Efficient glass substrate cleaning agent and preparation method thereof
By using a pH buffer and a composite metal complexing agent in the glass substrate cleaning agent, a highly efficient cleaning agent that does not corrode glass was prepared, solving the problem of glass corrosion caused by cleaning agents in the prior art, and achieving the effects of efficient cleaning and extended service life.
Patent Information
- Application Number
- CN202511759919.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-27
- Publication Date
- 2026-02-17
AI Technical Summary
Existing glass substrate cleaning agents tend to corrode the glass while removing contaminants, making it difficult to meet the needs of high-precision electronic manufacturing, and the cleaning effect is also unsatisfactory.
A highly efficient cleaning agent that does not corrode glass was prepared by using a pH buffer composed of sodium isopropylbenzenesulfonate, terephthalic acid, sodium barbital and hydrochloric acid to maintain the cleaning agent at a neutral pH value, combined with a composite metal complexing agent and surfactant, and adding a glass substrate protectant.
It effectively removes particles, oil, metal ions, and static-adhered dust from glass under neutral conditions, extending the service life of the cleaning agent, improving cleaning results, and without corroding the glass.
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Figure CN121538040A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of cleaning agent technology, and in particular to a high-efficiency glass substrate cleaning agent and its preparation method. Background Technology
[0002] Glass substrates are a crucial material, widely used in the manufacturing of products such as LCD displays, touch screens, and solar panels. Although glass substrates appear hard and smooth, they become contaminated with numerous tiny particles, oil stains, metal ions, and even statically deposited dust during production. If these contaminants are not thoroughly removed, they will affect subsequent processes such as coating and etching, ultimately impacting product yield and performance. Therefore, a water-based glass substrate cleaning agent plays a vital role in the entire manufacturing process.
[0003] Glass substrate cleaning agents include acidic and alkaline cleaning agents. Acidic cleaning agents are volatile, and if the acidity is too strong, it can easily scratch the glass and cause black spots; if the acidity is too weak, the cleaning effect is poor, and residual dust and particles can lead to short circuits, pattern transfer failures, or decreased optical performance. Using strong alkaline detergents to dissolve and remove hardened materials firmly adhered to the glass substrate can also slightly dissolve the substrate surface, damaging it. Furthermore, the substrate surface may be contaminated by alkaline components, making it difficult to meet the requirements of high-precision electronic manufacturing.
[0004] Therefore, there is an urgent need to develop a neutral cleaning agent that can effectively decompose grease, remove particles, reduce static electricity, remove inorganic pollutants, and not corrode glass, thus restoring the glass surface to a clean state. Summary of the Invention
[0005] To address the shortcomings of existing technologies, this invention provides a highly efficient glass substrate cleaning agent and its preparation method. The cleaning agent of this invention can effectively maintain a neutral pH and extend its service life. While effectively decomposing grease, removing particles, reducing static electricity, and eliminating inorganic contaminants, it has no corrosive effect on the glass, restoring the glass surface to a clean state.
[0006] To achieve the above objectives, the present invention adopts the following technical solution: A high-efficiency glass substrate cleaning agent, comprising the following components by weight percentage: Sodium cumenesulfonate 5-8%; Terephthalic acid 1.0-1.5%; Dipropylene glycol methyl ether 3-5%; Polyethylene glycol 0.5-1%; Sodium barbiturate 1.2-1.5%; Hydrochloric acid 0.15-0.18%; Kathon preservative 0.05-0.07%; Glass substrate protectant 5-7%; Metal complexing agent 6-8%; Surfactant 0.05-0.2%; The remainder is pure water.
[0007] Preferably, the glass substrate protectant is composed of 1% sodium nitrite, 5% disodium hydrogen phosphate, 10% sodium silicate, 5% phenylethanolamine, and 79% pure water.
[0008] Preferably, the metal complexing agent is composed of 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, 5% iminodisuccinic acid, and 75% pure water.
[0009] Preferably, the surfactant is composed of 45% sodium diisooctyl sulfosuccinate, 17% ethoxylated acetylenol, 35% isopropanol, and 3% tributyl phosphate.
[0010] Preferably, the pH value of the cleaning agent is 6.5-7.5.
