CN117228960A - Anti-dazzle treatment method for high-alumina glass - Google Patents

Anti-dazzle treatment method for high-alumina glass Download PDF

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Publication number
CN117228960A
CN117228960A CN202311342899.0A CN202311342899A CN117228960A CN 117228960 A CN117228960 A CN 117228960A CN 202311342899 A CN202311342899 A CN 202311342899A CN 117228960 A CN117228960 A CN 117228960A
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glass
treatment method
distilled water
etching
dazzle
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CN202311342899.0A
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王立成
张现峰
郭春燕
王鹏飞
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Anhui Yindong Optical Technology Co ltd
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Anhui Yindong Optical Technology Co ltd
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Abstract

The invention discloses an anti-dazzle treatment method of high-alumina glass, which relates to the technical field of anti-dazzle glass, and the treatment method provided by the invention not only can enable the high-alumina glass to have an anti-dazzle function, but also can enable the prepared anti-dazzle glass to have the characteristics of high transmittance, low roughness and high glossiness; and optical parameters such as roughness, glossiness and the like of the anti-dazzle glass can be adjusted by adjusting etching time and polishing time according to different user requirements.

Description

Anti-dazzle treatment method for high-alumina glass
Technical field:
the invention relates to the technical field of anti-dazzle glass, in particular to an anti-dazzle treatment method of high-alumina glass.
The background technology is as follows:
the antiglare glass (AG glass for short) is a glass in which the surface of the glass is subjected to a special chemical treatment to make the surface of the original glass a matte diffuse reflection surface. The AG glass is characterized in that the single-sided or double-sided of the high-quality glass is subjected to process treatment, so that the AG glass has lower reflectance compared with the common glass, the interference of ambient light is reduced, the definition of pictures is improved, the reflection of a screen is reduced, clear and transparent visual effect is created, and consumers have better visual experience. The high-alumina glass has the advantages of excellent mechanical property, good chemical stability, high transmittance, strong scratch resistance, impact resistance, crack resistance, strong dropping capability and the like due to high alumina content, and has wide application market in the fields of mobile phone display screens, tablet computers, outdoor information display cards, plasma displays, large glass showcases and the like after anti-dazzle treatment.
At present, 3 mature anti-dazzle glass treatment methods are available: sticking film, spraying and etching. The AG film-adhered glass has poor weather resistance and wear resistance, and is easy to fall off a film layer; and the hardness of the surface film of the glass is not high, and serious surface scratch can occur after the glass is used for a period of time. The AG spraying glass is also poor in weather resistance and wear resistance, is not suitable for being used on the glass with frequent touching and sliding, and is easy to cause the problems of screen pattern caused by coating falling and fat dissolution. The chemical etching method is simple, easy to operate and suitable for large-area glass etching and large-scale production. In the AG glass production process, factors such as chemical composition, etching time and etching temperature of etching liquid can influence the surface roughness and glossiness of glass after etching, so that the practical use value of the product is related. Aiming at the advantages and disadvantages of the AG glass processing method, the research on the AG glass processing method of the high-aluminum material has very important significance.
The invention comprises the following steps:
the invention aims to solve the technical problem of providing an anti-dazzle treatment method for high-alumina glass, which realizes the anti-dazzle treatment on the high-alumina glass through conventional pretreatment, etching, polishing and cleaning processes, so that the prepared anti-dazzle glass has the characteristics of high transmittance, low roughness and high glossiness.
The technical problems to be solved by the invention are realized by adopting the following technical scheme:
an anti-dazzle treatment method for high alumina glass comprises the following steps:
(1) Pretreatment: cleaning the high-alumina glass;
(2) Etching: placing the prepared etching solution in an etching groove, adhering a protective film on one surface of the high-alumina glass which is not required to be etched, and then soaking the surface in the etching solution;
(3) Polishing: washing the etched high-alumina glass with distilled water, and then putting the high-alumina glass into polishing solution for chemical polishing;
(4) Cleaning: and washing the polished high-alumina glass with distilled water, cleaning liquid and distilled water in sequence, tearing off the protective film, and drying to constant weight to obtain the anti-dazzle glass.
