Method for coating inner surface of glass container

Abstract

The invention relates to a method for coating the inner surface of a glass container, which comprises a frosting step and a silicification treatment step, and is characterized in that before silicification treatment, the frosted glass container is inverted, the inverted angle of the glass container is adjusted to be 75-85 degrees, and meanwhile, the rotating speed is adjusted to be 30-90 r / min. The preparation method has the advantages that the preparation method is simple, the condition is mild, the environmental protection requirement is met, the mechanical wear resistance of the film layer is improved, the prepared film layer has small thickness deviation, excellent uniformity and stable quality, and the preparation method is suitable for deep processing of glass storage bottles, especially storage bottles for high-purity chemical reagents.

Description

Technical Field

[0001] The present invention belongs to the field of glass deep processing and surface modification, and relates to a method for coating the inner surface of a glass container. Background Art

[0002] At present, some high-purity reagents on the market, such as high-purity chemicals for optics and electronics, high-purity chemicals for metal-oxide-semiconductor electronics industry, mass spectrometry pure grade reagents, etc., are very sensitive to light and temperature, are prone to aging, and extremely tiny impurities will also change their performance. Therefore, the requirements for packaging and storage are very strict.

[0003] Glass has excellent properties such as optics, mechanics, thermal stability, chemical stability, etc., and is an excellent material for storing and packaging high-purity reagents. However, using a glass bottle as a storage container will precipitate metal ions, affecting the use performance of the reagent. Therefore, it is urgent to treat the inner surface of the glass bottle.

[0004] Glass coating is a commonly used method in glass deep processing, especially in glass surface modification. The commonly used coating methods mainly include frosting (de-alkalization) treatment and silicification treatment. This method and process are more suitable for flat glass (which can ensure better film layer performance); but for curved glass, there will be a problem of thickness difference during the coating process, seriously affecting the uniformity of the film layer. Summary of the Invention

[0005] The purpose of the present invention is to solve the problem of poor film layer uniformity in the process of treating curved glass by the existing coating methods, and provide a method for coating the inner surface of a glass container. Before coating the inner surface of the glass container, the present invention obtains the inverted angle and rotation speed data of the glass container, can adjust the data in time, ensures that the glass container is in a good position before coating, avoids the situation that the silica sol layer coated on the inner surface of the glass container foams during sintering, reduces the deviation of the film formation thickness, improves the coating uniformity, ensures the film layer quality, and further blocks the precipitation of metal ions in the glass container body.

[0006] In order to achieve the above purpose, the technical solution adopted by the present invention is as follows: A method for coating the inner surface of a glass container, including a frosting step and a silicification treatment step, characterized in that: before the silicification treatment, the glass container after frosting treatment is inverted, the inverted angle of the glass container is adjusted to 75 - 85°, and at the same time, the rotation speed is adjusted to 30 - 90 r / min.

[0007] Further, the frosting step is: cleaning the glass container, putting a de-alkalizing agent into the bottle, then heating to 500 - 600 °C, keeping warm for 10 - 40 min, naturally cooling, and then cleaning the glass container with water, an alkali solution and an acid solution, and drying for use.

[0008] Furthermore, the de-alkalizing agent includes one or both of ferrous sulfate and ammonium sulfate.

[0009] Furthermore, the dosage of the de-alkalizing agent is 10 - 30 g / L.

[0010] Furthermore, the silicification treatment step is as follows: on the inner surface of a glass container with the inverted angle and rotation speed adjusted, a silica film is deposited by high-pressure spraying with silica sol, dried at a low temperature (80 - 120 °C), and then the deposition is repeated 0 - 6 times, followed by curing at a high temperature (350 - 550 °C).

[0011] Furthermore, the thickness of the silica film is 50–400 nm, which can be obtained by multiple sprayings according to performance requirements.

[0012] Furthermore, the silica sol is one of anti-reflective silica sol, weather-resistant silica sol, wear-resistant silica sol, etc.

