Self-cleaning low-emissivity hollow coated glass and preparation process thereof
By forming a yttrium-doped zinc oxide and neodymium-molybdenum co-doped tin dioxide coating structure on the glass surface, and combining it with modified sericite and talc to form a hydrophobic coating, the problems of low-emissivity glass reflecting infrared rays reducing visible light transmittance and hydrophobic coatings being prone to aging are solved, achieving highly efficient self-cleaning and UV aging resistance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- SHANDONG JINGCHENG GLASS TECH CO LTD
- Filing Date
- 2026-02-26
- Publication Date
- 2026-05-12
AI Technical Summary
Existing low-emissivity glass reduces visible light transmittance while reflecting infrared radiation, and the hydrophobic self-cleaning coating is prone to aging under ultraviolet light, resulting in easy contamination of the glass surface and high maintenance costs.
A hydrophobic coating is formed by using a yttrium-doped zinc oxide and neodymium-molybdenum co-doped tin dioxide coating structure, combined with modified sericite and talc. The coating is then applied to the glass surface using magnetron sputtering and calcination processes to form a multilayer film, which enhances infrared reflection and visible light transmittance, and improves hydrophobicity and resistance to ultraviolet aging.
It improves the infrared reflection effect and visible light transmittance of insulated coated glass, enhances its hydrophobic self-cleaning properties and UV aging resistance, and reduces surface reflectivity and maintenance costs.
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Figure CN122010422A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of coated glass technology, specifically to a self-cleaning, low-emissivity insulated coated glass and its preparation process. Background Technology
[0002] Building energy consumption accounts for a significant portion of overall energy consumption, with heat loss through doors and windows accounting for 30%-40% of that. Low-emissivity (Low-E) glass, by depositing a thin film with high infrared reflectivity on its surface, effectively blocks indoor and outdoor heat radiation exchange, significantly reducing building heating and cooling energy consumption. Therefore, using LOW glass to reduce building energy loss is a current research focus. However, regardless of whether the LOW-E film is prepared by magnetron sputtering or chemical vapor deposition, the core functional layer of LOW-coated glass, while effectively reflecting infrared light, also naturally absorbs and reflects visible light, thus reducing the visible light transmittance of the glass.
[0003] Low-emissivity (LEE) glass mainly comes in two types: SnO2-based and silver-based. However, silver-based LEE glass has higher production costs, unstable film structure, and relatively poor durability. SnO2-based LEE glass, on the other hand, has lower production costs and features good transmittance and stable chemical properties. However, the free charge carriers in ordinary SnO2 mainly originate from intrinsic oxygen vacancy defects, resulting in a low natural concentration and uneven defect distribution, failing to meet the requirement of "high-efficiency infrared reflection." Furthermore, the presence of numerous impurities and lattice distortions in the pure SnO2 lattice intensifies charge carrier scattering and reduces mobility, further weakening infrared reflection capabilities. Consequently, the emissivity of the prepared coated glass is relatively high. Moreover, the glass substrate surface is mainly composed of silicon-oxygen bonds, while the surface of ordinary SnO2 coatings is chemically inert and lacks active groups capable of forming stable chemical bonds with silanol groups. The interface between the two relies more on weak van der Waals forces or physical adsorption than chemical bonding, resulting in poor adhesion and susceptibility to external environmental influences, leading to easy detachment of the SnO2 coating.
[0004] In addition, the exterior surface of building glass is exposed to the atmospheric environment for a long time, making it extremely easy for dust, pollutants and organic stains to adhere to it. This not only seriously affects the building's aesthetics and lighting, but also brings high maintenance costs and safety risks due to frequent manual cleaning. In the existing technology, most of the glass has a self-cleaning function by preparing a hydrophobic self-cleaning coating on the exterior surface of the glass to prevent pollution. However, under long-term ultraviolet light irradiation, the cross-linking structure of the existing hydrophobic self-cleaning coating is easily destroyed, causing the coating to lose its hydrophobicity.
[0005] Therefore, there is a need to propose a self-cleaning, low-emissivity insulated coated glass with high visible light transmittance, coating adhesion, and resistance to ultraviolet aging, as well as its preparation process. Summary of the Invention
[0006] To address the shortcomings of existing technologies, the present invention aims to provide a self-cleaning, low-emissivity hollow coated glass and its preparation process.
[0007] This invention provides a process for preparing self-cleaning, low-emissivity insulated coated glass, comprising the following steps: S1: Preparation of single-layer coated glass Yttrium-doped zinc oxide powder was prepared using zinc oxide and yttrium oxide as raw materials, and then yttrium-doped zinc oxide target material was prepared by cold pressing and sintering. The yttrium-doped zinc oxide target material was then magnetron sputtered onto the outer surface of the pretreated insulating glass substrate to form a yttrium-doped zinc oxide coating, thus obtaining a single-layer coated glass. S2: Preparation of double-layer coated glass S2.1: Add tin tetrachloride pentahydrate to ethylene glycol at a ratio of 1g:(15-20)mL. Under nitrogen protection, heat and stir at 180-200℃ for 50-60min. When the temperature drops to 100℃, add molybdenum hexacarbonyl and neodymium pentahydrate. Continue stirring for 30-40min, cool to room temperature, add anhydrous ethanol for dilution, and ultrasonically disperse for 10-20min to obtain the precursor sol. S2.2: The above-mentioned precursor sol is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the above-mentioned single-layer coated glass. After drying for 30-40 minutes, it is placed in a muffle furnace and calcined at 400-500℃ for 2-3 hours to form a neodymium-molybdenum co-doped tin dioxide coating with a thickness of 60-80 nm, thus obtaining a double-layer coated glass. S3: Preparation of three-layer coated glass On the surface of the neodymium-molybdenum co-doped tin dioxide coating of the above-mentioned double-layer coated glass, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 120-130s at an argon flow rate of 20-30 sccm, an oxygen flow rate of 2-4 sccm, 110-120W, 0.5Pa and 130-150℃. After cooling, the glass is annealed at 200-250℃ for 20-30min to form a yttrium-doped zinc oxide coating, thus obtaining a three-layer coated glass. S4: Preparation of modified sericite powder and modified talc powder First, aluminum isopropoxide is used as a raw material to prepare alumina sol. Then, sericite is activated and dispersed in deionized water. Alumina sol is added and mixed thoroughly to prepare modified sericite powder. Then, tetraethyl orthosilicate is used as a raw material to prepare silica sol. Activated talc is added and mixed thoroughly to prepare modified talc powder. S5: Preparation of Insulating Coated Glass The modified sericite powder and modified talc powder were dispersed in anhydrous ethanol to form a suspension. Then, methyltriethoxysilane was dissolved in anhydrous ethanol, and hydrochloric acid and ammonia were added in sequence to form a crosslinking liquid. The suspension was then added to the mixture to form a hydrophobic coating, which was then uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass to obtain hollow coated glass.