The cleaning comprises sequentially performing organic solvent soaking, distilled water washing, acid liquor soaking and distilled water washing. Through cleaning, the influence of oil stains and dust on the surface of glass in the processing and transportation processes on the subsequent treatment process is reduced to the greatest extent. The soaking may be performed under ultrasound.
Preferably, the organic solvent is absolute ethanol or acetone.
Preferably, the acid liquor is dilute sulfuric acid, and the mass concentration is 1-3%.
The etching solution is obtained by mixing a component A and a component B in a mass ratio of 1:2 and adding nitric acid to adjust the pH value to 2-3; wherein the component A is formed by mixing (by mass ratio) ammonium bifluoride, potassium fluoride, barium sulfate, potassium nitrate, zinc acetate and oxalic acid, wherein the mass ratio of (50-100), (10-15), (3-5), (15-25), (10-30) and (5-10); the component B is prepared by mixing (by mass ratio) surfactant (1-3), sodium carboxymethyl starch, emulsifier, dispersant, pH regulator and distilled water (2-5), 5-10, 10-20 and 400-600).
The protective film may be selected from protective films commonly used in the art, preferably polyethylene films.
The surfactant may be selected from surfactants commonly used in the art including, but not limited to, cetyltrimethylammonium bromide.
The emulsifier may be selected from emulsifiers commonly used in the art including, but not limited to, polyoxyethylene lauryl ether, polyoxyethylene allyloxy ether.
The dispersant may be selected from dispersants commonly used in the art including, but not limited to, polyvinyl alcohol.
The pH adjustor can be selected from pH adjusters commonly used in the art including, but not limited to, sodium hexametaphosphate, sodium tripolyphosphate.
The etching temperature is 25 ℃ and the etching time is 2-10 min.
The polishing solution is formed by mixing hydrofluoric acid and sulfuric acid, the mass concentration of the hydrofluoric acid is 5-10%, and the mass concentration of the sulfuric acid is 10-20%.
The polishing time is 30-120 s.
And the water column of distilled water and cleaning liquid is 45-60 degrees with the surface of the glass during flushing.
The cleaning liquid comprises the following components: 5 to 10g/L of sodium hydroxide, 5 to 10g/L of anhydrous sodium carbonate, 1 to 3g/L of sodium citrate, 1 to 3g/L of citric acid, 0.5 to 1g/L of ethylenediamine tetramethylene phosphonic acid, 0.2 to 0.5g/L of sodium dodecyl sulfate, 0.2 to 0.5g/L of ethylene glycol and 0.1 to 0.3g/L of tributyl phosphate.
The surface roughness of the anti-dazzle glass is 0.05-0.1 mu m, and the 60-DEG glossiness is 110-120.
The beneficial effects of the invention are as follows:
1. the method directly and effectively etches the glass by utilizing hydrofluoric acid generated by the reaction of the fluoride and the nitric acid, avoids directly using the hydrofluoric acid with strong corrosiveness, and improves the process safety.
2. The high-alumina glass is washed by the cleaning solution after being etched, and compared with the washing by directly using distilled water, the anti-dazzle glass obtained by the method has cleaner surface.
3. The processing method provided by the invention not only can enable the high-alumina glass to have an anti-dazzle function, but also can enable the prepared anti-dazzle glass to have the characteristics of high transmittance, low roughness and high glossiness; and optical parameters such as roughness, glossiness and the like of the anti-dazzle glass can be adjusted by adjusting etching time and polishing time according to different user requirements.
The specific embodiment is as follows:
the invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
The alumina glass used in the following examples and comparative examples is the same type of alumina glass from the same batch of the same manufacturer; the polyvinyl alcohol used was polyvinyl alcohol 1799.
Examples 1 to 3
(1) Pretreatment: the high-alumina glass is sequentially soaked in absolute ethyl alcohol, washed by distilled water, soaked in dilute sulfuric acid (the mass concentration is 3%) and washed by distilled water.