[0011] Another object of the present invention is to disclose a method for preparing the above-mentioned high-efficiency glass substrate cleaning agent, comprising the following steps: In a cleanroom, half the volume of pure water was added to the reactor using a flow meter at room temperature. Stirring was started at 200 rpm, and sodium barbital and hydrochloric acid were added, stirring for 20 minutes. The reactor was then heated to 45°C with steam, and sodium isopropylbenzenesulfonate and glass substrate protectant were added sequentially. After 20 minutes, the temperature was raised to 55°C, and terephthalic acid and Kathon preservative were added. The temperature was maintained at 55°C and stirred for 30 minutes, then the steam was turned off. A metal complexing agent and the remaining pure water were added, and cooling water was turned on to lower the reactor temperature to 30°C. Dipropylene glycol methyl ether, polyethylene glycol, and surfactant were then slowly added, and the mixture was stirred for 1 hour. Samples were taken to analyze the solid content, density, pH, and surface tension. After passing the tests, the stirrer was turned off, and circulation filtration began. The mixture was circulated through 0.5μm, 0.2μm, and 0.1μm filter cartridges for 2 hours, and particle size was analyzed. After passing the tests, circulation was turned off, and the reactor material was transported through pipelines to a Class 100 cleanroom dispensing station for dispensing to obtain the finished product.
[0012] Preferably, the glass substrate protectant is prepared by the following steps: at room temperature, 79% pure water is added to a clean inorganic reactor through a flow meter, stirring is started at 200 rpm, 5% disodium hydrogen phosphate and 10% sodium silicate are added sequentially and stirred for 30 minutes, then 5% phenylethanolamine is slowly added and stirred for 20 minutes, and finally 1% sodium nitrite is added and stirred for 30 minutes. The mixture is then filtered and packaged using a 1-micron filter bag for later use.
[0013] Preferably, the metal complexing agent is prepared by the following steps: at room temperature, in a clean space, 75% pure water, 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, and 10% iminodisuccinic acid are added sequentially, stirred for 40 minutes, filtered and packaged using a 1-micron filter bag, and set aside for later use.
[0014] Preferably, the surfactant is prepared by the following steps: At 25°C, 35 kg of isopropanol is added to a clean 500 L stainless steel reactor, and stirring is started at 200 rpm. Then, 10 kg of ethoxylated acetylenol and 2 kg of tributyl phosphate are added. After stirring for 20 minutes, the stirring is turned off, and after the bubbles have completely disappeared, the temperature is raised to 40°C. At the same time, stirring is started at 120 rpm, and 0.5 kg of sodium diisooctyl sulfosuccinate is added every 5 minutes until all 45 kg of sodium diisooctyl sulfosuccinate has been added. The stirring is kept at a constant speed until all sodium diisooctyl sulfosuccinate is dissolved. The temperature is then lowered to 25°C, and the remaining 7 kg of ethoxylated acetylenol and 1 kg of tributyl phosphate are added. The stirring speed is adjusted to 200 rpm, and after stirring for 1 hour, the mixture is dispensed for use.
[0015] Compared with the prior art, the present invention has the following beneficial effects: The cleaning agent of the present invention maintains the pH value of the cleaning agent at around 7.0 by adding a pH buffer composed of sodium barbital and hydrochloric acid, thus maintaining the stability of the cleaning effect.
[0016] The cleaning agent of this invention can effectively remove particles, oil stains, metal ions, inorganic pollutants, and even statically attached dust from glass under neutral conditions, while not leaving water residue or fogging.
[0017] This invention incorporates a composite metal complexing agent, which efficiently complexes the cleaned metal impurities, thereby extending the service life of the cleaning agent.
[0018] This invention incorporates a composite surfactant, which reduces the surface tension of the cleaning agent to below 30 dyn / cm, thereby improving the cleaning effect.
[0019] Glass corrosion is a dynamic process involving multiple stages such as adsorption, diffusion, reaction, and product formation of the corrosive medium. The neutral pH of the cleaning agent significantly reduces its corrosive effect on the glass. Furthermore, the addition of a glass substrate protectant further prevents the cleaning agent from corroding the glass substrate. Therefore, the cleaning agent of this invention is non-corrosive to glass substrates. Attached Figure Description
[0020] Figure 1 This is an image of the glass substrate under OM (Obstacle Course) before cleaning; Figure 2 This is an image of the glass substrate after cleaning in Example 1, viewed under OM. Figure 3 This is an SEM image of the glass substrate after cleaning in Example 2; Figure 4 This is a SEM image of the glass substrate after cleaning, as shown in Comparative Example 1. Detailed Implementation
[0021] The present invention will be further described below with reference to embodiments. However, it should be noted that the embodiments do not constitute a limitation on the scope of protection of the present invention.
