A curing process for coated tempered glass

Abstract

The present application relates to the technical field of glass surface treatment, and particularly relates to a solidification process for coated tempered glass after coating, which comprises placing the first coated glass on an inlet conveying roller of a coating solidification furnace, solidifying the first coated glass in the coating solidification furnace, obtaining a coated glass after the solidification, placing the second coated glass on an inlet conveying roller of a second coating solidification furnace, the second coating solidification furnace being the same as the first coating solidification furnace except for the temperature, and obtaining the coated tempered glass after the solidification after the second coated glass leaves the second coating solidification furnace. The present application introduces epoxy group, amino group and perfluoroalkyl polyfunctional silane into the modified coating solution, so that the hydrolysis crosslinking sites are more and the reaction activity is higher, the condensation solidification can be quickly completed in the low-temperature section, the overall solidification rate is significantly improved, the residence time of the glass in the high-temperature zone is reduced, the warping risk is reduced from the source, the solid content of the coating solution is moderate, and the content of organic solvent is low.

Description

Technical Field

[0001] This invention relates to the field of glass surface treatment technology, and in particular to a curing process for coated tempered glass after coating. Background Technology

[0002] In the field of glass deep processing, coated tempered glass has been widely used in photovoltaic panels, electronic panels, appliance covers, automotive glass, building curtain walls and other scenarios due to its advantages such as high hardness, scratch resistance, hydrophobicity and stain resistance, and stable optical performance. In order to ensure the adhesion, density and durability of the film layer, constant temperature curing treatment is usually required after coating to allow the coating solution to fully cross-link and form a film.

[0003] Conventional curing processes often employ a single high-temperature curing mode or a stepped heating mode. However, the temperature range of stepped heating is relatively large, which easily leads to uneven heating of the glass. The shrinkage of the cured film and the thermal expansion of the glass are not coordinated, resulting in significant warping and failing to meet the requirements for ultra-thin glass applications. Ordinary silicon-based coating solutions have insufficient cross-linking and low hydrophobic group grafting rates, requiring longer high-temperature curing times, resulting in low production efficiency, high energy consumption, and prolonged high temperatures exacerbating glass warping and deformation. Therefore, to address the problems described above, this invention proposes a curing process for coated tempered glass after coating. Summary of the Invention

[0004] The purpose of this invention is to provide a curing process for coated tempered glass to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a curing process for coated tempered glass, applicable to tempered glass with a thickness of 1.6-2.5 mm, wherein the surface of the tempered glass is coated with a base film and a surface film, wherein the base film formed after the first coating and curing has a silicon dioxide content ≥90.0% and a thickness of 70-90 nm, a modified coating solution is coated on the base film, and a surface film is formed after a second coating and curing, with a thickness of 110-130 nm, characterized in that the curing process includes the following steps:

[0006] S1. Place the first coated glass after the coating process on the conveyor roller conveyor at the entrance of the coating curing furnace, adjust the position of the first coated glass to center it, and set the conveyor speed to 1.9-2.0m / min;

[0007] S2. The first-coated glass is cured in a first-coating curing oven, which is 12m long and divided into 6 sections. Each section is 2m long and has an effective inner wall width of 1.6m. Each section is independently temperature controlled and uses PID control mode. After curing, the first-coated glass is obtained.

[0008] The temperature settings for each segment are as follows:

[0009] The temperature in sections 1-2 is 60-70℃;

[0010] The temperature in sections 3-4 is 70-80℃;

[0011] The temperature of sections 5-6 is 80-90℃, and after curing, a glass-coated layer is obtained;

[0012] S3. Apply the modified coating solution to the surface of the first-coated glass using the same coating process to obtain the second-coated glass. Place the second-coated glass on the conveyor rollers at the inlet of the second-coating curing furnace. Except for the temperature, all other parameters of the second-coating curing furnace are the same as those of the first-coating curing furnace. The temperature settings for each section in the second-coating curing furnace are as follows:

[0013] The temperature for sections 1-3 is 180-200℃;

[0014] The temperature for sections 4-6 is 200-220℃;

[0015] S4. After the second-coated glass leaves the second-coating curing oven, it becomes second-coated glass and then enters the cooling section. It is cooled to 35-40℃ by air cooling. After cooling and passing the inspection, the cured coated tempered glass is obtained.

