96.5 1.0 Example 2 93.5 1.8 97.2 1.1 Example 3 93.8 3.7 95.3 0.8 Comparative Example 1 91.8 0.3 98.1 4.2 Comparative Example 2 88.5 7.6 82.3 1.5 Comparative Example 3 91.5 0.4 97.8 4.3 Comparative Example 4 87.2 8.9 78.5 1.3 Comparative Example 5 89.2 5.2 86.7 1.8 Table 2: Test Results of Mechanical Properties of Anti-Glare Tempered Glass Film Sample number Surface compressive stress (MPa) Depth of compressive stress layer (μm) Pass rate of impact test of 32g steel ball dropped from 1.5m (%) Example 1 702 12.5 100 Example 2 615 11.2 100 Example 3 798 13.8 100 Comparative Example 1 698 12.3 100 Comparative Example 2 695 12.2 95 Comparative Example 3 701 12.4 100 Comparative Example 4 692 12.1 95 Comparative Example 5 425 7.8 60 Table 3: Long-term reliability test results of anti-glare tempered glass film in constant humidity and heat environment (1000h 85℃ / 85%RH) Sample number Visible light transmittance retention rate (%) Image sharpness retention rate (%) Surface compressive stress retention rate (%) Pass rate of ball impact test after aging (%) Example 1 99.2 99.0 98.8 100 Example 2 99.0 99.1 98.5 100 Example 3 98.7 98.5 99.1 100 Comparative Example 1 98.5 98.8 98.2 100 Comparative Example 2 92.3 88.5 97.8 90 Comparative Example 3 98.3 98.7 98.1 100 Comparative Example 4 90.5 85.2 97.5 90 Comparative Example 5 82.6 75.8 82.1 30 Note: The surface condition of the samples in this experiment was observed using a 500x high-magnification optical microscope. The anti-glare functional surface of the samples after a 1000-hour constant humidity and heat test at 85℃ / 85%RH was scanned across the entire surface. The specific observation results are as follows: The anti-glare structure of the samples in Examples 1, 2, and 3 was intact, and no defects such as surface corrosion, microcracks, or structural detachment were observed. There was no significant difference from the initial surface state before the test. The glass surfaces of Comparative Example 1 and Comparative Example 3 did not have the phase-separated anti-glare structure designed in this scheme. After the test, no defects such as surface corrosion and microcracks were observed, and there was no significant difference from the initial surface state before the test. The anti-glare treatment surfaces of Comparative Examples 2 and 4 showed localized slight corrosion pitting, which was concentrated in areas of uneven phase separation on the glass surface. No other defects such as microcracks or structural detachment were observed. The anti-glare surface of the sample in Comparative Example 5, formed by hydrofluoric acid etching, showed obvious corrosion pits and irregular microcracks. The etched structure in some areas peeled off, and the surface morphology was significantly deteriorated compared with that before the test.
[0061] As can be seen from Examples 1-3 and Comparative Example 1, and Tables 1-3, the phase separation-induced composite component is the core foundation for constructing an anti-glare structure on the surface of the glass substrate. The presence or absence of this component directly determines whether the product can achieve an effective anti-glare effect. At the same time, the introduction of this component will not have a negative impact on the mechanical properties of the tempered glass or the structural stability during long-term use. It is a key raw material for achieving both anti-glare function and basic glass performance.
[0062] As can be seen from Examples 1-3 and Comparative Example 2, and Tables 1-3, there is a significant synergistic effect between the phase separation regulating flux composite component and the phase separation inducing composite component. This component can precisely regulate the nucleation rate and phase growth state during the glass phase separation process. The absence of this component will lead to the glass phase separation process going out of control, directly causing the deterioration of the product's optical performance. At the same time, it will also affect the chemical stability of the glass surface structure and reduce the long-term reliability of the product in harsh environments.