[0022] A high-efficiency glass substrate cleaning agent, comprising the following components by weight percentage: Sodium cumenesulfonate 5-8%; Terephthalic acid 1.0-1.5%; Dipropylene glycol methyl ether 3-5%; Polyethylene glycol 0.5-1%; Sodium barbiturate 1.2-1.5%; Hydrochloric acid 0.15-0.18%; Kathon preservative 0.05-0.07%; Glass substrate protectant 5-7%; Metal complexing agent 6-8%; Surfactant 0.05-0.2%; The remainder is pure water.
[0023] The glass substrate protectant consists of 1% sodium nitrite, 5% disodium hydrogen phosphate, 10% sodium silicate, 5% phenylethanolamine, and 79% pure water.
[0024] The glass substrate protectant is prepared by the following steps: At room temperature, 79% pure water is added to a clean inorganic reactor through a flow meter, and stirring is started at 200 rpm. Then, 5% disodium hydrogen phosphate and 10% sodium silicate are added sequentially and stirred for 30 minutes. Next, 5% phenylethanolamine is slowly added and stirred for 20 minutes. Finally, 1% sodium nitrite is added and stirred for 30 minutes. The mixture is then filtered through a 1-micron filter bag and packaged for later use.
[0025] The metal complexing agent is composed of 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, 5% iminodisuccinic acid, and 75% pure water.
[0026] The metal complexing agent is prepared by the following steps: Under room temperature conditions, in a clean space, 75% pure water, 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, and 10% iminodisuccinic acid are added sequentially, stirred for 40 minutes, filtered and packaged using a 1-micron filter bag, and set aside for later use.
[0027] The surfactant is composed of 45% sodium diisooctyl sulfosuccinate, 17% ethoxylated acetylenol, 35% isopropanol, and 3% tributyl phosphate.
[0028] In an embodiment of the present invention, the surfactant is prepared by the following steps: At 25°C, 35 kg of isopropanol is added to a clean 500 L stainless steel reactor, stirring is started at 200 rpm, then 10 kg of ethoxylated acetylenol and 2 kg of tributyl phosphate are added. After stirring for 20 minutes, the stirring is turned off, and after the bubbles have completely disappeared, the temperature is raised to 40°C, and stirring is started at 120 rpm. 0.5 kg of sodium diisooctyl sulfosuccinate is added every 5 minutes until 45 kg of sodium diisooctyl sulfosuccinate is added. Stirring is maintained at a constant speed until all sodium diisooctyl sulfosuccinate is dissolved. The temperature is then lowered to 25°C, and the remaining 7 kg of ethoxylated acetylenol and 1 kg of tributyl phosphate are added. The stirring speed is adjusted to 200 rpm, and after stirring for 1 hour, the mixture is dispensed for later use.
[0029] The cleaning agent of the present invention maintains the pH value of the cleaning agent at 6.5-7.5 by adding a pH buffer composed of sodium barbital and hydrochloric acid, thus maintaining the stability of the cleaning effect.
[0030] The preparation method of the above-mentioned high-efficiency glass substrate cleaning agent includes the following steps: In a clean space, at room temperature, half of the pure water is added to the reactor using a flow meter, stirring is started at 200 rpm, sodium barbital and hydrochloric acid are added, and stirring is carried out for 20 minutes; then the temperature is heated to 45°C with steam, and sodium isopropylbenzenesulfonate and glass substrate protectant are added sequentially; after 20 minutes, the temperature is raised to 55°C, terephthalic acid and Kathon preservative are added, and the temperature is maintained at 55°C while stirring for 30 minutes, and the steam is turned off; then a metal complexing agent and the remaining pure water are added, and the temperature of the reactor is lowered to 30°C by turning on the cooling water, and then dipropylene glycol methyl ether, polyethylene glycol and surfactant are slowly added, and stirring is carried out for 1 hour. Samples are taken to analyze the solid content, density, pH and surface tension. After passing the test, the stirrer is turned off, and circulation filtration is started. The reactor is circulated and filtered for 2 hours through 0.5μm, 0.2μm and 0.1μm filter cartridges. The particle size is taken to analyze. After passing the test, the circulation is turned off, and the material in the reactor is transported through pipeline to the dispensing station in a Class 100 clean room for dispensing to obtain the finished product.