[0016] As a preferred technical solution of the present invention, the coating process in step S1 adopts a roller coating method, the roller material is polyurethane, the roller speed is set to 10-14m / min, the coating speed is set to 11-15m / min, the liquid is automatically added by a peristaltic pump, and the coating temperature is set to 30-36℃.

[0017] As a preferred technical solution of the present invention, the heating method of the plating curing furnace in step S2 is to use far-infrared heating tubes. The far-infrared heating tubes are made of quartz glass with ceramic heads and are evenly arranged in the furnace. The far-infrared heating tubes heat up to the set temperature at 14-16℃ / min, and the temperature control method is digital display control.

[0018] As a preferred technical solution of the present invention, the plating curing furnace is divided into an inner layer, an inner insulation layer and an outer layer. The inner layer is made of mirror stainless steel plate. The upper and side thickness of the inner insulation layer is 150-160mm, and the lower thickness is 100-110mm. The insulation material is rock wool board. The outer layer is made of powder-coated carbon steel plate.

[0019] As a preferred embodiment of the present invention, the rollers of the conveyor roller track in the plating curing furnace are made of ceramic roller material, the distance between the rollers is 195-205mm, and the roller runout is set to 0.01-0.03mm.

[0020] The roller is driven by a variable frequency motor reducer that drives the transmission shaft through a sprocket and chain. The transmission shaft then drives the ceramic roller to rotate through a double polyurethane transmission belt.

[0021] As a preferred embodiment of the present invention, a circulating fan is installed at the top of each section of the plating and curing furnace to circulate and heat the air, creating turbulence in the furnace. The start and stop of the circulating fan are linked to the heater in the corresponding furnace section. When the heater is working, the circulating fan starts simultaneously, and its speed is adjusted by PID according to the difference between the furnace temperature and the set temperature. The PID adjustment calculates a control output (such as heating power or fan speed) by measuring the deviation between the current value (such as the furnace temperature) and the target set value in real time, according to the proportional, integral, and derivative components, so that the controlled variable follows the set value quickly, stably, and without steady-state error.

[0022] Each section of the plating and curing oven is equipped with a centrifugal exhaust fan at the top. The fan is controlled by a timer to start and stop, and the duration and interval of the exhaust are adjusted to discharge the volatile organic compounds from the oven.

[0023] The inner wall of the upper furnace body of each section of the plating and curing furnace gradually narrows from the middle towards the exhaust port, and the cross-section is inverted funnel shape.

[0024] As a preferred embodiment of the present invention, the modified coating solution is prepared by the following steps:

[0025] S101. Mix anhydrous ethanol, deionized water, and dilute hydrochloric acid evenly to prepare an acidic alcohol-water solution.

[0026] S102. Add the modified solution dropwise to the acidic alcoholic aqueous solution at a rate of 3-4 mL / min. After the addition is complete, stir at room temperature for 1-2 h. Then, heat to 40-45℃ under sealed conditions and stir for 20-24 h to obtain the sol.

[0027] S103. Cool the sol to room temperature, dilute it with anhydrous ethanol to a solid content of 4-5 wt%, and filter it through a 0.4-0.5 μm polytetrafluoroethylene filter membrane to obtain the modified coating solution.

[0028] As a preferred embodiment of the present invention, the modified solution in step S102 is prepared through the following steps:

[0029] S1021. Ethyl silicate, perfluorodecyltrimethoxysilane, γ-glycidoxypropyltrimethoxysilane, and γ-aminopropyltriethoxysilane are sequentially added to anhydrous ethanol and stirred for 5-8 min to obtain a homogeneous mixture. Acetylacetone is then added dropwise to the homogeneous mixture while stirring, and stirring is continued for 5-8 min to obtain a transparent silane mixture.

[0030] S1022. Premix deionized water and glacial acetic acid to prepare an acid-water solution. Add the acid-water solution dropwise to the transparent silane mixture at a rate of 10-15 mL / min while stirring, until the addition is complete, and then stir for 30-35 min.

[0031] S1023. After stopping stirring, seal and let stand for 1-1.5 hours to obtain a clear modified solution.

[0032] As a preferred embodiment of the present invention, the mass ratio of anhydrous ethanol, deionized water and dilute hydrochloric acid in step S101 is 100:(8-12):(0.8-1.2).

[0033] In step S102, the mass ratio of the acidic alcohol aqueous solution to the modified solution is 100:(25-35).