[0008] Furthermore, S1 includes the following steps: S1.1: The insulating glass substrate is ultrasonically cleaned with 75% ethanol solution and deionized water for 10-20 min in sequence, then dried with nitrogen gun, and then placed in magnetron sputtering vacuum chamber, and activated with argon gas at 80-100W plasma for 5-10 min to obtain pretreated glass substrate. S1.2: Dry zinc oxide powder and yttrium oxide powder at 110-120℃ for 2-3 hours, then add the dried zinc oxide powder and yttrium oxide powder to anhydrous ethanol at a ratio of (18-20) g: (0.5-0.6) g: (10-12) mL, ball mill at 200-300 rpm for 8-10 hours, and then heat and stir in a water bath at 80-90℃ until the ethanol is completely evaporated to obtain yttrium-doped zinc oxide powder; S1.3: Pass the above yttrium-doped zinc oxide powder through a 200-mesh sieve, then fill it evenly into a mold, cold press it at 200 MPa for 3-5 min, then place it in a muffle furnace, heat it to 500-600℃ at 5℃ / min in an oxygen atmosphere, hold it for 2-3 h, then continue to heat it to 1250-1300℃ at 3℃ / min, hold it for sintering for 2-3 h, and cool it to room temperature with the furnace to obtain the yttrium-doped zinc oxide target. S1.4: On the outer surface of the pretreated glass substrate, using the yttrium-doped zinc oxide target as the magnetron sputtering target, magnetron sputtering is performed for 120-130 seconds at an argon flow rate of 20-30 sccm, an oxygen flow rate of 2-4 sccm, a W of 110-120, a Pa of 0.5, and a temperature of 130-150°C. After cooling, the substrate is annealed at 200-250°C for 20-30 minutes to form a yttrium-doped zinc oxide coating, thus obtaining a single-layer coated glass.
[0009] Furthermore, S4 specifically includes the following steps: S4.1: Dissolve aluminum isopropoxide in anhydrous ethanol at a ratio of 1g:(2-4)mL, stir thoroughly until a transparent solution is formed, then add 26-28% of the volume of deionized water while stirring, continue stirring for 30-40min, add octadecyltrimethylammonium bromide, stir to dissolve, add citric acid to adjust the pH to 5-5.5, and then continue stirring to mature for 2-3h to obtain alumina sol; S4.2: Add sericite and anhydrous ethanol to deionized water at a ratio of (2.8-3) g: 1 mL: 1 mL, stir and mix for 10-20 min, then heat and stir at 45-55℃ for 2-3 h, cool, filter, wash with deionized water 2-3 times and dry to obtain activated sericite powder. S4.3: Add the above activated sericite powder to deionized water at a ratio of (3-4) g: 1 mL, and ultrasonically disperse for 10-20 min to obtain an activated sericite dispersion. Then, while stirring, add the above alumina sol and stir at 45-50℃ for 2-3 h. Then, ultrasonically treat for 20-30 min. After cooling, filter, vacuum dry, grind and sieve to obtain modified sericite powder. S4.4: Add talc powder to a hydrochloric acid solution with a pH of 3-4 at a ratio of (1.7-1.8) g: 1 mL, heat and stir at 45-50℃ for 1-2 h, cool, filter, wash three times with deionized water and dry to obtain activated talc powder; S4.5: Add tetraethyl orthosilicate to anhydrous ethanol at a ratio of 1g:(3.4-3.5)mL, stir thoroughly to dissolve, then add 10% deionized water (by volume of anhydrous ethanol) and 0.6-0.8% hydrochloric acid (by volume of anhydrous ethanol) at a concentration of 12mol / L. Continue stirring for 1-2 hours, then add polyethylene glycol 6000 and continue stirring for 2-3 hours to obtain silica sol. S4.6: Add the activated talc powder to the silica sol at a ratio of 1g:(1.3-1.5)mL, add 8-10% of the silica sol volume of deionized water and stir to form a suspension. Then heat and stir at 35-45℃ for 3-4h, then sonicate for 20-30min. After cooling, filter, vacuum dry, grind and sieve to obtain modified talc powder.
[0010] Furthermore, S5 includes the following steps: S5.1: Disperse the modified sericite powder obtained in step S4.3 and the modified talc powder obtained in step S4.6 in anhydrous ethanol at a mass ratio of 1:(3-5):(20-30), add hexadecyltrimethoxysilane, and stir for 1-2 hours to obtain a suspension. S5.2: Add methyltriethoxysilane to anhydrous ethanol at a volume ratio of 1:(8-10), stir and mix thoroughly, then add hydrochloric acid with a concentration of 0.01mol / L and an equal volume to methyltriethoxysilane, and stir and react for 1-2 hours. Then add ammonia water with a mass fraction of 28%, and continue stirring and reacting for 30-40 minutes. After standing for 8-10 hours, a crosslinking liquid is obtained. Then add the above suspension, stir and mix thoroughly to obtain a hydrophobic coating. S5.3: The above-mentioned hydrophobic coating is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass prepared in step S3. After drying and curing, a hydrophobic protective layer with a thickness of 50-60nm is formed, and hollow coated glass is obtained.
[0011] Furthermore, the amount of molybdenum hexacarbonyl added is 5-8% of the mass of tin tetrachloride pentahydrate, and the amount of neodymium pentahydrate added is 5-6% of the mass of tin tetrachloride pentahydrate.
[0012] Furthermore, the amount of octadecyltrimethylammonium bromide added is 0.1% of the mass of aluminum isopropoxide, and the volume ratio of alumina sol to activated sericite dispersion is (2.5-3):1.
[0013] Furthermore, the amount of polyethylene glycol 6000 added is 1.7-1.8% of the mass of tetraethyl orthosilicate.
[0014] Furthermore, both sericite and talc have a particle size of 4-6 μm.
[0015] Furthermore, the amount of hexadecyltrimethoxysilane added is 25% of the total mass of modified sericite powder and modified talc powder, the amount of ammonia added is 15-20% of the volume of methyltriethoxysilane, and the amount of suspension added is 28-32% of the volume of crosslinking liquid.
[0016] A self-cleaning, low-emissivity insulated coated glass, which is prepared by the preparation process of a self-cleaning, low-emissivity insulated coated glass described in any one of the above claims.
