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CN115368023A - Etching solution, micro-flash AG effect glass and application thereof - Google Patents

Etching solution, micro-flash AG effect glass and application thereof Download PDF

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Publication number
CN115368023A
CN115368023A CN202210936225.2A CN202210936225A CN115368023A CN 115368023 A CN115368023 A CN 115368023A CN 202210936225 A CN202210936225 A CN 202210936225A CN 115368023 A CN115368023 A CN 115368023A
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glass
etching solution
flash
micro
parts
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CN115368023B (en
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吴建勇
魏中凯
张韦好
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Hefei Jinlonghao Technology Co ltd
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Hefei Jinlonghao Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00Surface treatment of glass, not in the form of fibres or filaments, by etching
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00Etching, surface-brightening or pickling compositions
    • C09K13/04Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention discloses an etching solution which comprises the following raw materials in parts by weight: 3-5 parts of ammonium bifluoride, 0.3-2.1 parts of additive, 0.8-1.8 parts of barium sulfate, 0.3-0.9 part of dispersant, 0.2-0.4 part of hydrofluoric acid, 2-3.3 parts of hydrochloric acid and 0.6-1.5 parts of water, wherein the additive is a mixture consisting of ammonium hexafluorosilicate and calcium fluosilicate. The invention also discloses a preparation method of the etching solution. The invention also discloses micro-flash AG-effect glass, which is obtained by etching the glass by using the etching solution. The invention also discloses application of the micro-flash AG effect glass. The etching solution can etch various kinds of glass, generates stable micro-flash, fine and smooth sand effect and soft hand feeling AG effect, and can meet new requirements of users; can be produced in batches and has high AG yield.