[0034] As a preferred embodiment of the present invention, in step S1021, the mass ratio of ethyl silicate, perfluorodecyltrimethoxysilane, γ-glycidyl etheroxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, anhydrous ethanol, and acetylacetone is 100:(8-12):(5-9):(3-7):(200-300):(4-8).

[0035] In step S1022, the mass ratio of deionized water to glacial acetic acid is 100:(1.5-2.5).

[0036] In step S1022, the mass ratio of the acid aqueous solution to the transparent silane mixture is 1:(3-4.5).

[0037] Compared with the prior art, the beneficial effects of the present invention are:

[0038] 1. This invention introduces epoxy, amino, and perfluoroalkyl polyfunctional silanes into the modified coating solution, resulting in more hydrolysis crosslinking sites and higher reactivity. This allows for rapid condensation curing in the medium- and low-temperature range, significantly improving the overall curing rate and reducing the time the glass spends in the high-temperature zone. This reduces the risk of warping from the source and provides dense support for the underlying high-purity silica. The surface film itself possesses both rigidity and flexibility, acting as a stress buffer. After curing, the film layer has a more matching elastic modulus with the tempered glass, making it less prone to warping due to shrinkage differences during high-temperature cooling. The coating solution has a moderate solid content and low organic solvent content, resulting in low volatile gas emissions and stable release during curing. Combined with the furnace exhaust design, it prevents film defects caused by localized solvent boiling, resulting in high film uniformity.

[0039] 2. This invention employs a two-stage stepped curing process combining a first-stage curing oven and a second-stage curing oven. The first-stage curing oven pre-cures the bottom film at a low temperature, while the second-stage curing oven rapidly cross-links the surface film at a high temperature. This allows the glass to experience a gentle temperature gradient during the curing process, avoiding the accumulation of thermal stress caused by sudden temperature increases or prolonged high-temperature exposure. Simultaneously, a centrifugal exhaust fan periodically discharges volatile organic compounds, and the inverted funnel-shaped inner wall structure prevents localized solvent boiling that could lead to film defects. Attached Figure Description

[0040] Figure 1 This is a schematic diagram of the curing process in this invention;

[0041] Figure 2 This is a schematic diagram of the preparation process of the modified coating solution in this invention;

[0042] Figure 3 This is a schematic diagram of the preparation process of the modified solution in this invention. Detailed Implementation

[0043] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0044] Please see Figures 1-3 This invention provides a technical solution for the curing process of coated tempered glass:

[0045] Example 1:

[0046] A curing process for coated tempered glass includes the following steps:

[0047] S1. Place the first coated glass, after the coating process, on the conveyor roller conveyor at the entrance of the coating curing oven. The coating process adopts the roller coating method. The rubber roller material is polyurethane. The rubber roller speed is set to 10m / min, the coating speed is set to 11m / min, the liquid is automatically added by the peristaltic pump, the coating temperature is set to 30℃, the distance between the rollers is 195mm, the roller runout is set to 0.01mm, adjust the position of the first coated glass to center it, and set the conveyor speed to 1.9m / min.

[0048] S2. The first-coated glass is cured in a curing oven, which is 12m long and divided into 6 sections. Each section is 2m long and has an effective inner wall width of 1.6m. The upper and side insulation layers are 150mm thick, and the lower layer is 100mm thick. The insulation material is rock wool board, and the outer layer is powder-coated carbon steel plate. Each section is independently temperature controlled using PID control mode. Far-infrared heating tubes are used to raise the temperature at a rate of 14℃ / min. The temperature of sections 1-2 is 60℃, the temperature of sections 3-4 is 70℃, and the temperature of sections 5-6 is 80℃. After curing, the first-coated glass is obtained, which is the bottom film. The thickness of the bottom film is 70nm.

[0049] S3. Apply the modified coating solution to the surface of the first-coated glass using the same coating process to obtain the second-coated glass. Place the second-coated glass on the conveyor roller at the entrance of the second-coating curing furnace. Except for the temperature, all other parameters of the second-coating curing furnace are the same as those of the first-coating curing furnace. The temperature of the first to third sections of the second-coating curing furnace is 180℃, and the temperature of the fourth to sixth sections is 200℃.

[0050] S4. After the second-coated glass leaves the second-coating curing oven, the second-coated glass is obtained. The second coating is the surface film with a thickness of 110nm. It enters the cooling section and is cooled to 35℃ by forced air cooling with an axial flow fan. After cooling, it passes the inspection and obtains the cured coated tempered glass.