(2) Etching: placing the prepared etching solution into an etching groove, adhering a polyethylene film on one surface of the high-alumina glass which is not required to be etched, and then soaking the surface in the etching solution, wherein the etching temperature is 25 ℃, and the etching time is 8min. The etching solution is prepared by mixing a component A and a component B in a mass ratio of 1:2, adding nitric acid to adjust the pH value to 2-3, wherein the component A is prepared by mixing ammonium bifluoride, potassium fluoride, barium sulfate, potassium nitrate, zinc acetate and oxalic acid in a mass ratio of (50-100) 12:4:20:20:5, and the component B is prepared by mixing cetyltrimethylammonium bromide, sodium carboxymethyl starch, polyoxyethylene lauryl ether, polyvinyl alcohol, sodium hexametaphosphate and distilled water in a mass ratio of 1:2.5:5:15:500.
(3) Polishing: and (3) washing the etched high-alumina glass with distilled water, and then placing the high-alumina glass into a polishing solution for chemical polishing, wherein the polishing solution is formed by mixing hydrofluoric acid and sulfuric acid, the mass concentration of the hydrofluoric acid is 5%, the mass concentration of the sulfuric acid is 10%, and the polishing time is 60s.
(4) Cleaning: and (3) washing the polished high-alumina glass with distilled water, cleaning liquid and distilled water in sequence, wherein the water column of the distilled water and the cleaning liquid is 60 degrees with the surface of the glass during washing, tearing off the protective film, and drying to constant weight to obtain the anti-dazzle glass. Wherein the cleaning liquid comprises the following components: 6.75g/L of sodium hydroxide, 8.5g/L of anhydrous sodium carbonate, 1g/L of sodium citrate, 1.25g/L of citric acid, 1g/L of ethylenediamine tetramethylene phosphonic acid, 0.25g/L of sodium dodecyl sulfate, 0.25g/L of ethylene glycol and 0.15g/L of tributyl phosphate.
Examples 1-3 were obtained by adjusting the ammonium bifluoride content in the etching solution. Specifically, the mass content of ammonium bifluoride in the etching solution used in example 1 was 5%, the mass content of ammonium bifluoride in the etching solution used in example 2 was 6%, and the mass content of ammonium bifluoride in the etching solution used in example 3 was 7%.
Comparative example 1
Comparative example 1 differs from examples 1 to 3 only in that the mass content of ammonium bifluoride in the etching liquid was adjusted to 9%.
The high alumina glasses treated with the antiglare treatments of examples 1 to 3 and comparative example 1 were each subjected to roughness and glossiness measurement, and the results are shown in table 1.
TABLE 1
Ammonium bifluoride content/% Roughness/. Mu.m Gloss value
Example 1 5 0.08 115
Example 2 6 0.08 110
Example 3 7 0.06 113
Comparative example 1 9 0.15 127
As can be seen from Table 1, NH is present in the etchant 4 HF 2 The content is increased from 5% to 7%, NH in the etching liquid 4 + Concentration is continuously increased, NH 4 + And SiF generated in etching liquid 6 2+ Can form a more soluble (NH) 4 ) 2 SiF 6 Resulting in smaller crystallite particles on the glass surface. At the same time prevent indissoluble K 2 SiF 6 The number of large-sized microcrystals is reduced. Therefore, the surface roughness of the glass is reduced, and at the same time, more uniform small bulges are formed, the light reflectance is reduced, and the glossiness value is reduced. When NH 4 HF 2 When the content was further increased to 9%, it was found that a layer of white substance was generated on the surface of the glass, the transmittance of the glass was decreased, the surface roughness was increased, and the change in the gloss value of the glass surface was large.
Examples 4 to 5
(1) Pretreatment: the high-alumina glass is sequentially soaked in absolute ethyl alcohol, washed by distilled water, soaked in dilute sulfuric acid (the mass concentration is 3%) and washed by distilled water.