[0017] The present invention has the following advantages: 1. In this invention, tin tetrachloride pentahydrate is first dissolved, and then molybdenum hexacarbonyl and neodymium pentahydrate are added and thoroughly stirred to prepare a precursor sol. This sol is then uniformly coated onto the surface of the yttrium-doped zinc oxide coating of a single-layer coated glass. After calcination to form a neodymium-molybdenum co-doped tin dioxide coating, molybdenum transfers excess electrons to the conduction band of tin dioxide, increasing the concentration of free carriers. Neodymium can suppress carrier recombination and optimize the lattice arrangement of tin dioxide, reducing the resistance to carrier migration. The high concentration and high mobility of free carriers can efficiently reflect infrared radiation. In addition, neodymium-molybdenum co-doping can limit the degree of crystallization of tin dioxide, forming a loose amorphous crystalline structure, which disrupts the absorption path of infrared light, reduces energy loss, and further enhances the infrared reflection effect, thereby reducing the emissivity of the hollow coated glass.
[0018] 2. In this invention, by preparing yttrium-doped zinc oxide coatings before and after preparing the neodymium-molybdenum co-doped tin dioxide coating, forming a yttrium-doped zinc oxide coating-neodymium-molybdenum co-doped tin dioxide coating-yttrium-doped zinc oxide coating structure, the inner yttrium-doped zinc oxide coating can form strong covalent bonds with the hydroxyl groups on the surface of the insulating glass substrate. Simultaneously, the middle neodymium-molybdenum co-doped tin dioxide coating and the yttrium-doped zinc oxide coating are bonded through Sn-O-Zn bonds, effectively improving the adhesion between the neodymium-molybdenum co-doped tin dioxide coating and the insulating glass substrate. Furthermore, since both the yttrium-doped zinc oxide coating and the neodymium-molybdenum co-doped tin dioxide coating are wide-bandgap transparent materials, and the yttrium-doped zinc oxide coating-neodymium-molybdenum co-doped tin dioxide coating-yttrium-doped zinc oxide coating structure can smooth the large abrupt change in refractive index from air to glass, allowing light energy to penetrate more gently rather than be reflected, thereby significantly reducing the total surface reflectivity and increasing visible light transmittance.
[0019] 3. In this invention, modified sericite is coated with nano-alumina, and modified talc is coated with nano-silica. The modified sericite powder and modified talc are then dispersed in anhydrous ethanol, and a suspension is prepared by adding hexadecyltrimethoxysilane. This suspension is then added to a crosslinking liquid prepared using methyltriethoxysilane as a raw material to create a hydrophobic coating. This coating is then applied to the surface of a yttrium-doped zinc oxide layer on a three-layer coated glass to form a hydrophobic protective layer. Because the modified sericite powder and modified talc are mixed, the sheet-like substrates are interleaved and stacked, forming a concave nano-coating layer. The dense micro-nano surface with alternating convex phases increases the surface roughness of the coating, thereby further amplifying the hydrophobic effect and achieving the goal of synergistically improving the self-cleaning performance of the hydrophobic protective coating. In addition, the modified sericite and modified talc have complementary particle sizes and are stacked in parallel in the coating to form a dense ultraviolet barrier. At the same time, the alumina on the surface of the modified sericite and the silica on the surface of the modified talc can absorb ultraviolet photons and convert them into crystal nucleation vibration energy, preventing ultraviolet rays from damaging the cross-linked structure in the hydrophobic coating, thereby synergistically improving the anti-ultraviolet aging performance of the hydrophobic protective layer. Attached Figure Description
[0020] Figure 1 This is a flowchart illustrating the manufacturing process of the self-cleaning, low-emissivity insulated coated glass used in an embodiment of the present invention. Detailed Implementation
[0021] To enable those skilled in the art to better understand the technical solutions of this invention, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of this invention.
[0022] Example 1: A preparation process for self-cleaning, low-emissivity insulated coated glass, such as... Figure 1 As shown, it includes the following steps: S1: Preparation of single-layer coated glass S1.1: The insulating glass substrate is ultrasonically cleaned with 75% ethanol solution and deionized water for 10 min in sequence, then dried with nitrogen gun, and then placed in magnetron sputtering vacuum chamber, and activated with argon gas at 80W plasma for 5 min to obtain pretreated glass substrate. S1.2: Dry zinc oxide powder and yttrium oxide powder at 110℃ for 2 hours, then add the dried zinc oxide powder and yttrium oxide powder to anhydrous ethanol at a ratio of 18g:0.5g:10mL, ball mill at 200rpm for 8 hours, and then heat and stir in an 80℃ water bath until the ethanol is completely evaporated to obtain yttrium-doped zinc oxide powder. S1.3: The above yttrium-doped zinc oxide powder is passed through a 200-mesh sieve and then uniformly filled into a mold. It is cold-pressed at 200 MPa for 3 min and then placed in a muffle furnace. Under an oxygen atmosphere, the temperature is increased to 500°C at 5°C / min and held for 2 h. Then, the temperature is increased to 1250°C at 3°C / min and held for sintering for 2 h. The furnace is then cooled to room temperature to obtain the yttrium-doped zinc oxide target. S1.4: On the outer surface of the pretreated glass substrate, the yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 120 seconds at an argon flow rate of 20 sccm, an oxygen flow rate of 2 sccm, a W of 110 W, a Pa of 0.5 Pa, and a temperature of 130°C. After cooling, the substrate is annealed at 200°C for 20 minutes to form a yttrium-doped zinc oxide coating and obtain a single-layer coated glass. S2: Preparation of double-layer coated glass S2.1: Add tin tetrachloride pentahydrate to ethylene glycol at a ratio of 1g:15mL. Under nitrogen protection, heat and stir at 180℃ for 50min. When the temperature drops to 100℃, add molybdenum hexacarbonyl and neodymium pentahydrate. Continue stirring for 30min, cool to room temperature, dilute with anhydrous ethanol, and ultrasonically disperse for 10min to obtain the precursor sol. The amount of molybdenum hexacarbonyl added is 6% of the mass of tin tetrachloride pentahydrate, and the amount of neodymium pentahydrate added is 5% of the mass of tin tetrachloride pentahydrate. S2.2: The above precursor sol is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the single-layer coated glass obtained in step S1.4. After drying for 30 minutes, it is placed in a muffle furnace and calcined at 400°C for 2 hours to form a neodymium-molybdenum co-doped tin dioxide coating with a thickness of 60 nm, thus obtaining a double-layer coated glass. S3: Preparation of three-layer coated glass On the surface of the neodymium-molybdenum