[0051] The modified coating solution is prepared through the following steps:

[0052] I. Preparation of modified solution:

[0053] S1021. Weigh 100g of ethyl silicate, 8g of perfluorodecyltrimethoxysilane, 5g of γ-glycidoxypropyltrimethoxysilane, and 3g of γ-aminopropyltriethoxysilane, add them to 200g of anhydrous ethanol, mix and stir for 5min to obtain a homogeneous mixture; add 4g of acetylacetone dropwise while stirring, and continue stirring for 5min to obtain a transparent silane mixture.

[0054] S1022. Weigh 100g of deionized water and 1.5g of glacial acetic acid, mix them evenly to prepare an acid-water solution, and add 100g of the acid-water solution dropwise to 300g of transparent silane mixture at a rate of 10mL / min while stirring, until the solution is completely added and then continue stirring for 30min.

[0055] S1023. After stopping stirring, seal and let stand for 1 hour to obtain a clear modified solution.

[0056] II. Preparation of Modified Coating Solution:

[0057] S101. Weigh 100g of anhydrous ethanol, 8g of deionized water, and 0.8g of 1% dilute hydrochloric acid, and mix them evenly to prepare an acidic alcohol-water solution.

[0058] S102. Take 25g of the modified solution and add it dropwise to 100g of acidic alcoholic aqueous solution at a rate of 3mL / min. After the addition is complete, stir at room temperature for 1h. Seal and heat to 40℃, keep warm and stir for 20h to obtain a sol.

[0059] S103. Cool the sol to room temperature, dilute it with anhydrous ethanol to a solid content of 4wt%, and filter it through a 0.4μm polytetrafluoroethylene filter membrane to obtain the modified coating solution.

[0060] Example 2:

[0061] A curing process for coated tempered glass includes the following steps:

[0062] S1. Place the first coated glass, after the coating process, on the conveyor roller conveyor at the entrance of the coating curing furnace. The coating process adopts the roller coating method. The rubber roller material is polyurethane. The rubber roller speed is set to 12m / min, the coating speed is set to 13m / min, the liquid is automatically added by the peristaltic pump, the coating temperature is set to 33℃, the distance between the rollers is 200mm, the roller runout is set to 0.02mm, adjust the position of the first coated glass to center it, and set the conveyor speed to 1.95m / min.

[0063] S2. The first-coated glass is cured in a curing oven, which is 12m long and divided into 6 sections. Each section is 2m long and has an effective inner wall width of 1.6m. The upper and side insulation layers are 155mm thick, and the lower layer is 105mm thick. The insulation material is rock wool board, and the outer layer is powder-coated carbon steel plate. Each section is independently temperature controlled using PID control mode. Far-infrared heating tubes are used to raise the temperature at a rate of 15℃ / min. The temperature of sections 1-2 is 65℃, the temperature of sections 3-4 is 75℃, and the temperature of sections 5-6 is 85℃. After curing, a first-coated glass is obtained, which is the bottom film. The thickness of the bottom film is 80nm.

[0064] S3. Apply the modified coating solution to the surface of the first-coated glass using the same coating process to obtain the second-coated glass. Place the second-coated glass on the conveyor roller at the entrance of the second-coating curing furnace. Except for the temperature, all other parameters of the second-coating curing furnace are the same as those of the first-coating curing furnace. The temperature of the first to third sections of the second-coating curing furnace is 190℃, and the temperature of the fourth to sixth sections is 210℃.

[0065] S4. After the second-coated glass leaves the second-coating curing oven, the second-coated glass is obtained. The second coating is the surface film with a thickness of 120nm. It enters the cooling section and is cooled to 38℃ by forced air cooling with an axial flow fan. After cooling, it passes the inspection and obtains the cured coated tempered glass.

[0066] The modified coating solution is prepared through the following steps:

[0067] I. Preparation of modified solution:

[0068] S1021. Weigh 100g of ethyl silicate, 10g of perfluorodecyltrimethoxysilane, 7g of γ-glycidoxypropyltrimethoxysilane, and 5g of γ-aminopropyltriethoxysilane. Add 250g of anhydrous ethanol and mix for 6 minutes to obtain a homogeneous mixture. Add 6g of acetylacetone dropwise while stirring, and continue stirring for 6 minutes to obtain a transparent silane mixture.

[0069] S1022. Weigh 100g of deionized water and 2g of glacial acetic acid, mix them evenly to prepare an acid-water solution, and add 100g of the acid-water solution dropwise to 370g of transparent silane mixture at a rate of 13mL / min while stirring, until the solution is completely added, and then continue stirring for 33min.