[0063] As can be seen from Examples 1-3 and Comparative Example 3, and Tables 1-3, the two-stage gradient air-cooling quenching process is the core process design for achieving simultaneous tempering and phase separation. The first stage of hot air quenching provides the necessary temperature window and reaction time for the controllable metastable phase separation on the glass surface. Without this step, an effective anti-glare structure cannot be formed during the tempering process. At the same time, this process design will not have an adverse effect on the mechanical properties of the tempered glass. It is a key link in achieving both process simplification and product performance.
[0064] As can be seen from Examples 1-3 and Comparative Example 4, and Tables 1-3, the low-frequency alternating electric field-assisted treatment can directionally drive the migration of functional ions in the glass, allowing the phase separation process to be precisely limited to a set depth range on the glass surface. The absence of this electric field-assisted step will cause the phase separation process to diffuse into the glass body, which will not only cause serious deterioration of the product's optical performance, but also destroy the uniformity of the glass surface structure, thereby affecting the product's long-term environmental resistance.
[0065] As can be seen from Examples 1-3 and Comparative Example 5, and Tables 1-3, this solution utilizes the technical route of constructing an integrated anti-glare structure through phase separation of the glass substrate itself. Compared with the industry mainstream process of tempering followed by chemical etching, this solution can fundamentally avoid damage to the tempered stress layer of the glass during the anti-glare treatment process. At the same time, it achieves a balance between anti-glare effect and high light transmittance and high-definition display performance, and significantly improves the long-term reliability of the product in high temperature and high humidity environments. It comprehensively solves the core performance pain points that have long existed in the existing mainstream processes.
[0066] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.
Claims
1. A tempered glass film for electronic screens with anti-glare function, characterized in that: The tempered glass film includes a tempered glass substrate, which is prepared from the following raw materials in parts by weight: 65-72 parts silicon dioxide, 12-16 parts sodium oxide, 6-9 parts calcium oxide, 1.5-3.5 parts aluminum oxide, 3.5-7 parts phase separation inducing composite component, 0.4-1.0 parts phase separation regulating fluxing composite component, 0.2-0.5 parts composite clarifying agent, and 0.3-0.8 parts lithium carbonate; The tempered glass substrate has a nanoscale concave-convex anti-glare structure integrally formed on one side surface. The nanoscale concave-convex anti-glare structure is formed by metastable phase separation of the glass substrate, with the phase separation region size being 100-300nm and the structure depth being 0.5-1μm.
2. The tempered glass film for electronic screens with anti-glare function according to claim 1, characterized in that: The phase-separation regulating fluxing composite component is composed of strontium oxide, sodium fluorosilicate, and phosphorus pentoxide in a mass ratio of (2.8-3.2):(1.8-2.2):(0.8-1.2). The phase separation-induced composite component is composed of boron oxide, magnesium fluoride, and zirconium oxide in a mass ratio of (3.8-4.2):(1.8-2.2):(0.8-1.2). The mass ratio of the phase separation-controlled fluxing composite component to the phase separation-induced composite component is (0.8-1.2):
6.
3. The tempered glass film for electronic screens with anti-glare function according to claim 1, characterized in that: The composite clarifying agent is composed of cerium oxide and sodium chloride in a mass ratio of (0.9-1.1):
1.
4. The tempered glass film for electronic screens with anti-glare function according to claim 1, characterized in that: The thickness of the tempered glass substrate is 0.2-0.4 mm, and a monolayer silicon dioxide passivation film is formed in situ on the surface of the nanoscale concave-convex anti-glare structure, the thickness of which is 1-5 nm.
