Glass durability dynamic erosion device and evaluation method

Abstract

The application provides a glass corrosion resistance dynamic erosion device and an evaluation method, and belongs to the technical field of glass performance evaluation. A circulating spray system formed by an erosion liquid circulating pump and a spray nozzle sprays the erosion liquid in the form of mist droplets to the sample surface continuously and uniformly. This not only washes away the corrosion products on the surface, so that the fresh erosion liquid continuously contacts the sample and accelerates the reaction, but also simulates the actual dynamic working conditions such as rain and moisture splashing. Through the combination of the dynamic erosion device and the intermittent ion content detection, the loss rate of each component in the erosion process is monitored in real time to evaluate the erosion rate of the glass, which helps to analyze the erosion mechanism and guide product improvement. Meanwhile, the dynamic circulating spray device can wash away the corrosion products formed on the surface of the glass in time, simulates the glass use environment, and improves the accuracy of the evaluation effect.

Description

Technical Field

[0001] This invention belongs to the field of glass performance evaluation technology, specifically relating to a dynamic corrosion resistance device and evaluation method for glass. Background Technology

[0002] During the manufacturing process of display modules, the substrate glass undergoes a series of complex chemical treatment steps, including frequent rinsing in various etching solutions (from acidic to neutral to alkaline). These chemical liquids are designed to clean, etch, or modify the glass surface to prepare for subsequent thin-film transistors (TFTs) or display pixel layers. Therefore, the substrate glass must possess excellent chemical resistance to ensure that it does not undergo excessive corrosion under the action of various etching solutions and does not produce any visible residues, so as not to affect the optical performance and yield of the display.

[0003] Currently, the traditional method for evaluating the chemical resistance of substrate glass mainly employs the static immersion method. This method is relatively simple to operate; typically, the glass sample is immersed in a chemical solution of a specific concentration and temperature, removed after a fixed time, and its corrosion resistance is assessed by measuring the mass loss per unit surface area of ​​the sample (e.g., the weight loss method). However, this method has significant technical limitations: Interference from corrosion product layer: During static immersion, corrosion products on the glass surface tend to accumulate near the sample and form a relatively stable coating layer. This layer hinders the continuous contact between the chemical medium and the fresh glass surface, thus slowing down or even blocking subsequent corrosion processes. This results in the measured corrosion rate often being lower than the actual corrosion rate of the glass under real dynamic erosion conditions, leading to a significant deviation between the test results and actual application conditions.

[0004] Static immersion methods fail to reflect dynamic corrosion processes: the final result (such as total mass loss) provided by static immersion methods is a cumulative, averaged value. It cannot reveal the dynamic process of chemical corrosion over time, such as the initial change in corrosion rate, whether acceleration or deceleration phases occur, and the instantaneous corrosion rate at different time points. This dynamic information is crucial for understanding the corrosion mechanism of glass, optimizing glass composition, and assessing its time-tolerance window in manufacturing processes.

[0005] The results are inconsistent with actual working conditions: Chemical treatments during module manufacturing are often dynamic, involving solution flow, rinsing, renewal, and continuous or phased changes in concentration and pH. Static immersion test conditions differ fundamentally from this dynamic and interactive actual working environment, thus limiting the representativeness and guiding value of the test results.

[0006] Due to the aforementioned limitations, there is an urgent need to develop a testing method and evaluation system that is closer to actual working conditions, can dynamically monitor and more accurately reflect the corrosion resistance of substrate glass under dynamic chemical erosion environment, so as to provide a reliable basis for the research and development, quality control and process optimization of high-performance display substrate glass. Summary of the Invention

[0007] The purpose of this invention is to overcome the problems of existing technologies, such as the formation of a corrosion product layer on the sample surface in a static etching solution, which leads to large errors in test results and fails to reflect the etching rate during the experiment. This invention provides a dynamic etching device and evaluation method for glass chemical resistance. The device has a simple structure and is easy to operate. The dynamic circulating spray device can wash away the corrosion products formed on the glass surface. Simultaneously, it can be used in conjunction with an ion concentration detection device to monitor the loss rate of each component during etching in real time, analyze the corrosion mechanism, and guide product improvement.