[0070] S1023. After stopping stirring, seal and let stand for 1.3 hours to obtain a clear modified solution.

[0071] II. Preparation of Modified Coating Solution:

[0072] S101. Weigh 100g of anhydrous ethanol, 10g of deionized water, and 1g of 1% dilute hydrochloric acid, and mix them evenly to prepare an acidic alcohol-water solution.

[0073] S102. Take 30g of the modified solution and add it dropwise to 100g of acidic alcohol aqueous solution at a rate of 3.5mL / min. After the addition is complete, stir at room temperature for 1.5h. Seal and heat to 43℃, keep warm and stir for 22h to obtain the sol.

[0074] S103. Cool the sol to room temperature, dilute it with anhydrous ethanol to a solid content of 4.5 wt%, and filter it through a 0.45 μm polytetrafluoroethylene filter membrane to obtain the modified coating solution.

[0075] Example 3:

[0076] A curing process for coated tempered glass includes the following steps:

[0077] S1. Place the first-coated glass, after the coating process, on the conveyor roller conveyor at the entrance of the coating curing oven. The coating process adopts the roller coating method. The rubber roller material is polyurethane. The rubber roller speed is set to 14m / min, the coating speed is set to 15m / min, the liquid is automatically added by the peristaltic pump, the coating temperature is set to 36℃, the distance between the rollers is 205mm, the roller runout is set to 0.03mm, adjust the position of the first-coated glass to center it, and set the conveyor speed to 2.0m / min.

[0078] S2. The first-coated glass is cured in a curing oven, which is 12m long and divided into 6 sections. Each section is 2m long and has an effective inner wall width of 1.6m. The upper and side insulation layers are 160mm thick, and the lower layer is 110mm thick. The insulation material is rock wool board, and the outer layer is powder-coated carbon steel plate. Each section is independently temperature controlled using PID control mode. Far-infrared heating tubes are used to raise the temperature at a rate of 16℃ / min. The temperature of sections 1-2 is 70℃, the temperature of sections 3-4 is 80℃, and the temperature of sections 5-6 is 90℃. After curing, a first-coated glass is obtained, which is the bottom film. The bottom film thickness is 90nm.

[0079] S3. Apply the modified coating solution to the surface of the first-coated glass using the same coating process to obtain the second-coated glass. Place the second-coated glass on the conveyor roller at the entrance of the second-coating curing furnace. Except for the temperature, all other parameters of the second-coating curing furnace are the same as those of the first-coating curing furnace. The temperature of the first to third sections of the second-coating curing furnace is 200℃, and the temperature of the fourth to sixth sections is 220℃.

[0080] S4. After the second-coated glass leaves the second-coating curing oven, the second-coated glass is obtained. The second coating is the surface film with a thickness of 130nm. It enters the cooling section and is cooled to 40℃ by forced air cooling with an axial flow fan. After cooling, it passes the inspection and obtains the cured coated tempered glass.

[0081] The modified coating solution is prepared through the following steps:

[0082] I. Preparation of modified solution:

[0083] S1021. Weigh 100g of ethyl silicate, 12g of perfluorodecyltrimethoxysilane, 9g of γ-glycidoxypropyltrimethoxysilane, and 7g of γ-aminopropyltriethoxysilane. Add 300g of anhydrous ethanol and mix for 8 minutes to obtain a homogeneous mixture. Add 8g of acetylacetone dropwise while stirring, and continue stirring for 8 minutes to obtain a transparent silane mixture.

[0084] S1022. Weigh 100g of deionized water and 2.5g of glacial acetic acid, mix them evenly to prepare an acid-water solution, and add 100g of the acid-water solution dropwise to 450g of transparent silane mixture at a rate of 15mL / min while stirring, until the solution is completely added, and then continue stirring for 35min.

[0085] S1023. After stopping stirring, seal and let stand for 1.5 hours to obtain a clear modified solution.

[0086] II. Preparation of Modified Coating Solution:

[0087] S101. Weigh 100g of anhydrous ethanol, 12g of deionized water, and 1.2g of 1% dilute hydrochloric acid, and mix them evenly to prepare an acidic alcohol-water solution.

[0088] S102. Take 35g of the modified solution and add it dropwise to 100g of acidic alcoholic aqueous solution at a rate of 4mL / min. After the addition is complete, stir at room temperature for 2h. Seal and heat to 45℃, keep warm and stir for 24h to obtain the sol.