[0031] To illustrate the advantages of the present invention, the following description is provided through a comparison of Examples 1-4 and Comparative Examples 1-4, as shown in Table 1: Table 1 Formulations of Examples 1-4 and Comparative Examples 1-4
[0032] The cleaning agents prepared in Examples 1-4 and Comparative Examples 1-4 were subjected to performance tests respectively: (1) Test method for cleaning ability of dirt and impurities on glass substrate: Under the same conditions, the cleaning agents of Examples 1-4 and Comparative Lists 1-4 were diluted 30 times respectively. The same glass substrate was sprayed for 2 minutes at 40°C in spray mode with a spray pressure of 0.15 MPa. Then, it was rinsed with ultrapure water for 1 minute and dried with nitrogen. The changes of the sample before and after cleaning were observed using OE and SEM.
[0033] (2) Test method for corrosion of glass substrate: Cut the glass substrate into 2cm×2cm square pieces, treat with isopropanol at room temperature for 5min, wash with pure water, dry with nitrogen, and then immerse in the cleaning agents of Examples 1-4 and Comparative Examples 1-4 at 40℃ for 5 hours. After rinsing with deionized water, dry with nitrogen and observe the changes on the glass surface before and after under SEM. At the same time, check the aluminum content in the cleaning agent. The glass substrate contains aluminum. If it is corroded, the aluminum content in the cleaning agent will increase.
[0034] (3) Test on the change of glass substrate roughness before and after cleaning: The cleaning agents of Examples 1-4 and Comparative Examples 1-4 were diluted 30 times with ultrapure water to prepare diluted cleaning solutions. At 40°C, a 2cm×2cm square glass substrate was placed in the solution and soaked for 5 hours. After rinsing with deionized water, it was dried with nitrogen gas and the roughness Ra value was measured by AFM.
[0035] (4) Test method for cleaning agent service life: Cut the glass substrate into 10cm×10cm square pieces, take 2L of diluted cleaning agent, and spray it at 40℃ until the glass is basically not cleaned. Record the number of pieces cleaned.
[0036] The test results for each performance indicator are shown in Table 2: Table 2. Performance test results of the cleaning agents prepared in Examples 1-4 and Comparative Examples 1-4
[0037] Experiments showed that Examples 1-4 all met the requirements, effectively decomposing grease, removing particles, reducing static electricity, and eliminating inorganic pollutants without corroding glass.
[0038] Figure 1 This is an image of the glass substrate under OM (Obstacle Course) before cleaning; Figure 2 This is an image of the glass substrate after cleaning in Example 1, viewed under OM. Figure 3 The image shown is an SEM image of the glass substrate after cleaning in Example 2. It can be seen that the glass substrate cleaned by the embodiment of the present invention not only removes stains but also shows no signs of glass corrosion.
[0039] In Comparative Example 1, no glass substrate protectant was used. After immersion for 5 hours, the aluminum ion concentration in the cleaning agent increased, resulting in increased roughness and significant corrosion of the glass substrate after cleaning. Figure 4 As shown.
[0040] In contrast, the absence of a pH buffer in column 2 made it difficult to maintain a neutral pH value in the later stages of cleaning, resulting in a reduced cleaning agent lifespan.
[0041] In Comparative Example 3, the complexing agent addition was 4%, which reduced the complexing effect and resulted in a higher metal impurity coefficient in the later stage. The 0.05-micron filter element became clogged after 55 hours, and the lifespan of the cleaning agent was reduced.
[0042] In Comparative Example 4, no complexing agent was added, and the 0.05-micron filter cartridge became clogged after 24 hours, indicating that the cleaning agent had a very short lifespan.
[0043] The technical solutions provided by the embodiments of the present invention have been described in detail above. Specific examples have been used to illustrate the principles and implementation methods of the embodiments of the present invention. The descriptions of the embodiments above are only for helping to understand the principles of the embodiments of the present invention. At the same time, for those skilled in the art, there will be changes in the specific implementation methods and application scope based on the embodiments of the present invention. Therefore, the content of this specification should not be construed as a limitation of the present invention.
Claims
1. A high-efficiency glass substrate cleaning agent, characterized in that, Includes the following components by mass percentage: Sodium cumenesulfonate 5-8%; Terephthalic acid 1.0-1.5%; Dipropylene glycol methyl ether 3-5%; Polyethylene glycol 0.5-1%; Sodium barbiturate 1.2-1.5%; Hydrochloric acid 0.15-0.18%; Kathon preservative 0.05-0.07%; Glass substrate protectant 5-7%; Metal complexing agent 6-8%; Surfactant 0.05-0.2%; The remainder is pure water.