[0008] To achieve the above objectives, the present invention adopts the following technical solution: In a first aspect, the present invention provides a dynamic etching device for glass chemical resistance, comprising a constant temperature water bath containing a chemical etching device, the chemical etching device including an etching liquid circulation spray system, the etching liquid circulation spray system including an etching liquid circulation pump, a spray nozzle being provided at the end of the etching liquid circulation pump, a sample being fixed by a sample support frame and a sealing ring provided on the sample support frame, the spray nozzle acting on the sample, and a separation profile being horizontally arranged inside the chemical etching device, the spray chamber being isolated from the etching liquid circulation tank by the separation profile having a leakage hole.

[0009] The chemical etching device is convex in shape, with a sample support frame located at the top of the device and a sealing ring positioned in the middle of the support frame. The sealing ring vertically fixes the sample above the separation profile.

[0010] The sample is equipped with erosion liquid circulation pumps on both sides, and the spray nozzles at the end of the erosion liquid circulation pumps act on the sample.

[0011] The diameter of the droplets sprayed from the spray nozzle is 5~50um.

[0012] A liquid sampling port is opened on one side of the chemical etching device, and a liquid sampling gun is inserted into the etching liquid through the liquid sampling port.

[0013] A through hole is opened on the other side of the chemical etching device, through which an etching liquid thermometer is installed.

[0014] The constant temperature water bath is equipped with a water bath heater at the bottom and a water bath thermocouple on the side wall.

[0015] The constant temperature water bath is equipped with a water inlet on its top.

[0016] Secondly, the present invention provides a method for evaluating the dynamic corrosion resistance of glass, comprising: The glass sample to be evaluated is vertically placed into the spray chamber through the sample support frame until the sample contacts the separating profile. The etching solution circulation pump is turned on to start the test. At fixed intervals, the etching solution is collected using a sampling gun and the content of each ion in the etching solution is detected. The sample is taken out, cleaned, dried and weighed. At the same time, the etching rate of the glass is calculated by combining the detection results of the content of each ion in the etching solution.

[0017] The erosion rate of the glass is calculated as follows:

[0018] in, C is the erosion rate; M is the detected ion concentration (mg / L); S is the volume of the erosion solution (L); and S is the surface area in contact with the erosion solution (cm²). 2 t represents the cumulative erosion time during liquid collection, in minutes.

[0019] Compared with the prior art, the present invention has the following beneficial effects: This invention provides a dynamic etching device and evaluation method for glass chemical resistance. A circulating spray system, formed by an etching solution circulation pump and spray nozzles, continuously and uniformly sprays the etching solution as droplets onto the sample surface. This not only washes away surface corrosion products, ensuring constant contact of fresh etching solution with the sample and accelerating the reaction, but also simulates actual dynamic conditions such as rain and moisture splashing. An internally designed horizontally arranged perforated profile cleverly divides the device into an upper spray chamber and a lower etching solution circulation tank. This design ensures uniform droplet descent and smooth return of excess etching solution, achieving separation and circulation between the dynamic spraying process and the static storage area, thus guaranteeing the stability of the spray solution composition and flow rate. By combining the dynamic etching device with intermittent ion content detection, the loss rate of each component during etching can be monitored in real time to evaluate the glass etching rate. This helps analyze the etching mechanism, guide product improvement, and the dynamic circulating spray device promptly washes away corrosion products formed on the glass surface, simulating the glass's usage environment and improving the accuracy of the evaluation results.

[0020] Furthermore, by setting spray nozzles on both sides of the sample and limiting the droplet diameter (5~50μm), double-sided, uniform, and high specific surface area atomized contact was achieved, which further enhanced the kinetic conditions of the erosion process and significantly shortened the test cycle required to obtain effective corrosion data.

[0021] Furthermore, the sample is vertically fixed using a sample support frame and sealing ring, ensuring effective isolation between the sample testing area and the external environment and non-testing areas. This prevents edge corrosion or leakage caused by improper installation and improves the reliability and repeatability of experimental results.

[0022] Furthermore, the entire chemical etching apparatus is placed in a constant temperature water bath, where the temperature is precisely controlled by the water bath heater and thermocouples. Combined with the etching solution thermometer, the temperature of the etching solution can be dually monitored and controlled with high precision, eliminating the influence of temperature fluctuations on the corrosion rate and meeting the stringent requirements of standard testing.