[0013] Furthermore, the pressure of the high-pressure spraying is 0.3 - 0.9 Mpa, and the spraying time is 1 - 5 min.

[0014] Furthermore, the drying time is 10 - 30 min, and the curing time is 5 - 15 min.

[0015] Before coating the inner surface of the glass container, the present invention adjusts the inverted angle and rotation speed of the glass container to appropriate data, ensuring that the glass container is in a good position before coating, avoiding the foaming of the silica sol layer coated on the inner surface of the glass container during sintering, reducing the deviation of the film thickness, improving the uniformity of the coating, ensuring the film quality, and thus blocking the precipitation of metal ions in the glass container body.

[0016] The beneficial effects of the present invention: The preparation method of the present invention is simple, the conditions are mild, meeting the environmental protection requirements, improving the mechanical wear resistance of the film layer, the obtained film layer has a small thickness deviation and excellent uniformity, and the quality is relatively stable, being applicable to the deep processing of glass storage bottles, especially for storage bottles of high-purity chemical reagents. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is the film thickness effect diagram obtained in Example 1; Figure 2 It is the film thickness effect diagram obtained in Example 2; Figure 3 It is the film thickness effect diagram obtained in Example 3. DETAILED DESCRIPTION OF THE INVENTION

[0018] A method for coating the inner surface of a glass container, the specific implementation steps are as follows Example 1

[0019] (1) Use a glass bottle with a volume of 4 L. First, clean the glass bottle thoroughly. Put 40 g of ammonium sulfate into the bottle, perform a removal treatment on the glass surface, then heat it up to 550 °C, keep it warm for 20 min, and cool it naturally; (2) Then use water, an alkali solution (mass concentration ratio of potassium hydroxide: ethylenediaminetetraacetic acid: stearic acid: deionized water is 1:0.28:0.18:9.2) and an acid solution (mass concentration ratio of potassium hydroxide: glycerol: citric acid: glycerol fatty acid ester: deionized water is 1:0.32:28:0.42:17.5) to clean the glass bottle, dry it at 80 °C for 10 min for later use; (3) Invert the glass bottle dried in step (2), determine whether the data of the inversion angle and rotation speed meet the preset conditions, and then adjust as needed, where the inversion angle is 80° and the rotation speed is 40 r / min; (4) Coat a silica film on the inner surface of the glass bottle with adjusted inversion angle and rotation speed by means of high-pressure spraying of anti-reflective silica sol. The spraying pressure is 0.8 Mpa and the spraying time is 2 min. Then dry it at a low temperature of 80 °C for 10 min, and then repeat the process of coating a silica film by means of high-pressure spraying of anti-reflective silica sol. After drying at a low temperature of 80 °C for 10 min, cure it at a high temperature of 450 °C for 10 min. Example 2

[0020] (1) Use a glass bottle with a volume of 4 L. First, clean the glass bottle thoroughly. Put 20 g of ammonium sulfate and 42 g of ferrous sulfate into the bottle, perform a removal treatment on the glass surface by using a mixed de-alkalizing agent, then heat it up to 500 °C, keep it warm for 30 min, and cool it naturally; (2) Then use water, an alkali solution (mass concentration ratio of potassium hydroxide: ethylenediaminetetraacetic acid: stearic acid: deionized water is 1:0.4:0.5:12) and an acid solution (mass concentration ratio of potassium hydroxide: glycerol: citric acid: glycerol fatty acid ester: deionized water is 1:0.4:5:0.6:20) to clean the glass bottle, dry it at 100 °C for 8 min for later use; (3) Invert the glass bottle dried in step (2), determine whether the data of the inversion angle and rotation speed meet the preset conditions, and then adjust as needed, where the inversion angle is 75° and the rotation speed is 60 r / min; (4) A silica film is deposited on the inner surface of the glass bottle with the inverted angle and rotation speed adjusted by means of high-pressure spraying of weather-resistant silica sol. The spraying pressure is 0.5 Mpa, the spraying time is 4 min. Then it is dried at a low temperature of 80 °C for 10 min, and then a silica film is deposited again by repeating the method of high-pressure spraying of weather-resistant silica sol. After drying at a low temperature of 100 °C for 10 min, it is cured at a high temperature of 500 °C for 15 min. Example 3