co-doped tin dioxide coating of the above-mentioned double-layer coated glass, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 120s at an argon flow rate of 20sccm, an oxygen flow rate of 2sccm, 110W, 0.5Pa and 130℃. After cooling, the glass is annealed at 200℃ for 20min to form a yttrium-doped zinc oxide coating, thus obtaining a three-layer coated glass. S4: Preparation of modified sericite powder and modified talc powder S4.1: Dissolve aluminum isopropoxide in anhydrous ethanol at a ratio of 1 g: 2 mL, and stir thoroughly until a clear solution is formed. Then, while stirring, add 26% deionized water (by volume of anhydrous ethanol), and continue stirring for 30 min. Add octadecyltrimethylammonium bromide, stir to dissolve, and add citric acid to adjust the pH to 5. Then, continue stirring and aging for 2 h to obtain alumina sol. The amount of octadecyltrimethylammonium bromide added is 0.1% of the mass of aluminum isopropoxide. S4.2: Add sericite with a particle size of about 4μm and anhydrous ethanol to deionized water at a ratio of 2.8g:1mL:1mL, stir and mix for 10min, then heat and stir at 45℃ for 2h, cool, filter, wash twice with deionized water and dry to obtain activated sericite powder. S4.3: Add the above activated sericite powder to deionized water at a ratio of 3g:1mL, and ultrasonically disperse for 10min to obtain an activated sericite dispersion. Then, while stirring, add the above alumina sol and stir at 45℃ for 2h. After ultrasonic treatment for 20min, cool, filter, vacuum dry, grind and sieve to obtain modified sericite powder. The volume ratio of alumina sol to activated sericite dispersion is 2.5:1. S4.4: Add talc powder with a particle size of about 4 μm to a hydrochloric acid solution with pH 3 at a ratio of 1.7 g: 1 mL, heat and stir at 45 °C for 1 h, cool, filter, wash three times with deionized water and dry to obtain activated talc powder; S4.5: Add tetraethyl orthosilicate to anhydrous ethanol at a ratio of 1 g: 3.4 mL, stir thoroughly to dissolve, then add 10% deionized water (by volume of anhydrous ethanol) and 0.6% hydrochloric acid (by volume of anhydrous ethanol) at a concentration of 12 mol / L. Continue stirring for 1 hour, then add polyethylene glycol 6000 and continue stirring for 2 hours to obtain silica sol. The amount of polyethylene glycol 6000 added is 1.7% of the mass of tetraethyl orthosilicate. S4.6: Add the activated talc powder to the silica sol at a ratio of 1g:1.3mL, add 8% of the silica sol volume of deionized water and stir to form a suspension, then heat and stir at 35℃ for 3h, then sonicate for 20min, cool, filter, vacuum dry, grind and sieve to obtain modified talc powder. S5: Preparation of Insulating Coated Glass S5.1: Disperse the modified sericite powder obtained in step S4.3 and the modified talc powder obtained in step S4.6 in anhydrous ethanol at a mass ratio of 1:3:20, add hexadecyltrimethoxysilane, and stir for 1 hour to obtain a suspension, wherein the amount of hexadecyltrimethoxysilane added is 25% of the total mass of the modified sericite powder and the modified talc powder; S5.2: Add methyltriethoxysilane to anhydrous ethanol at a volume ratio of 1:8, stir and mix thoroughly, then add hydrochloric acid with a concentration of 0.01 mol / L and an equal volume to methyltriethoxysilane, and stir and react for 1 hour. Then add ammonia water with a mass fraction of 28%, continue stirring and reacting for 30 minutes, and let stand for 8 hours to obtain a crosslinking liquid. Then add the above suspension, stir and mix thoroughly to obtain a hydrophobic coating. The amount of ammonia water added is 15% of the volume of methyltriethoxysilane, and the amount of suspension added is 28% of the volume of the crosslinking liquid. S5.3: The above-mentioned hydrophobic coating is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass prepared in step S3. After drying and curing, a hydrophobic protective layer with a thickness of 50 nm is formed, and hollow coated glass is obtained.
[0023] Example 2: A preparation process for self-cleaning, low-emissivity insulated coated glass, such as... Figure 1 As shown, it includes the following steps: S1: Preparation of single-layer coated glass S1.1: The insulating glass substrate was ultrasonically cleaned with 75% ethanol solution and deionized water for 15 min in sequence, then dried with nitrogen gun, and then placed in magnetron sputtering vacuum chamber, and activated with argon gas at 90W plasma for 7.5 min to obtain pretreated glass substrate. S1.2: Zinc oxide powder and yttrium oxide powder were dried at 115℃ for 2.5h, and then the dried zinc oxide powder and yttrium oxide powder were added to anhydrous ethanol at a ratio of 19g:0.55g:11mL. The mixture was ball-milled at 250rpm for 9h, and then heated and stirred in a water bath at 85℃ until the ethanol was completely evaporated to obtain yttrium-doped zinc oxide powder. S1.3: The above-mentioned yttrium-doped zinc oxide powder is passed through a 200-mesh sieve and then uniformly filled into a mold. It is cold-pressed at 200 MPa for 4 min, and then placed in a muffle furnace. Under an oxygen atmosphere, the temperature is increased to 550°C at 5°C / min and held for 2.5 h. Then, the temperature is increased to 1275°C at 3°C / min and held for sintering for 2.5 h. The furnace is then cooled to room temperature to obtain the yttrium-doped zinc oxide target. S1.4: On the outer surface of the pretreated glass substrate, the yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 125 seconds at an argon flow rate of 25 sccm, an oxygen flow rate of 3 sccm, 115 W, 0.5 Pa, and 140 °C. After cooling, the substrate is annealed at 225 °C for 25 minutes to form a yttrium-doped zinc oxide coating and obtain a single-layer coated glass. S2: Preparation of double-layer coated glass S2.1: Add stannous tetrachloride pentahydrate to ethylene glycol at a ratio of 1g:17.5mL. Under nitrogen protection, heat and stir at 190℃ for 55min. When the temperature drops to 100℃, add molybdenum hexacarbonyl and neodymium pentahydrate. Continue stirring for 35min, cool to room temperature, dilute with anhydrous ethanol, and ultrasonically disperse for 15min to obtain the precursor sol. The amount of molybdenum hexacarbonyl added is 7% of the mass of stannous tetrachloride pentahydrate, and the amount of neodymium pentahydrate added is 5.5% of the mass of stannous tetrachloride pentahydrate. S2.2: The above precursor sol is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the single-layer coated glass obtained in step S1.4. After drying for 35 minutes, it is placed in a muffle furnace and calcined at 450°C for 2.5 hours to form a neodymium-molybdenum co-doped tin dioxide coating with a thickness of 70 nm, thus obtaining a double-layer coated glass. S3: Preparation of three-layer coated glass On the surface of the neodymium-molybdenum co-doped tin dioxide coating of the above-mentioned double-layer coated glass, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed at 25 sccm argon flow rate, 3 sccm oxygen flow rate, 115 W, 0.5 Pa and 140 °C for 125 s. After cooling, it is annealed at 225 °C for 25 min to form a yttrium-doped zinc oxide coating, thus obtaining a three-layer coated glass. S4: Preparation