[0023] Furthermore, the design of the liquid sampling port and sampling gun on the side wall allows for the periodic extraction of the etching liquid for analysis without interrupting the testing process or damaging the sealed environment, thereby enabling real-time and dynamic monitoring of the glass corrosion process. Attached Figure Description

[0024] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0025] Figure 1 This is a schematic diagram of the dynamic corrosion resistance device for glass according to the present invention; Figure 2 This is a schematic diagram of the erosion rate in Embodiment 2 of the present invention.

[0026] The following are the labels in the attached diagram: 1. Constant temperature water bath; 2. Water bath heater; 3. Water bath thermocouple; 4. Water inlet; 5. Etching solution circulation pump; 6. Spray nozzle; 7. Liquid outlet; 8. Liquid sampling gun; 9. Etching solution thermometer; 10. Separation profile; 11. Etching solution; 12. Sealing ring; 13. Sample support frame; 14. Protective cover; 15. Sample. Detailed Implementation

[0027] In the following description, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments can be modified in various ways without departing from the spirit or scope of the invention. Therefore, the drawings and description are considered to be exemplary in nature and not restrictive.

[0028] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0029] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a communication connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0030] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can include direct contact between the first and second features, or contact between the first and second features through another feature between them. Furthermore, "above," "over," and "on top" of the second feature includes the first feature being directly above or diagonally above the second feature, or simply indicates that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature includes the first feature being directly above or diagonally above the second feature, or simply indicates that the first feature is at a lower horizontal level than the second feature.

[0031] It should be understood that, when used in this specification and the appended claims, the terms "comprising" and "including" indicate the presence of the described features, integrals, steps, operations, elements and / or components, but do not exclude the presence or addition of one or more other features, integrals, steps, operations, elements, components and / or collections thereof.

[0032] It should also be understood that the terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. As used in this specification and the appended claims, the singular forms “a,” “an,” and “the” are intended to include the plural forms unless the context clearly indicates otherwise.

[0033] It should also be further understood that the term "and / or" as used in this specification and the appended claims refers to any combination of one or more of the associated listed items and all possible combinations, and includes such combinations.

[0034] The accompanying drawings illustrate various structural schematic diagrams according to embodiments disclosed in this invention. These drawings are not to scale, and some details have been enlarged for clarity, and some details may have been omitted. The shapes of the various regions and layers shown in the drawings, as well as their relative sizes and positional relationships, are merely exemplary and may deviate from reality due to manufacturing tolerances or technical limitations. Furthermore, those skilled in the art can design regions / layers with different shapes, sizes, and relative positions as needed.

[0035] The embodiments of the present invention will now be described in detail with reference to the accompanying drawings.

[0036] Example 1 A dynamic etching device for glass chemical resistance has the following structural components: like Figure 1 As shown, a dynamic etching device for glass chemical resistance includes a constant-temperature water bath 1, which contains deionized water or heat-conducting oil as the heat transfer medium. The constant-temperature water bath 1 holds the chemical etching device. A water bath heater 2 is installed at the bottom of the constant-temperature water bath 1 to heat the heat transfer medium. A water bath thermocouple 3 is installed on the side wall of the constant-temperature water bath 1 to monitor and feedback the temperature of the heat transfer medium to the temperature control system in real time, achieving precise closed-loop temperature control. A water inlet 4 is provided at the top of the constant-temperature water bath 1 to replenish the heat transfer medium lost through evaporation. The constant-temperature water bath 1 contains the chemical etching device.

[0037] The chemical etching apparatus has a convex overall structure, is made of chemically corrosion-resistant material, and is immersed in the heat transfer medium of a constant-temperature water bath 1 to achieve constant temperature control of the etching solution within the chamber. The interior of the chamber is divided into a spray chamber and an etching solution circulation tank by a horizontally positioned perforated separating profile 10. The spray chamber is used to fix the sample 15 to be tested, while the etching solution circulation tank stores the etching solution 11. The etching solution 11 can be configured according to evaluation criteria or actual application environment, such as deionized water, acidic solutions (e.g., acetic acid solution with pH=4), alkaline solutions, etc. The chemical etching apparatus includes an etching solution circulation spray system, including at least one etching solution circulation pump 5, preferably a corrosion-resistant magnetically driven pump or peristaltic pump. The inlet of the etching solution circulation pump 5 extends through a pipe into the etching solution 11 at the bottom of the chamber. The outlet of the etching solution circulation pump 5 is connected to a spray nozzle 6, which is preferably an atomizing nozzle capable of atomizing the etching solution into fine droplets with a diameter range of 5~50μm. The finer droplets ensure that the etching solution 11 is in full contact with the surface of the sample 15, and can also wash away the corrosion products formed on the glass surface.