(2) Etching: placing the prepared etching solution into an etching groove, adhering a polyethylene film on one surface of the high-alumina glass which is not required to be etched, and then soaking the surface in the etching solution, wherein the etching temperature is 25 ℃, and the etching time is 8min. The etching solution is prepared by mixing a component A and a component B in a mass ratio of 1:2, adding nitric acid to adjust the pH value to 2-3, wherein the component A is prepared by mixing ammonium bifluoride, potassium fluoride, barium sulfate, potassium nitrate, zinc acetate and oxalic acid in a mass ratio of 80:12:4:20 (10-30:5), and the component B is prepared by mixing cetyltrimethylammonium bromide, sodium carboxymethyl starch, polyoxyethylene laurate, polyvinyl alcohol, sodium hexametaphosphate and distilled water in a mass ratio of 1:2.5:5:15:500.
(3) Polishing: and (3) washing the etched high-alumina glass with distilled water, and then placing the high-alumina glass into a polishing solution for chemical polishing, wherein the polishing solution is formed by mixing hydrofluoric acid and sulfuric acid, the mass concentration of the hydrofluoric acid is 5%, the mass concentration of the sulfuric acid is 10%, and the polishing time is 60s.
(4) Cleaning: and (3) washing the polished high-alumina glass with distilled water, cleaning liquid and distilled water in sequence, wherein the water column of the distilled water and the cleaning liquid is 60 degrees with the surface of the glass during washing, tearing off the protective film, and drying to constant weight to obtain the anti-dazzle glass. Wherein the cleaning liquid comprises the following components: 6.75g/L of sodium hydroxide, 8.5g/L of anhydrous sodium carbonate, 1g/L of sodium citrate, 1.25g/L of citric acid, 1g/L of ethylenediamine tetramethylene phosphonic acid, 0.25g/L of sodium dodecyl sulfate, 0.25g/L of ethylene glycol and 0.15g/L of tributyl phosphate.
Examples 4 to 5 were obtained by adjusting the zinc acetate content in the etching solution. Specifically, the mass content of zinc acetate in the etching solution used in example 4 was 1%, and the mass content of zinc acetate in the etching solution used in example 5 was 2%.
Comparative examples 2 to 3
Comparative examples 2 to 3 differ from examples 4 to 5 only in that the mass content of zinc acetate in the etching solution was adjusted to 3% and 5%, respectively.
The high alumina glasses treated with the antiglare treatments of examples 4 to 5 and comparative examples 2 to 3 described above were respectively subjected to roughness and glossiness measurement, and the results are shown in table 2.
TABLE 2
Zinc acetate content/% Roughness/. Mu.m Gloss value
Example 4 1 0.08 115
Implementation of the embodimentsExample 5 2 0.06 108
Comparative example 2 3 0.10 120
Comparative example 3 5 0.12 129
As can be seen from table 2, as the zinc acetate content in the etching solution increases, the roughness of the glass tends to decrease and then increase. When the zinc acetate content reaches 2%, the roughness of the glass is the lowest; however, when the zinc acetate content exceeds 2%, the roughness of the glass increases with the increase in the content. Zinc acetate can also be mixed with SiF in etching solution 6 2+ Reacting to generate soluble ZnSiF 6 ,ZnSiF 6 Immediately after generation, the glass is dissolved, and the particle size of the fine particles on the etched glass surface becomes small, so that the surface roughness becomes small.
In order to further optimize the anti-glare treatment effect, the invention also prepares the glyceryl ether modified polyvinyl alcohol to replace the polyvinyl alcohol as a dispersing agent. Therefore, the roughness can be further reduced without increasing the dosage of the polyvinyl alcohol, and meanwhile, the glossiness is not influenced.
The dispersing agent is glycerol ether modified polyvinyl alcohol, and the preparation method thereof comprises the following steps: adding polyvinyl alcohol and anhydrous aluminum trichloride into glycidyl ether, heating to 120 ℃ for heat preservation reaction, stopping the reaction when the hydroxyl content in a reaction system is not changed, filtering while the reaction system is hot, and naturally cooling filtrate to obtain the glycerol ether modified polyvinyl alcohol. The mass ratio of the polyvinyl alcohol to the glycidyl ether to the anhydrous aluminum trichloride is 1:1:0.05.
Glycidyl ether CAS:13236-02-7.