[0089] S103. Cool the sol to room temperature, dilute it with anhydrous ethanol to a solid content of 5wt%, and filter it through a 0.5μm polytetrafluoroethylene filter membrane to obtain the modified coating solution.

[0090] Comparative Example 1:

[0091] Compared to Example 1, Comparative Example 1 sets the temperature of sections 1-6 of the two-coating curing oven to 180°C, while the remaining steps are exactly the same as in Example 1.

[0092] Comparative Example 2:

[0093] Comparative Example 2 differs from Example 1 in that the modified solution is replaced with an equal mass of γ-glycidoxypropyltrimethoxysilane solution, while the remaining steps are exactly the same as in Example 1.

[0094] Comparative Example 3:

[0095] Comparative Example 3 differs from Example 1 in that the modified coating solution was replaced with an equal mass of a conventional commercially available SiO2 coating solution (model X-40-2182), and the remaining steps were exactly the same as in Example 1.

[0096] Based on the curing process of coated tempered glass provided by the present invention, the modified coating solutions prepared in Examples 1-3 and Comparative Examples 1-3 and the cured coated tempered glass were subjected to the following performance tests, with a focus on curing rate, warpage of coated tempered glass and film stability.

[0097] I. Performance Testing of Modified Coating Solution:

[0098] Curing rate (thermo-curing kinetics):

[0099] The thermal curing behavior of the coating solution was tested by differential scanning calorimetry (DSC). 10 mg of the coating solution was placed in an aluminum crucible and heated from 30 °C to 300 °C at a rate of 10 °C / min under a nitrogen atmosphere. The onset temperature and peak temperature of the exothermic peak were recorded.

[0100] Evaluation indicators: curing initiation temperature (the lower the temperature, the stronger the low-temperature curing ability); curing peak temperature (reflecting the main cross-linking reaction range); apparent activation energy (calculated by Kissinger method, the lower the temperature, the faster the curing rate). The specific test results are shown in Table 1 below.

[0101] Table 1: Performance Test Table of Modified Coating Solution

[0102]

[0103] As can be seen from the data in Table 1, the introduction of the triple functional groups of perfluoroalkyl, epoxy, and amino in Examples 1-3 significantly reduced the curing reaction energy barrier of the coating solution. Among them, the amino group has a self-catalytic ring-opening effect on the epoxy group, which enables the crosslinking reaction to proceed rapidly in the medium and low temperature range. The fluorine segment enhances far-infrared absorption and assists in heat conduction. Due to the better silane ratio, Example 2 has the lowest curing start temperature (102℃), the lowest peak temperature (168℃), and the lowest activation energy (55 kJ / mol), and its curing rate is slightly better than that of Examples 2 and 3. Comparative Example 2 lacks fluorine and amino groups, and its crosslinking activity is greatly reduced. The commercially available product in Comparative Example 3 requires a higher temperature to cure, resulting in high energy consumption and low efficiency. Therefore, the modified coating solution of the present invention has outstanding low-temperature rapid curing capability.

[0104] II. Performance Testing of Coated Tempered Glass:

[0105] 1. Warpage of coated tempered glass (refer to GB / T33234-2016 "Test Method for Warpage of Photothermal Glass")

[0106] After the coating has been cured, the tempered glass is placed on a calibrated marble plate, and the maximum gap (in mm) between the four corners and the center point of the glass and the plate is measured using a feeler gauge or laser displacement sensor.

[0107] Warpage calculation formula:

[0108]

[0109] in, For the maximum gap, For minimum gap, The diagonal length of the glass is used. Five pieces of glass are tested in each group, and the average value is taken. The measurements are taken immediately after curing in the hot state and 24 hours after cooling to room temperature (cold state).

[0110] 2. Film stability:

[0111] 2.1 Adhesion (cross-cut test):

[0112] Referring to GB / T9286-2021, use a cross-cutting tool to draw 1mm×1mm squares (10×10) on the film surface, attach 3M 600 tape and then quickly peel it off to observe the area of ​​coating peeling.

[0113] 2.2 Resistance to damp heat aging:

[0114] According to GB / T1740-2007, the sample was placed in a constant temperature and humidity chamber (temperature 60℃, relative humidity 95%) and left for 500 hours before being taken out to test the adhesion and appearance changes.