[0038] Preferably, the chemical corrosion resistant material is a combination of one or more of the following: high-quality stainless steel, polytetrafluoroethylene, reinforced polyvinyl chloride, and ceramics, to avoid differences in ion concentration caused by chemical corrosion of the device materials.

[0039] The upper part of the chemical etching apparatus is equipped with a sample support frame 13, which is typically a flat plate with a central circular hole. A sealing ring 12 is fitted into the central circular hole of the sample support frame 13. This sealing ring 12 is preferably made of a material with excellent elasticity and chemical corrosion resistance (such as fluororubber or silicone rubber). During testing, the glass sample 15 to be tested (usually a sheet) is placed vertically, and its edges are pressed between the sealing ring 12 and the top cover of the cavity (not shown in the figure) or another pressing component, thereby fixing the sample and sealing the cavity. After fixing, the lower surface of the sample 15 (i.e., the surface being tested) is in contact with the separating profile 10, which has a leakage hole. The upper surface of the sample 15 is more than 30 mm above the spray chamber, and its surface is directly facing the etching liquid droplets from the spray nozzle 6. A protective cover 14 is provided on the top of the chemical etching apparatus.

[0040] The sample 15 is vertically placed in the sample support frame 13 using a polymer sealing ring 12, with its bottom in contact with the separating profile 10. This ensures that the sample surface area in contact with the etching liquid 11 is the same in each test, increasing the accuracy of the comparison sample results and preventing leakage of the etching liquid. The protective cover 14 then creates a sealed space for the entire dynamic etching device, enhancing safety.

[0041] As a preferred embodiment, two sets of erosion liquid circulation spraying systems are symmetrically arranged on both sides of the sample 15, namely, two erosion liquid circulation pumps 5 and their corresponding spray nozzles 6. This double-sided spraying design can ensure that the two main surfaces of the sample 15 are subjected to uniform and sufficient dynamic erosion, eliminating the influence of concentration gradients or temperature gradients that may be caused by single-sided spraying, making the test results more representative and comparable.

[0042] Furthermore, to monitor test conditions and perform sampling analysis in real time, a sampling port 7 is provided on one side of the chemical etching apparatus. A sampling gun 8 passes through this port and extends into the etching solution 11 at the bottom without damaging the cavity seal, periodically extracting etching solution samples for subsequent analysis of the concentration of dissolved ions in the etching solution, thereby calculating the glass etching rate. A through-hole is provided on the other side of the chemical etching apparatus to install an etching solution thermometer 9, which is used to directly and accurately monitor the actual temperature of the etching solution 11, serving as a supplementary verification of the water bath temperature control.

[0043] Example 2 A method for evaluating the dynamic corrosion resistance of glass includes the following steps: Step 1: Cut the glass sample 15 into standard size 150*100*0.5mm, and polish the edges of the sample to be smooth and burr-free; wipe the sample surface with anhydrous ethanol, let it dry naturally, mark the top of the sample in a position that does not come into contact with the chemical medium, then accurately measure the size of sample 15 and weigh it, and record the results. Step 2: Prepare 5L of chemical etching medium that meets the experimental requirements using a container made of a chemically resistant polymer material such as polytetrafluoroethylene. After stirring evenly, pour the medium into the etching solution circulation tank of the chemical etching device through the liquid outlet.

[0044] Step 3: Fill the constant temperature water bath 1 with water through water inlet 4. Set the temperature and time according to the test requirements, and set the duration to be 0.5-1 hour longer than the test duration. Begin heating. The water in the constant temperature water bath 1 heats up, transferring heat to the etching solution circulation tank. Observe the etching solution thermometer 9. After the chemical medium is heated to the test temperature and stabilized for 20 minutes, vertically place sample 15 into the spray chamber through sample support frame 13 until it touches the bottom. Ensure that the dimensions of sample 15 placed in the spray chamber are 100*100*0.5mm. Cover with the protective cover, turn on the spray circulation system, and begin the test. Calculate the sample surface area S (in cm²) in contact with the etching solution. 2 ), Step 4: At fixed intervals, use the liquid sampling gun 8 to take 5 mL of etching solution and test the content of each ion in the etching solution 11; Step 5: Take samples of the etching solution at fixed intervals, repeating Step 4 until the experiment is completed. Then, take another sample of the etching solution for ion content analysis. Remove the sample, clean and dry it, and weigh it. Simultaneously, combine the ion content analysis results from each etching solution analysis in Step 4 to calculate the glass etching rate, such as... Figure 2 As shown.