of modified sericite powder and modified talc powder S4.1: Dissolve aluminum isopropoxide in anhydrous ethanol at a ratio of 1 g: 3 mL, and stir thoroughly until a clear solution is formed. Then, while stirring, add 27% deionized water (by volume of anhydrous ethanol), and continue stirring for 35 min. Add octadecyltrimethylammonium bromide, stir to dissolve, and add citric acid to adjust the pH to 5. Then, continue stirring and aging for 2.5 h to obtain alumina sol. The amount of octadecyltrimethylammonium bromide added is 0.1% of the mass of aluminum isopropoxide. S4.2: Add sericite with a particle size of about 5 μm and anhydrous ethanol to deionized water at a ratio of 2.9 g: 1 mL: 1 mL, stir and mix for 15 min, then heat and stir at 50 °C for 2.5 h, cool, filter, wash twice with deionized water and dry to obtain activated sericite powder. S4.3: The activated sericite powder was added to deionized water at a ratio of 3.5g:1mL, and ultrasonically dispersed for 15min to obtain an activated sericite dispersion. Then, the alumina sol was added while stirring, and the mixture was stirred at 47.5℃ for 2.5h, followed by ultrasonic treatment for 25min. After cooling, the mixture was filtered, vacuum dried, ground, and sieved to obtain modified sericite powder. The volume ratio of alumina sol to activated sericite dispersion was 2.75:1. S4.4: Add talc powder with a particle size of about 5 μm to a hydrochloric acid solution with a pH of 3.5 at a ratio of 1.75 g: 1 mL, heat and stir at 47.5 °C for 1.5 h, cool, filter, wash three times with deionized water and dry to obtain activated talc powder; S4.5: Add tetraethyl orthosilicate to anhydrous ethanol at a ratio of 1 g: 3.45 mL, stir thoroughly to dissolve, then add 10% deionized water (by volume of anhydrous ethanol) and 0.7% hydrochloric acid (by volume of anhydrous ethanol) at a concentration of 12 mol / L. Continue stirring for 1.5 h, then add polyethylene glycol 6000 and continue stirring for 2.5 h to obtain silica sol. The amount of polyethylene glycol 6000 added is 1.75% of the mass of tetraethyl orthosilicate. S4.6: Add the activated talc powder to the silica sol at a ratio of 1g:1.4mL, add 9% of the silica sol volume of deionized water and stir to form a suspension, then heat and stir at 40℃ for 3.5h, then sonicate for 25min, cool, filter, vacuum dry, grind and sieve to obtain modified talc powder. S5: Preparation of Insulating Coated Glass S5.1: Disperse the modified sericite powder obtained in step S4.3 and the modified talc powder obtained in step S4.6 in anhydrous ethanol at a mass ratio of 1:4:25, add hexadecyltrimethoxysilane, and stir for 1.5 h to obtain a suspension, wherein the amount of hexadecyltrimethoxysilane added is 25% of the total mass of the modified sericite powder and the modified talc powder; S5.2: Methyltriethoxysilane was added to anhydrous ethanol at a volume ratio of 1:9. After thorough mixing, hydrochloric acid with a concentration of 0.01 mol / L and an equal volume to methyltriethoxysilane was added. The mixture was stirred and reacted for 1.5 h. Then, ammonia water with a mass fraction of 28% was added, and the mixture was stirred and reacted for another 35 min. After standing for 9 h, a crosslinking liquid was obtained. The above suspension was then added, and the mixture was stirred and mixed thoroughly to obtain a hydrophobic coating. The amount of ammonia water added was 17.5% of the volume of methyltriethoxysilane, and the amount of suspension added was 30% of the volume of the crosslinking liquid. S5.3: The above-mentioned hydrophobic coating is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass prepared in step S3. After drying and curing, a hydrophobic protective layer with a thickness of 55nm is formed, and hollow coated glass is obtained.
[0024] Example 3: A preparation process for self-cleaning, low-emissivity insulated coated glass, such as... Figure 1 As shown, it includes the following steps: S1: Preparation of single-layer coated glass S1.1: The insulating glass substrate is ultrasonically cleaned with 75% ethanol solution and deionized water for 20 min in sequence, then dried with nitrogen gun, and then placed in magnetron sputtering vacuum chamber, and activated with argon gas at 100W plasma for 10 min to obtain pretreated glass substrate. S1.2: Dry zinc oxide powder and yttrium oxide powder at 120℃ for 3 hours, then add the dried zinc oxide powder and yttrium oxide powder to anhydrous ethanol at a ratio of 20g:0.6g:12mL, ball mill at 300rpm for 10 hours, and then heat and stir in a 90℃ water bath until the ethanol is completely evaporated to obtain yttrium-doped zinc oxide powder. S1.3: The above-mentioned yttrium-doped zinc oxide powder is passed through a 200-mesh sieve and then uniformly filled into a mold. It is cold-pressed at 200 MPa for 5 min and then placed in a muffle furnace. Under an oxygen atmosphere, the temperature is increased to 600°C at 5°C / min and held for 3 h. Then, the temperature is increased to 1300°C at 3°C / min and held for sintering for 3 h. The furnace is then cooled to room temperature to obtain the yttrium-doped zinc oxide target. S1.4: On the outer surface of the pretreated glass substrate, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 130s at an argon flow rate of 30sccm, an oxygen flow rate of 4sccm, 120W, 0.5Pa and 150℃. After cooling, the substrate is annealed at 250℃ for 30min to form a yttrium-doped zinc oxide coating and obtain a single-layer coated glass. S2: Preparation of double-layer coated glass S2.1: Add tin tetrachloride pentahydrate to ethylene glycol at a ratio of 1g:20mL. Under nitrogen protection, heat and stir at 200℃ for 60min. When the temperature drops to 100℃, add molybdenum hexacarbonyl and neodymium pentahydrate. Continue stirring for 40min, cool to room temperature, dilute with anhydrous ethanol, and ultrasonically disperse for 20min to obtain the precursor sol. The amount of molybdenum hexacarbonyl added is 8% of the mass of tin tetrachloride pentahydrate, and the amount of neodymium pentahydrate added is 6% of the mass of tin tetrachloride pentahydrate. S2.2: The above precursor sol is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the single-layer coated glass obtained in step S1.4. After drying for 40 minutes, it is placed in a muffle furnace and calcined at 500°C for 3 hours to form a neodymium-molybdenum co-doped tin dioxide coating with a thickness of 80 nm, thus obtaining a double-layer coated glass. S3: Preparation of three-layer coated glass On the surface of the neodymium-molybdenum co-doped tin dioxide coating of the above-mentioned double-layer coated glass, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed at 30 sccm argon flow rate, 4 sccm oxygen flow rate, 120 W, 0.5 Pa and 150 °C for 130 s. After cooling, it is annealed at 250 °C for 30 min to form a yttrium-doped zinc oxide coating, thus obtaining a triple-layer coated glass. S4: Preparation of modified sericite powder and modified talc powder S4.1: Dissolve aluminum isopropoxide in anhydrous ethanol at a ratio of 1 g: 4 mL, and stir thoroughly until a clear solution is formed. Then, while stirring, add 28% deionized water (by volume of anhydrous ethanol), and continue stirring for 40 