2. The high-efficiency glass substrate cleaning agent according to claim 1, characterized in that, The glass substrate protectant is composed of 1% sodium nitrite, 5% disodium hydrogen phosphate, 10% sodium silicate, 5% phenylethanolamine, and 79% pure water.
3. The high-efficiency glass substrate cleaning agent according to claim 1, characterized in that, The metal complexing agent is composed of 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, 5% iminodisuccinic acid, and 75% pure water.
4. The high-efficiency glass substrate cleaning agent according to claim 1, characterized in that, The surfactant is composed of 45% sodium diisooctyl sulfosuccinate, 17% ethoxylated acetylenol, 35% isopropanol, and 3% tributyl phosphate.
5. The high-efficiency glass substrate cleaning agent according to claim 1, characterized in that, The cleaning agent has a pH value of 6.5-7.
5.
6. The method for preparing a high-efficiency glass substrate cleaning agent as described in any one of claims 1-5, characterized in that, Includes the following steps: In a cleanroom, half the volume of pure water was added to the reactor using a flow meter at room temperature. Stirring was started at 200 rpm, and sodium barbital and hydrochloric acid were added, stirring for 20 minutes. The reactor was then heated to 45°C with steam, and sodium isopropylbenzenesulfonate and glass substrate protectant were added sequentially. After 20 minutes, the temperature was raised to 55°C, and terephthalic acid and Kathon preservative were added. The temperature was maintained at 55°C and stirred for 30 minutes, then the steam was turned off. A metal complexing agent and the remaining pure water were added, and cooling water was turned on to lower the reactor temperature to 30°C. Dipropylene glycol methyl ether, polyethylene glycol, and surfactant were then slowly added, and the mixture was stirred for 1 hour. Samples were taken to analyze the solid content, density, pH, and surface tension. After passing the tests, the stirrer was turned off, and circulation filtration began. The mixture was circulated through 0.5μm, 0.2μm, and 0.1μm filter cartridges for 2 hours, and particle size was analyzed. After passing the tests, circulation was turned off, and the reactor material was transported through pipelines to a Class 100 cleanroom dispensing station for dispensing to obtain the finished product.
7. The method for preparing a high-efficiency glass substrate cleaning agent according to claim 6, characterized in that, The glass substrate protectant is prepared by the following steps: at room temperature, 79% pure water is added to a clean inorganic reactor through a flow meter, stirring is started at 200 rpm, 5% disodium hydrogen phosphate and 10% sodium silicate are added sequentially and stirred for 30 minutes, then 5% phenylethanolamine is slowly added and stirred for 20 minutes, and finally 1% sodium nitrite is added and stirred for 30 minutes. The mixture is then filtered and packaged using a 1-micron filter bag for later use.
8. The method for preparing a high-efficiency glass substrate cleaning agent according to claim 6, characterized in that, The metal complexing agent is prepared by the following steps: at room temperature, in a clean space, 75% pure water, 10% diethylenetriaminepentaacetic acid, 10% sodium ethylenediaminetetramethylene phosphate, and 10% iminodisuccinic acid are added sequentially, stirred for 40 minutes, filtered and packaged using a 1-micron filter bag, and set aside for later use.
9. The method for preparing a high-efficiency glass substrate cleaning agent according to claim 6, characterized in that, The surfactant is prepared by the following steps: At 25°C, 35 kg of isopropanol is added to a clean 500 L stainless steel reactor, and stirring is started at 200 rpm. Then, 10 kg of ethoxylated acetylenol and 2 kg of tributyl phosphate are added. After stirring for 20 minutes, the stirring is turned off, and after the bubbles have completely disappeared, the temperature is raised to 40°C. At the same time, stirring is started at 120 rpm, and 0.5 kg of sodium diisooctyl sulfosuccinate is added every 5 minutes until all 45 kg of sodium diisooctyl sulfosuccinate has been added. The stirring is kept at a constant speed until all sodium diisooctyl sulfosuccinate is dissolved. The temperature is then lowered to 25°C, and the remaining 7 kg of ethoxylated acetylenol and 1 kg of tributyl phosphate are added. The stirring speed is adjusted to 200 rpm, and after stirring for 1 hour, the mixture is dispensed for use.