[0115] 2.3 Acid / Alkali Resistance:

[0116] 5% H2SO4 and 5% NaOH solutions were dropped onto the surface of the membrane, respectively. The membrane was covered with a watch glass and washed after 24 hours. The results were observed to see if the membrane lost its gloss, changed color, or peeled off. The specific test results are shown in Table 2 below.

[0117] Table 2: Performance Test Table for Coated Tempered Glass

[0118]

[0119] As can be seen from the data in Table 2, the cold-state warpage of Examples 1-3 was only 0.09%-0.12%, the coating peeling area was 0, the adhesion grade was 0, and after 500 hours of humid heat, there was no blistering, loss of gloss, or peeling in appearance, and the acid and alkali resistance remained unchanged. Among them, Example 2 had the lowest warpage (0.09% in cold state), and its overall performance was slightly better than Examples 1 and 3. Comparative Example 1 (190℃ throughout) had a cold-state warpage of 0.19%, a coating peeling of 5%, an adhesion grade of 1, and slight loss of gloss after humid heat. Comparative Example 2 had a warpage of 0.13%, a peeling of 2%, an adhesion grade of 1, local blistering after humid heat, and slight peeling under alkaline solution. Comparative Example 3 had the most severe warpage (0.36%), a peeling of 15%, an adhesion grade of 2, obvious blistering and peeling after humid heat, and obvious acid and alkali corrosion.

[0120] This invention employs a stepped, mild curing process combined with a triple-modified coating solution, enabling the film layer to fully cross-link at low temperatures. This results in uniform heating and slow cooling of the glass, leading to low internal stress. Fluorosilane imparts a superhydrophobic and corrosion-resistant network, while epoxy-amino cross-linking enhances density and adhesion. In Example 2, the glass thickness was moderate and the temperature parameters were optimized, resulting in optimal warpage control. In Comparative Example 3, the commercially available coating solution required high-temperature, long-term curing, leading to severe glass warpage and film deterioration. Therefore, the process of this invention significantly improves the dimensional stability and film durability of coated tempered glass.

[0121] The above are merely specific embodiments of the present invention, but the technical features of the present invention are not limited thereto. Any simple changes, equivalent substitutions, or modifications made based on the present invention to solve essentially the same technical problems and achieve essentially the same technical effects are all covered within the protection scope of the present invention.

Claims

1. A curing process for coated tempered glass, applicable to tempered glass with a thickness of 1.6-2.5 mm, wherein the tempered glass surface is coated with a base film and a surface film, wherein the base film formed after the first coating and curing has a silicon dioxide content ≥90.0% and a thickness of 70-90 nm, a modified coating solution is coated on the base film, and a surface film is formed after a second coating and curing, the surface film having a thickness of 110-130 nm, characterized in that... The curing process includes the following steps: S1. Place the first coated glass after the coating process on the conveyor roller conveyor at the entrance of the coating curing furnace, adjust the position of the first coated glass to center it, and set the conveyor speed to 1.9-2.0m / min; S2. The first-coated glass is cured in a first-coating curing oven, which is 12m long and divided into 6 sections. Each section is 2m long and has an effective inner wall width of 1.6m. Each section is independently temperature controlled and uses PID control mode. After curing, the first-coated glass is obtained. The temperature settings for each segment are as follows: The temperature in sections 1-2 is 60-70℃; The temperature in sections 3-4 is 70-80℃; The temperature in sections 5 and 6 is 80-90℃; S3. Apply the modified coating solution to the surface of the first-coated glass using the same coating process to obtain the second-coated glass. Place the second-coated glass on the conveyor rollers at the inlet of the second-coating curing furnace. Except for the temperature, all other parameters of the second-coating curing furnace are the same as those of the first-coating curing furnace. The temperature settings for each section in the second-coating curing furnace are as follows: The temperature for sections 1-3 is 180-200℃; The temperature for sections 4-6 is 200-220℃; S4. After the second-coated glass leaves the second-coating curing furnace, it becomes second-coated glass and then enters the cooling section. It is cooled to 35-40℃ by air cooling. After cooling and passing the inspection, it undergoes a tempering process to obtain coated tempered glass.

2. The curing process for coated tempered glass according to claim 1, characterized in that: In step S1, the coating process adopts a roller coating method. The roller material is polyurethane, the roller speed is set to 10-14 m / min, the coating speed is set to 11-15 m / min, the liquid is automatically added by a peristaltic pump, and the coating temperature is set to 30-36℃.