min. Add octadecyltrimethylammonium bromide, stir to dissolve, and add citric acid to adjust the pH to 5.5. Then, continue stirring and aging for 3 h to obtain alumina sol. The amount of octadecyltrimethylammonium bromide added is 0.1% of the mass of aluminum isopropoxide. S4.2: Add sericite with a particle size of about 6 μm and anhydrous ethanol to deionized water at a ratio of 3 g: 1 mL: 1 mL, stir and mix for 20 min, then heat and stir at 55 °C for 3 h, cool, filter, wash three times with deionized water and dry to obtain activated sericite powder. S4.3: Add the above activated sericite powder to deionized water at a ratio of 4g:1mL, and ultrasonically disperse for 20min to obtain an activated sericite dispersion. Then, while stirring, add the above alumina sol and stir at 50℃ for 3h. After ultrasonic treatment for 30min, cool, filter, vacuum dry, grind and sieve to obtain modified sericite powder. The volume ratio of alumina sol to activated sericite dispersion is 3:1. S4.4: Add talc powder with a particle size of about 6 μm to a hydrochloric acid solution with pH 4 at a ratio of 1.8 g: 1 mL, heat and stir at 50 °C for 2 h, cool, filter, wash three times with deionized water and dry to obtain activated talc powder; S4.5: Add tetraethyl orthosilicate to anhydrous ethanol at a ratio of 1 g: 3.5 mL, stir thoroughly to dissolve, then add 10% deionized water (by volume of anhydrous ethanol) and 0.8% hydrochloric acid (by volume of anhydrous ethanol) at a concentration of 12 mol / L. Continue stirring for 2 hours, then add polyethylene glycol 6000 and continue stirring for 3 hours to obtain silica sol. The amount of polyethylene glycol 6000 added is 1.8% of the mass of tetraethyl orthosilicate. S4.6: Add the activated talc powder to the silica sol at a ratio of 1g:1.5mL, add 10% of the silica sol volume of deionized water and stir to form a suspension, then heat and stir at 45℃ for 4h, then sonicate for 30min, cool, filter, vacuum dry, grind and sieve to obtain modified talc powder. S5: Preparation of Insulating Coated Glass S5.1: Disperse the modified sericite powder obtained in step S4.3 and the modified talc powder obtained in step S4.6 in anhydrous ethanol at a mass ratio of 1:5:30, add hexadecyltrimethoxysilane, and stir for 2 hours to obtain a suspension, wherein the amount of hexadecyltrimethoxysilane added is 25% of the total mass of the modified sericite powder and the modified talc powder; S5.2: Add methyltriethoxysilane to anhydrous ethanol at a volume ratio of 1:10, stir and mix thoroughly, then add hydrochloric acid with a concentration of 0.01 mol / L and an equal volume to methyltriethoxysilane, and stir and react for 2 hours. Then add ammonia water with a mass fraction of 28%, and continue stirring and reacting for 40 minutes. After standing for 10 hours, a crosslinking liquid is obtained. Then add the above suspension, stir and mix thoroughly to obtain a hydrophobic coating. The amount of ammonia water added is 20% of the volume of methyltriethoxysilane, and the amount of suspension added is 32% of the volume of the crosslinking liquid. S5.3: The above-mentioned hydrophobic coating is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass prepared in step S3. After drying and curing, a hydrophobic protective layer with a thickness of 60nm is formed, and hollow coated glass is obtained.
[0025] Comparative Example 1 differs from Example 1 in that: molybdenum hexacarbonyl and neodymium pentachloride hexahydrate are removed in step S2.1, while the remaining steps remain unchanged.
[0026] Comparative Example 2 differs from Example 1 in that the hexacarbonyl molybdenum in step S2.1 is removed, while the remaining steps remain unchanged.
[0027] Comparative Example 3 differs from Example 1 in that neodymium pentahydrate in step S2.1 is removed, while the remaining steps remain unchanged.
[0028] Comparative Example 4 differs from Example 1 in that steps S1.2-1.4 and S3 are removed, while the remaining steps remain unchanged. Specifically, a neodymium-molybdenum co-doped tin dioxide coating and a hydrophobic protective layer are directly prepared on the surface of the pretreated glass substrate obtained in step S1.1.
[0029] Comparative Example 5 differs from Example 1 in that steps S1.2-1.4 are removed, while the remaining steps remain unchanged. Specifically, a neodymium-molybdenum co-doped tin dioxide coating, a yttrium-doped zinc oxide coating, and a hydrophobic protective layer are sequentially prepared on the surface of the pretreated glass substrate obtained in step S1.1.
[0030] Comparative Example 6 differs from Example 1 in that step S3 is removed, while the remaining steps remain unchanged, i.e., a hydrophobic protective layer is directly prepared on the surface of the neodymium-molybdenum co-doped tin dioxide coating.
[0031] Comparative Example 7 differs from Example 1 in that the modified sericite powder in step S5.1 is replaced with an equal amount of modified talc powder.
[0032] Comparative Example 8 differs from Example 1 in that the modified talc powder in step S5.1 is replaced with an equal amount of modified sericite powder.
[0033] Test example: Test 1: The emissivity of the hollow coated glass prepared in Examples 1-3 and Comparative Examples 1-3 was tested using an emissivity meter. Each group was tested three times, and the average value was taken. The results are shown in Table 1.
[0034] Table 1: Emissivity Test Results of Coated Insulating Glass emissivity Example 1 0.18 Example 2 0.16 Example 3 0.15 Comparative Example 1 0.52 Comparative Example 2 0.38 Comparative Example 3 0.33 As shown in Table 1, the emissivity of the hollow coated glass prepared in Comparative Example 1 after removing molybdenum hexacarbonyl and neodymium pentachloride hexahydrate was significantly higher than that in Example 1. In Comparative Examples 2 and 3, when only neodymium pentachloride hexahydrate or molybdenum hexacarbonyl was added, the emissivity of the hollow coated glass was lower than that in Comparative Example 1, but still higher than that in Example 1. It can be seen that by first dissolving tin tetrachloride pentahydrate, then adding molybdenum hexacarbonyl and neodymium pentachloride hexahydrate, stirring and dissolving thoroughly to prepare a precursor sol, and then uniformly coating it on the surface of the yttrium-doped zinc oxide coating of a single-layer coated glass, and calcining to form a neodymium-molybdenum co-doped tin dioxide coating, the emissivity of the hollow coated glass can be effectively reduced.
[0035] Test 2: Using a cross-cutting tool, a 1mm × 1mm grid (100 grids) was cut into the surface of the neodymium molybdenum co-doped tin dioxide coating prepared in Examples 1-3 and Comparative Example 4, penetrating the coating to the glass substrate. Adhesive tape was then applied, pressed firmly, and quickly peeled off. This process was repeated 10 times, and the number of grids where the coating eventually detached was recorded. The grid detachment rate was calculated using the following formula: The grid detachment rate is calculated as (number of detached grids / total number of grids) × 100%. Each group was tested three times, and the average value was taken. The results are shown in Table 2.