[0021] (1) Use a glass bottle with a volume of 4 L. First, clean the glass bottle, put 10 g of ammonium sulfate and 63 g of ferrous sulfate into the bottle, and perform a removal treatment on the glass surface by using a mixed dealkalizing agent. Then heat it to 600 °C, keep it warm for 15 min, and cool it naturally. (2) Then clean the glass bottle with water, an alkali solution (the mass concentration ratio of potassium hydroxide: ethylenediaminetetraacetic acid: stearic acid: deionized water is 1:0.48:0.62:14.5) and an acid solution (the mass concentration ratio of potassium hydroxide: glycerol: citric acid: fatty acid glycerol ester, deionized water is 1:0.52:72:0.85:21.5), and dry it at 80 °C for 10 min for use. (3) Invert the glass bottle dried in step (2), judge whether the data of the inverted angle and rotation speed meet the preset conditions, and then adjust as needed. The inverted angle is 78°, and the rotation speed is 70 r / min. (4) A silica film is deposited on the inner surface of the glass bottle with the inverted angle and rotation speed adjusted by means of high-pressure spraying of antireflective silica sol. The spraying pressure is 0.9 Mpa, the spraying time is 3 min. Then it is dried at a low temperature of 110 °C for 15 min, and then a silica film is deposited again by repeating the method of high-pressure spraying of weather-resistant silica sol. After drying at a low temperature of 110 °C for 15 min, it is cured at a high temperature of 450 °C for 20 min.

[0022]

[0023] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. It should be noted that for those of ordinary skill in the art, without departing from the inventive concept of the present invention, several improvements and transformations can still be made, and these all belong to the protection scope of the present invention.

Claims

1. A method for coating the inner surface of a glass container, comprising a frosting step and a siliconization step, characterized in that: Before the siliconization treatment, the frosted glass container is inverted, and the inversion angle of the glass container is adjusted to 75-85 degrees, and the rotation speed is adjusted to 30-90 r / min.

2. The method for coating the inner surface of a glass container according to claim 1, characterized in that: The frosting step is: clean the glass container, put the de-alkali agent into the bottle, then heat it to 500-600°C, keep it warm for 10-40 minutes, cool it naturally, then clean the glass container with water, alkaline solution and acid solution, and dry it for use.

3. The method for coating the inner surface of a glass container according to claim 2, characterized in that: The dealkalizing agent includes one or both of ferrous sulfate and ammonium sulfate.

4. A method for coating the inner surface of a glass container according to claim 2 or 3, characterized in that: The dosage of the dealkalizing agent is 10-30 g / L.

5. A method for coating the inner surface of a glass container according to claim 1 or 2, characterized in that: The siliconization treatment steps are: using silica sol to plate a silica film on the inner surface of the glass container with adjusted inverted angle and rotation speed by high-pressure spraying, drying at low temperature, repeating the plating 0-6 times, and then curing at high temperature.

6. A method for coating the inner surface of a glass container according to claim 5, characterized in that: The thickness of the silicon dioxide film is 50-400 nm and is prepared by multiple spraying according to performance requirements.

7. The method for coating the inner surface of a glass container according to claim 5, characterized in that: The silica sol is one of anti-reflective silica sol, weather-resistant silica sol and wear-resistant silica sol.

8. The method for coating the inner surface of a glass container according to claim 5, characterized in that: The pressure of the high-pressure spraying is 0.3-0.9 MPa, and the spraying time is 1-5 min.

9. The method for coating the inner surface of a glass container according to claim 5, characterized in that: The drying time is 10 to 30 minutes, and the curing time is 5 to 15 minutes.

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