[0045] The formula for calculating the erosion rate of glass is as follows:

[0046] in, C is the erosion rate; M is the detected ion concentration (mg / L); S is the volume of the erosion solution (L); and S is the surface area in contact with the erosion solution (cm²). 2 t represents the cumulative erosion time during liquid collection, in minutes.

[0047] The corrosion resistance of different glass samples is objectively evaluated by comparing their corrosion rate values ​​under standardized dynamic or static erosion conditions. A slower corrosion rate indicates better corrosion resistance.

[0048] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that modifications or equivalent substitutions can still be made to the specific implementation of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A dynamic etching device for glass chemical resistance, characterized in that, The device includes a constant temperature water bath (1), which contains a chemical etching device. The chemical etching device includes an etching liquid circulation spray system, which includes an etching liquid circulation pump (5). The end of the etching liquid circulation pump (5) is provided with a spray nozzle (6). The sample (15) is fixed by a sample support frame (13) and a sealing ring (12) provided on the sample support frame (13). The spray nozzle (6) acts on the sample (15). A separation profile (10) is horizontally arranged inside the chemical etching device. The spray chamber is isolated from the etching liquid circulation box by the separation profile (10) with a leakage hole.

2. The dynamic etching device for glass chemical resistance according to claim 1, characterized in that, The chemical etching device is convex in shape. The sample support frame (13) is located on the upper part of the chemical etching device, and the sealing ring (12) is located in the middle of the sample support frame (13). The sealing ring (12) vertically fixes the sample (15) above the separation profile (10).

3. The dynamic etching device for glass chemical resistance according to claim 2, characterized in that, The sample (15) is provided with erosion liquid circulation pumps (5) on both sides, and the spray nozzle (6) at the end of the erosion liquid circulation pump (5) acts on the sample (15).

4. The dynamic etching device for glass chemical resistance according to claim 3, characterized in that, The diameter of the droplets sprayed from the spray nozzle (6) is 5~50um.

5. The dynamic etching device for glass chemical resistance according to claim 2, characterized in that, A liquid sampling port (7) is opened on one side of the chemical etching device, and a liquid sampling gun (8) is inserted into the etching liquid (11) through the liquid sampling port (7).

6. The dynamic etching device for glass chemical resistance according to claim 5, characterized in that, A through hole is opened on the other side of the chemical etching device, and an etching liquid thermometer (9) is installed through the through hole.

7. The dynamic etching device for glass chemical resistance according to claim 1, characterized in that, The constant temperature water bath (1) is equipped with a water bath heater (2) at the bottom and a water bath thermocouple (3) on the side wall.

8. The dynamic etching device for glass chemical resistance according to claim 7, characterized in that, The constant temperature water bath (1) is provided with a water inlet (4) at the top.

9. A method for evaluating the dynamic corrosion resistance of glass, based on the dynamic corrosion resistance device for glass as described in any one of claims 1 to 8, characterized in that, include: The glass sample (15) to be evaluated is vertically placed into the spray chamber through the sample support frame (13) until the sample (15) contacts the separation profile (10). The etching liquid circulation pump (5) is turned on to start the test. At fixed intervals, the etching liquid (11) is taken with the liquid gun (8) and the content of each ion in the etching liquid (11) is detected. The sample (15) is taken out, cleaned and dried and weighed. At the same time, the etching rate of the glass is calculated by combining the detection results of the content of each ion in the etching liquid (11).

10. The method for evaluating the dynamic corrosion resistance of glass according to claim 9, characterized in that, The erosion rate of the glass is calculated as follows: in, C is the erosion rate; M is the detected ion concentration (mg / L); S is the volume of the erosion solution (L); and S is the surface area in contact with the erosion solution (cm²). 2 t represents the cumulative erosion time during liquid collection, in minutes.

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