3. The curing process for coated tempered glass according to claim 1, characterized in that: In step S2, the heating method of the plating curing oven is to use far-infrared heating tubes. The far-infrared heating tubes are made of quartz glass with ceramic heads and are evenly arranged in the oven. The far-infrared heating tubes heat up to the set temperature at a rate of 14-16℃ / min. The temperature is controlled by digital display.

4. The curing process for coated tempered glass according to claim 1, characterized in that: The plating curing oven is divided into an inner layer, an inner insulation layer, and an outer layer. The inner layer is made of mirror stainless steel plate. The upper and side thickness of the inner insulation layer is 150-160mm, and the lower thickness is 100-110mm. The insulation material is rock wool board. The outer layer is made of powder-coated carbon steel plate.

5. The curing process for coated tempered glass according to claim 1, characterized in that: The rollers of the conveyor roller track in the plating curing furnace are made of ceramic rollers, the distance between the rollers is 195-205mm, and the roller runout is set to 0.01-0.03mm. The roller is driven by a variable frequency motor reducer that drives the transmission shaft through a sprocket and chain. The transmission shaft then drives the ceramic roller to rotate through a double polyurethane transmission belt.

6. The curing process for coated tempered glass according to claim 1, characterized in that: Each section of the plating and curing oven is equipped with a circulating fan at the top to circulate and heat the air, creating turbulence in the oven. The starting and stopping of the circulating fan is linked to the heater in the corresponding oven section. When the heater is working, the circulating fan starts simultaneously, and its speed is PID-regulated according to the difference between the oven temperature and the set temperature. Each section of the plating and curing oven is equipped with a centrifugal exhaust fan at the top. The fan is controlled by a timer to start and stop. Adjusting the duration and interval of the fan's exhaust will remove the volatile organic compounds from the oven. The inner wall of the upper furnace body of each section of the plating and curing furnace gradually narrows from the middle towards the exhaust port, and the cross-section is inverted funnel shape.

7. The curing process for coated tempered glass according to claim 1, characterized in that: The modified coating solution is prepared through the following steps: S101. Mix anhydrous ethanol, deionized water, and dilute hydrochloric acid evenly to prepare an acidic alcohol-water solution. S102. Add the modified solution dropwise to the acidic alcohol aqueous solution at a rate of 3-4 mL / min. After the addition is complete, stir at room temperature for 1-2 h. Then, heat to 40-45℃ under sealed conditions and stir for 20-24 h to obtain the sol. S103. Cool the sol to room temperature, dilute it with anhydrous ethanol to a solid content of 4-5 wt%, and filter it through a 0.4-0.5 μm polytetrafluoroethylene filter membrane to obtain the modified coating solution.

8. The curing process for coated tempered glass according to claim 7, characterized in that: The modified solution in step S102 is prepared through the following steps: S1021. Ethyl silicate, perfluorodecyltrimethoxysilane, γ-glycidyl etheroxypropyltrimethoxysilane, and γ-aminopropyltriethoxysilane are added sequentially to anhydrous ethanol and stirred for 5-8 min to obtain a homogeneous mixture. Acetylacetone is added dropwise to the homogeneous mixture while stirring, and stirring is continued for 5-8 min to obtain a transparent silane mixture. S1022. Premix deionized water and glacial acetic acid to prepare an acid-water solution. Add the acid-water solution dropwise to the transparent silane mixture at a rate of 10-15 mL / min while stirring, until the addition is complete, and then stir for 30-35 min. S1023. After stopping stirring, seal and let stand for 1-1.5 hours to obtain a clear modified solution.

9. The curing process for coated tempered glass according to claim 7, characterized in that: In step S101, the mass ratio of anhydrous ethanol, deionized water, and dilute hydrochloric acid is 100:(8-12):(0.8-1.2). In step S102, the mass ratio of the acidic alcohol aqueous solution to the modified solution is 100:(25-35).

10. The curing process for coated tempered glass according to claim 8, characterized in that: In step S1021, the mass ratio of ethyl silicate, perfluorodecyltrimethoxysilane, γ-glycidyl etheroxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, anhydrous ethanol, and acetylacetone is 100:(8-12):(5-9):(3-7):(200-300):(4-8). In step S1022, the mass ratio of deionized water to glacial acetic acid is 100:(1.5-2.5); in step S1022, the mass ratio of the acid aqueous solution to the transparent silane mixture is 1:(3-4.5).

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