[0036] Table 2: Test results of mesh peeling rate of neodymium molybdenum co-doped tin dioxide coating Mesh shedding rate (%) Example 1 4 Example 2 2 Example 3 2 Comparative Example 4 15 As shown in Table 2, in Comparative Example 4, after removing the yttrium-doped zinc oxide coating between the insulating glass substrate and the NdMo co-doped tin dioxide coating, the mesh shedding rate of the resulting NdMo co-doped tin dioxide coating was significantly higher than that in Example 1. This demonstrates that by preparing yttrium-doped zinc oxide coatings before and after the preparation of the NdMo co-doped tin dioxide coating, forming a yttrium-doped zinc oxide coating-NdMo co-doped tin dioxide coating-yttrium-doped zinc oxide coating structure, the adhesion between the NdMo co-doped tin dioxide coating and the insulating glass substrate can be effectively improved.
[0037] Test 3: Using a UV-Vis-NIR spectrophotometer, the average visible light transmittance of the hollow coated glass prepared in Examples 1-3 and Comparative Examples 4-6 was tested in the wavelength range of 400-760nm. Each group was tested three times, and the average value was taken. The results are shown in Table 3.
[0038] Table 3: Test Results of Visible Light Transmittance of Coated Insulating Glass Visible light transmittance (%) Example 1 83.7 Example 2 84.2 Example 3 84.4 Comparative Example 4 72.1 Comparative Example 5 78.4 Comparative Example 6 76.8 As shown in Table 3, in Comparative Example 4, after removing the yttrium-doped zinc oxide coatings on both sides of the neodymium-molybdenum co-doped tin dioxide coating, the visible light transmittance of the hollow coated glass was much lower than that of Example 1. In Comparative Examples 5 and 6, only a layer of yttrium-doped zinc oxide coating was prepared on the surface of the neodymium-molybdenum co-doped tin dioxide coating, and the visible light transmittance of the hollow coated glass was lower than that of Example 1. It can be seen that the structure of yttrium-doped zinc oxide coating-neodymium-molybdenum co-doped tin dioxide coating-yttrium-doped zinc oxide coating can increase the visible light transmittance.
[0039] Test 4: The water contact angle of the hydrophobic protective layer of the hollow coated glass prepared in Examples 1-3 and Comparative Examples 7-8 was measured using a contact angle meter. Each group was tested three times, and the average value was taken. Then, the hollow coated glass prepared in Examples 1-3 and Comparative Examples 7-8 was continuously irradiated with a UV lamp for 500 hours using an accelerated UV aging test chamber. After removal, the water contact angle of the hydrophobic protective layer was measured again, and the hydrophobicity retention rate was calculated using the following formula: Hydrophobicity retention rate = water contact angle after aging / water contact angle before aging × 100%. Each group was tested three times and the average value was taken. The results are shown in Table 4.
[0040] Table 4: Water contact angle test results of hydrophobic protective layer of insulated coated glass before and after UV aging Water contact angle before aging (°) Hydrophobicity retention rate (%) Example 1 153 94.2 Example 2 155 94.5 Example 3 158 95.1 Comparative Example 7 138 80.3 Comparative Example 8 142 85.6 As shown in Table 4, in Comparative Examples 7 and 8, when only one modified talc powder or one modified sericite powder was added, the water contact angle of the hydrophobic protective layer was lower than that of Example 1, and the hydrophobic retention rate after UV aging was also lower than that of Example 1. It can be seen that by coating modified sericite with nano-alumina, then coating modified talc with nano-silica, dispersing the modified sericite powder and modified talc powder in anhydrous ethanol, adding hexadecyltrimethoxysilane to make a suspension, and then adding it to a crosslinking liquid prepared with methyltriethoxysilane as a raw material to make a hydrophobic coating, and coating it on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass to form a hydrophobic protective layer, the modified sericite powder and modified talc powder can synergistically improve the self-cleaning performance and UV aging resistance of the hydrophobic protective coating.
[0041] It should be understood that those skilled in the art can make improvements or modifications based on the above description, and all such improvements and modifications should fall within the protection scope of the appended claims. Parts not described in detail in this specification are prior art known to those skilled in the art.
Claims
1. A manufacturing process for self-cleaning, low-emissivity insulated coated glass, characterized in that, Includes the following steps: S1: Preparation of single-layer coated glass Yttrium-doped zinc oxide powder was prepared using zinc oxide and yttrium oxide as raw materials, and then yttrium-doped zinc oxide target material was prepared by cold pressing and sintering. The yttrium-doped zinc oxide target material was then magnetron sputtered onto the outer surface of the pretreated insulating glass substrate to form a yttrium-doped zinc oxide coating, thus obtaining a single-layer coated glass. S2: Preparation of double-layer coated glass S2.1: Add tin tetrachloride pentahydrate to ethylene glycol at a ratio of 1g:(15-20)mL. Under nitrogen protection, heat and stir at 180-200℃ for 50-60min. When the temperature drops to 100℃, add molybdenum hexacarbonyl and neodymium pentahydrate. Continue stirring for 30-40min, cool to room temperature, add anhydrous ethanol for dilution, and ultrasonically disperse for 10-20min to obtain the precursor sol. S2.2: The above-mentioned precursor sol is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the above-mentioned single-layer coated glass. After drying for 30-40 minutes, it is placed in a muffle furnace and calcined at 400-500℃ for 2-3 hours to form a neodymium-molybdenum co-doped tin dioxide coating with a thickness of 60-80 nm, thus obtaining a double-layer coated glass. S3: Preparation of three-layer coated glass On the surface of the neodymium-molybdenum co-doped tin dioxide coating of the above-mentioned double-layer coated glass, the above-mentioned yttrium-doped zinc oxide target is used as the magnetron sputtering target. Magnetron sputtering is performed for 120-130s at an argon flow rate of 20-30 sccm, an oxygen flow rate of 2-4 sccm, 110-120W, 0.5Pa and 130-150℃. After cooling, the glass is annealed at 200-250℃ for 20-30min to form a yttrium-doped zinc oxide coating, thus obtaining a three-layer coated glass. S4: Preparation of modified sericite powder and modified talc powder First, aluminum isopropoxide is used as a raw material to prepare alumina sol. Then, sericite is activated and dispersed in deionized water. Alumina sol is added and mixed thoroughly to prepare modified sericite powder. Then, tetraethyl orthosilicate is used as a raw material to prepare silica sol. Activated talc is added and mixed thoroughly to prepare modified talc powder. S5: Preparation of Insulating Coated Glass The modified sericite powder and modified talc powder were dispersed in anhydrous ethanol to form a suspension. Then, methyltriethoxysilane was dissolved in anhydrous ethanol, and hydrochloric acid and ammonia were added in sequence to form a crosslinking liquid. The suspension was then added to the mixture to form a hydrophobic coating, which was then uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass to obtain hollow coated glass.
2. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 1, characterized in that, S1 includes the following steps: S1.1: The insulating glass substrate is ultrasonically cleaned with 75% ethanol solution and deionized water for 10-20 min in sequence, then dried with nitrogen gun, and then placed in magnetron sputtering vacuum chamber, and activated with argon gas at 80-100W plasma for 5-10 min to obtain pretreated glass substrate. S1.2: Dry zinc oxide powder and yttrium oxide powder at 110-120℃ for 2-3 hours, then add the dried zinc oxide powder and yttrium oxide powder to anhydrous ethanol at a ratio of (18-20) g: (0.5-0.6) g: (10-12) mL, ball mill at 200-300 rpm for 8-10 hours, and then heat and stir in a water bath at 80-90℃ until the ethanol is completely evaporated to obtain yttrium-doped zinc oxide powder; S1.3: Pass the above yttrium-doped zinc oxide powder through a 200-mesh sieve, then fill it evenly into a mold, cold press it at 200 MPa for 3-5 min, then place it in a muffle furnace, heat it to 500-600℃ at 5℃ / min in an oxygen atmosphere, hold it for 2-3 h, then continue to heat it to 1250-1300℃ at 3℃ / min, hold it for sintering for 2-3 h, and cool it to room temperature with the furnace to obtain the yttrium-doped zinc oxide target. S1.4: On the outer surface of the pretreated glass substrate, using the yttrium-doped zinc oxide target as the magnetron sputtering target, magnetron sputtering is performed for 120-130 seconds at an argon flow rate of 20-30 sccm, an oxygen flow rate of 2-4 sccm, a W of 110-120, a Pa of 0.5, and a temperature of 130-150°C. After cooling, the substrate is annealed at 200-250°C for 20-30 minutes to form a yttrium-doped zinc oxide coating, thus obtaining a single-layer coated glass.
3. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 2, characterized in that, S4 includes the following steps: S4.1: Dissolve aluminum isopropoxide in anhydrous ethanol at a ratio of 1g:(2-4)mL, stir thoroughly until a transparent solution is formed, then add 26-28% of the volume of deionized water while stirring, continue stirring for 30-40min, add octadecyltrimethylammonium bromide, stir to dissolve, add citric acid to adjust the pH to 5-5.5, and then continue stirring to mature for 2-3h to obtain alumina sol; S4.2: Add sericite and anhydrous ethanol to deionized water at a ratio of (2.8-3) g: 1 mL: 1 mL, stir and mix for 10-20 min, then heat and stir at 45-55℃ for 2-3 h, cool, filter, wash with deionized water 2-3 times and dry to obtain activated sericite powder. S4.3: Add the above activated sericite powder to deionized water at a ratio of (3-4) g: 1 mL, and ultrasonically disperse for 10-20 min to obtain an activated sericite dispersion. Then, while stirring, add the above alumina sol and stir at 45-50℃ for 2-3 h. Then, ultrasonically treat for 20-30 min. After cooling, filter, vacuum dry, grind and sieve to obtain modified sericite powder. S4.4: Add talc powder to a hydrochloric acid solution with a pH of 3-4 at a ratio of (1.7-1.8) g: 1 mL, heat and stir at 45-50℃ for 1-2 h, cool, filter, wash three times with deionized water and dry to obtain activated talc powder; S4.5: Add tetraethyl orthosilicate to anhydrous ethanol at a ratio of 1g:(3.4-3.5)mL, stir thoroughly to dissolve, then add 10% deionized water (by volume of anhydrous ethanol) and 0.6-0.8% hydrochloric acid (by volume of anhydrous ethanol) at a concentration of 12mol / L. Continue stirring for 1-2 hours, then add polyethylene glycol 6000 and continue stirring for 2-3 hours to obtain silica sol. S4.6: Add the activated talc powder to the silica sol at a ratio of 1g:(1.3-1.5)mL, add 8-10% of the silica sol volume of deionized water and stir to form a suspension. Then heat and stir at 35-45℃ for 3-4h, then sonicate for 20-30min. After cooling, filter, vacuum dry, grind and sieve to obtain modified talc powder.
4. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 3, characterized in that, S5 includes the following steps: S5.1: Disperse the modified sericite powder obtained in step S4.3 and the modified talc powder obtained in step S4.6 in anhydrous ethanol at a mass ratio of 1:(3-5):(20-30), add hexadecyltrimethoxysilane, and stir for 1-2 hours to obtain a suspension. S5.2: Add methyltriethoxysilane to anhydrous ethanol at a volume ratio of 1:(8-10), stir and mix thoroughly, then add hydrochloric acid with a concentration of 0.01mol / L and an equal volume to methyltriethoxysilane, and stir and react for 1-2 hours. Then add ammonia water with a mass fraction of 28%, and continue stirring and reacting for 30-40 minutes. After standing for 8-10 hours, a crosslinking liquid is obtained. Then add the above suspension, stir and mix thoroughly to obtain a hydrophobic coating. S5.3: The above-mentioned hydrophobic coating is uniformly coated on the surface of the yttrium-doped zinc oxide coating of the three-layer coated glass prepared in step S3. After drying and curing, a hydrophobic protective layer with a thickness of 50-60nm is formed, and hollow coated glass is obtained.
5. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 1, characterized in that, The amount of molybdenum hexacarbonyl added is 6-8% of the mass of tin tetrachloride pentahydrate, and the amount of neodymium pentahydrate added is 5-6% of the mass of tin tetrachloride pentahydrate.
6. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 3, characterized in that, The amount of octadecyltrimethylammonium bromide added was 0.1% of the mass of aluminum isopropoxide, and the volume ratio of alumina sol to activated sericite dispersion was (2.5-3):
1.
7. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 3, characterized in that, The amount of polyethylene glycol 6000 added is 1.7-1.8% of the mass of tetraethyl orthosilicate.
8. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 3, characterized in that, Both sericite and talc have a particle size of 4-6 μm.
9. The preparation process of a self-cleaning, low-emissivity insulated coated glass according to claim 4, characterized in that, The amount of hexadecyltrimethoxysilane added is 25% of the total mass of modified sericite powder and modified talc powder, the amount of ammonia added is 15-20% of the volume of methyltriethoxysilane, and the amount of suspension added is 28-32% of the volume of crosslinking liquid.
10. A self-cleaning, low-emissivity insulated coated glass, characterized in that, It is prepared by the preparation process of a self-cleaning low-emissivity hollow coated glass as described in any one of claims 1-9.