Example 6
Example 6 differs from example 3 only in that the polyvinyl alcohol is replaced by the same amount of glycerol ether modified polyvinyl alcohol.
The high alumina glass treated with the antiglare treatment of example 6 was subjected to roughness and glossiness measurement, and the results are shown in table 3.
TABLE 3 Table 3
As can be seen from table 3, when the glyceryl ether modified polyvinyl alcohol is used instead of polyvinyl alcohol as the dispersing agent, the surface roughness of the high-alumina glass can be reduced from 0.06 to 0.05, while the change value of the roughness is only 0.01, the change rate of the roughness reaches 16.67%, and the dispersing agent is very little in the etching solution, so that the invention can realize substantial improvement of the surface roughness of the high-alumina glass under the condition of not increasing the consumption of the dispersing agent; and the surface glossiness of the high-alumina glass is not affected by adopting the glyceryl ether modified polyvinyl alcohol as a dispersing agent instead of the polyvinyl alcohol.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. An anti-dazzle treatment method for high-alumina glass is characterized by comprising the following steps:
(1) Pretreatment: cleaning the high-alumina glass;
(2) Etching: placing the prepared etching solution in an etching groove, adhering a protective film on one surface of the high-alumina glass which is not required to be etched, and then soaking the surface in the etching solution;
(3) Polishing: washing the etched high-alumina glass with distilled water, and then putting the high-alumina glass into polishing solution for chemical polishing;
(4) Cleaning: and washing the polished high-alumina glass with distilled water, cleaning liquid and distilled water in sequence, tearing off the protective film, and drying to constant weight to obtain the anti-dazzle glass.
2. The antiglare treatment method according to claim 1, wherein: the cleaning comprises sequentially performing organic solvent soaking, distilled water washing, acid liquor soaking and distilled water washing.
3. The antiglare treatment method according to claim 1, wherein: the etching solution is obtained by mixing a component A and a component B in a mass ratio of 1:2 and adding nitric acid to adjust the pH value to 2-3; wherein the component A is formed by mixing (by mass ratio) ammonium bifluoride, potassium fluoride, barium sulfate, potassium nitrate, zinc acetate and oxalic acid, wherein the mass ratio of (50-100), (10-15), (3-5), (15-25), (10-30) and (5-10); the component B is prepared by mixing (by mass ratio) surfactant (1-3), sodium carboxymethyl starch, emulsifier, dispersant, pH regulator and distilled water (2-5), 5-10, 10-20 and 400-600).
4. The antiglare treatment method according to claim 1, wherein: the protective film is a polyethylene film.
5. The antiglare treatment method according to claim 1, wherein: the etching temperature is 25 ℃ and the etching time is 2-10 min.
6. The antiglare treatment method according to claim 1, wherein: the polishing solution is formed by mixing hydrofluoric acid and sulfuric acid, the mass concentration of the hydrofluoric acid is 5-10%, and the mass concentration of the sulfuric acid is 10-20%.
7. The antiglare treatment method according to claim 1, wherein: the polishing time is 30-120 s.
8. The antiglare treatment method according to claim 1, wherein: and the water column of distilled water and cleaning liquid is 45-60 degrees with the surface of the glass during flushing.
9. The antiglare treatment method according to claim 1, wherein: the cleaning liquid comprises the following components: 5 to 10g/L of sodium hydroxide, 5 to 10g/L of anhydrous sodium carbonate, 1 to 3g/L of sodium citrate, 1 to 3g/L of citric acid, 0.5 to 1g/L of ethylenediamine tetramethylene phosphonic acid, 0.2 to 0.5g/L of sodium dodecyl sulfate, 0.2 to 0.5g/L of ethylene glycol and 0.1 to 0.3g/L of tributyl phosphate.
10. The antiglare treatment method according to claim 1, wherein: the surface roughness of the anti-dazzle glass is 0.05-0.1 mu m, and the 60-DEG glossiness is 110-120.
CN202311342899.0A 2023-10-17 2023-10-17 Anti-dazzle treatment method for high-alumina glass Pending CN117228960A (en)

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