5. A method for preparing a tempered glass film for an electronic screen with anti-glare function, characterized in that, A tempered glass film for an electronic screen with anti-glare function as described in any one of claims 1-4, comprising the following steps: S1. Batching and Melting: Weigh each raw material for preparing the tempered glass substrate, and use a staged batch feeding method to complete high-temperature melting, clarification and homogenization. Then, use the overflow pull-down method to form the glass sheet. S2. Preheating and Homogenization and Atmosphere Control: After cleaning and drying, the glass sheet is sent to the preheating section of the tempering furnace to complete the preheating and homogenization treatment under a protective atmosphere. S3, Tempering-Phase Separation Synchronous Gradient Quenching and Electric Field Assisted Coupling: The preheated glass sheet is sent into the tempering furnace quenching section. A two-stage gradient air cooling quenching process including hot air quenching and cold air quenching is adopted. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied to the glass sheet for auxiliary treatment, so as to achieve controllable metastable phase separation on the glass surface while completing physical tempering. S4. Integrated rinsing-passivation treatment: The tempered glass sheet is first rinsed with a weak acid solution of citric acid, and then soaked in a sodium silicate solution for in-situ passivation treatment, forming a nano-level concave-convex anti-glare structure on the glass surface and completing the size locking. S5. Drying and post-processing cutting: Rinse and dry the processed glass sheet, and complete the functional layer coating and size cutting according to the requirements to obtain the finished tempered glass film.
6. The method for preparing an anti-glare tempered glass film for electronic screens according to claim 5, characterized in that: In step S1, the specific process of high-temperature melting with phased and batch feeding is as follows: In the first stage, silicon dioxide, sodium oxide, calcium oxide, aluminum oxide and lithium carbonate are weighed according to the weight parts, and mixed evenly to obtain the basic batch material. The basic batch material is melted at 1450-1500℃ for 2-3 hours, and the mixture is continuously stirred during the melting process to form a glass base melt. In the second stage, while maintaining a melting temperature of 1450-1500℃, a composite clarifying agent is added to the glass base melt, and stirring is continued for 30-60 minutes to complete the clarification and homogenization. In the third stage, the glass melt is cooled to 1250-1300℃, and phase separation induction composite components and phase separation regulation fluxing composite components are added to the melt. After stirring continuously for 40-80 minutes, the temperature is lowered to 1200-1250℃, and the glass sheet with a thickness of 0.2-0.4mm is formed by overflow pull-down method. After cutting, it is naturally cooled to room temperature.
7. The method for preparing an anti-glare tempered glass film for electronic screens according to claim 5, characterized in that: In step S2, the protective atmosphere is nitrogen with a purity of ≥99.99%, the oxygen content in the furnace is controlled to be ≤50ppm, and a slight positive pressure of 50-100Pa is maintained in the furnace. The atmosphere control continues until the end of the hot air quenching stage in step S3. The preheating temperature is 620-650℃ and the preheating time is 80-120s.
8. The method for preparing an anti-glare tempered glass film for electronic screens according to claim 5, characterized in that: In step S3, the two-stage gradient air cooling quenching process is as follows: first, the first stage of hot air quenching and electric field assisted treatment is performed, and then the second stage of cold air quenching, tempering and shaping is performed. The parameters for the first stage of hot air quenching and electric field assisted treatment are as follows: hot air quenching with a wind pressure of 0.3-0.5MPa and a wind temperature of 180-220℃ is used for 15-25s. At the same time, a low-frequency alternating electric field perpendicular to the glass surface is applied. The electric field parameters are AC voltage of 500-800V and frequency of 15-25Hz. After treatment, the glass surface temperature drops to 580-600℃. The parameters for the second stage of cold air quenching and tempering are as follows: stop applying the electric field, switch to cold air quenching with a wind pressure of 0.8-1.2MPa and a wind temperature of 20-30℃, and continue for 30-40 seconds to form a compressive stress layer on the glass surface.
9. The method for preparing an anti-glare tempered glass film for electronic screens according to claim 5, characterized in that: In step S4, the citric acid aqueous solution has a mass fraction of 0.5-1.0% and a rinsing time of 10-15s; the sodium silicate aqueous solution has a mass fraction of 0.2-0.5% and a soaking time of 8-12s; after soaking, the glass slide is rinsed with deionized water until the pH of the rinsing solution is neutral.
10. The method for preparing an anti-glare tempered glass film for electronic screens according to claim 5, characterized in that: In step S5, the hot air temperature for drying is 100-120℃, and the drying time is 15-20 minutes to obtain an anti-glare tempered glass substrate. After the glass substrate is treated with a functional layer, it is cut and trimmed according to a preset size to obtain a finished electronic screen tempered glass film with anti-glare function.