Description

Etching solution, micro-flash AG effect glass and application thereof
Technical Field
The invention relates to the technical field of etching solution, in particular to etching solution, micro-flash AG effect glass and application thereof.
Background
The AG glass is also called anti-dazzle glass, non-reflection glass or anti-reflection glass, and the like, and a glass substrate is subjected to special surface treatment, so that the glass substrate has lower reflectance compared with common glass, and the light transmission is not influenced basically. The AG glass can improve the visual angle and brightness of a display picture, so that the image is clearer, the color is more gorgeous and the color is more saturated, thereby obviously improving the display effect. Can be widely used for manufacturing liquid crystal display screens, mobile phone cover plates and the like.
At present, the glass is etched by using the etching solution, but the glass etched by the existing etching solution has high flash, coarse sand effect and rough hand feeling; moreover, the existing etching solution AG has poor stability of effect, can only be used for Corning GG5 glass, and has the phenomena of uneven etching and easy punctiform point penetration at the edge position of the etched glass for other glass materials.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the etching solution, the micro-flash AG effect glass and the application thereof, the etching solution can etch various kinds of glass, and can generate stable micro-flash, fine sand effect and soft hand feeling AG effect, and can meet new requirements of users; can be produced in batches and has high AG yield.
The invention provides an etching solution which comprises the following raw materials in parts by weight: 3-5 parts of ammonium bifluoride, 0.3-2.1 parts of additive, 0.8-1.8 parts of barium sulfate, 0.3-0.9 part of dispersant, 0.2-0.4 part of hydrofluoric acid, 2-3.3 parts of hydrochloric acid and 0.6-1.5 parts of water, wherein the additive is a mixture consisting of ammonium hexafluorosilicate and calcium fluosilicate.
Preferably, the weight ratio of ammonium hexafluorosilicate to calcium fluorosilicate is 5-15.
Preferably, the etching solution also contains borax, and the weight ratio of barium sulfate to borax is 8-18.
Preferably, the dispersing agent is starch.
Preferably, the hydrofluoric acid is a 50-55wt% aqueous hydrogen fluoride solution.
Preferably, the hydrochloric acid is 34-38wt% of hydrochloric acid aqueous solution.
Taking silicon dioxide and sodium silicate as examples, the etching mechanism of the invention is as follows:
4HF+SiO 2 =SiF 4 ↑+2H 2 O;(SiF 4 very soluble in water);
6HF+Na 2 SiO 3 =2NaF+3H 2 O+SiF 4 ↑;
SiF 4 +2NaF=Na 2 SiF 6 ↓。
elements such as Al, ca, K and the like in the glass can also react with HF to form a fluosilicate protective layer, so that the glass is prevented from further reacting to form the rugged AG effect.
The invention also provides a preparation method of the etching solution, which comprises the following steps: mixing the above materials, sealing and aging at 15-20 deg.C to obtain etching solution.
Preferably, the time for sealing and curing is more than or equal to 24 hours.
Preferably, during the curing process, the stirring is carried out once every 1 to 3 hours, and each stirring time is carried out for 5 to 15min.
The invention also provides micro-flash AG effect glass, and the micro-flash AG effect glass is obtained by etching the glass by using the etching solution.
Preferably, the micro-flash AG effect glass has a haze of 85 to 90% and a roughness of 2.0 to 2.5 μm.
Preferably, the surface of the micro-flash AG effect glass has crystals with protruding structures, and the crystals are connected with each other and uniformly distributed to form uniformly distributed concave-convex textures.
Preferably, the etched glass is at least one of king panda second generation glass, corning GG5 glass and corning GG6 glass.
The king panda second-generation glass, the corning GG5 glass and the corning GG6 glass are commercially available.
Preferably, the etching temperature is 16-25 ℃.
Preferably, the etching method is: brushing the substrate in the etching solution for 10-30s, and soaking the substrate in the etching solution for 60-110s.
And a better anti-dazzle effect can be obtained by selecting proper etching conditions.
Before etching, the glass protects the surface of glass which does not need to be etched, and the surface of the glass which needs to be etched is sequentially subjected to ultrasonic water washing, mixed acid soaking and water washing; after the glass is etched, the glass is sequentially subjected to water washing, acid liquor soaking and water washing.
The water in the invention can be tap water, purified water or deionized water and the like.
The invention also provides application of the micro-flash AG effect glass in electronic equipment.
Preferably in an electronic device housing.
Has the advantages that:
the invention selects ammonium bifluoride which is easily dissolved in cold water, the aqueous solution of the ammonium bifluoride has strong acidity and is decomposed into hydrogen fluoride and ammonia gas in hot water, and the aqueous solution of the ammonium bifluoride can react with silicon dioxide in glass at the temperature of 25-30 ℃ to generate silicon fluoride; the silicon fluoride further reacts with elements such as sodium, calcium, aluminum, potassium and the like of the glass seeds to form a fluosilicate crystal protective layer, and the glass is prevented from further reacting to form an uneven anti-dazzle effect; according to the invention, ammonium hexafluorosilicate and calcium fluosilicate are selected to be matched with each other in a proper proportion, so that the flash degree can be reduced, and the glass can keep the micro-flash AG effect; the barium sulfate or the barium sulfate and the borax are matched with each other, so that the surface roughness of the glass can be reduced in the etching process, and the AG glass has fine sand effect and soft hand feeling; the proper dispersant is selected to promote barium sulfate to be uniformly dispersed in the etching solution, so that the sand effect and the hand feeling of the AG glass are further improved; the generated crystals can be uniformly distributed and accumulated by selecting a proper amount of hydrofluoric acid, so that uniformly distributed concave-convex textures are obtained; in addition, the invention can improve the haze of the glass, improve the stability and uniformity of AG effect and avoid the phenomenon that the edge position of the glass is easy to have point-shaped transparent points through the mutual matching of all the components; the etching solution can etch various glasses (such as panda two-strength glass, corning GG6 glass, corning GG5 glass and the like), and generates a stable micro-flash AG effect, can be produced in batches, and has high AG yield; the operation is simple; the formed AG effect with micro flash, fine sand effect and soft hand feeling can meet the new requirements of users.
Drawings
FIG. 1 is a 300-fold electron microscope photograph of the surface of glass etched in example 4.
FIG. 2 is a 300-fold electron microscopic image of the surface of glass obtained by etching in comparative example 3.
Fig. 3 is a 200-fold electron microscope photograph of the surface of glass obtained by etching in comparative example 3.
FIG. 4 is a photograph showing the edge positions of glass after etching in example 4 and comparative example 3, wherein a is example 4 and b is comparative example 3.
FIG. 5 is an appearance of a glass surface after etching in example 4 and comparative example 3, wherein a is example 4 and b is comparative example 3.
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
An etching solution comprises the following raw materials in parts by weight: 4kg of ammonium bifluoride, 1kg of ammonium hexafluorosilicate, 0.4kg of calcium fluosilicate, 1.3kg of barium sulfate, 0.6kg of starch, 0.3kg of hydrofluoric acid aqueous solution with the mass fraction of 50wt%, 2.6kg of hydrochloric acid aqueous solution with the mass fraction of 38wt% and 1kg of water.
Example 2
An etching solution comprises the following raw materials in parts by weight: 3kg of ammonium bifluoride, 1.5kg of ammonium hexafluorosilicate, 0.6kg of calcium fluosilicate, 1.8kg of barium sulfate, 0.3kg of starch, 0.7kg of borax, 0.2kg of hydrofluoric acid aqueous solution with the mass fraction of 55wt%, 3.3kg of hydrochloric acid aqueous solution with the mass fraction of 34wt% and 0.6kg of water.
Example 3
An etching solution comprises the following raw materials in parts by weight: 5kg of ammonium bifluoride, 0.5kg of ammonium hexafluorosilicate, 0.2kg of calcium fluorosilicate, 0.8kg of barium sulfate, 0.9kg of starch, 0.5kg of borax, 0.4kg of a hydrofluoric acid aqueous solution with a mass fraction of 55wt%, 2kg of a hydrochloric acid aqueous solution with a mass fraction of 36wt%, and 1.5kg of water.
Example 4
The etching solution comprises the following raw materials in parts by weight: 4kg of ammonium bifluoride, 1kg of ammonium hexafluorosilicate, 0.4kg of calcium fluosilicate, 1.3kg of barium sulfate, 0.6kg of starch, 0.6kg of borax, 0.3kg of hydrofluoric acid aqueous solution with the mass fraction of 55wt%, 2.6kg of hydrochloric acid aqueous solution with the mass fraction of 36wt% and 1kg of water.
Example 5
Examples 1-4 were prepared in the same manner, including the steps of: weighing raw materials according to the weight of the formula, uniformly mixing the raw materials according to the sequence of ammonium bifluoride, ammonium hexafluorosilicate, barium sulfate, calcium fluosilicate, borax, starch, water, hydrofluoric acid and hydrochloric acid, and placing the mixture in a sealed tank body at 17 ℃ for curing for 24 hours, wherein the stirring is carried out once every 2 hours in the curing process, and the stirring is carried out for 5-15 minutes every time.
Comparative example 1
The procedure is as in example 4 except that "barium sulfate and borax" are not contained.
Comparative example 2
The procedure is as in example 4 except that "starch" is not included.
Comparative example 3
The existing commercial etching solution HHDS-02 is purchased from Zhengzhou Henhao optical science and technology Limited.
Comparative example 4
The procedure of example 4 was otherwise the same as except that ammonium hexafluorosilicate and calcium fluorosilicate were not contained.
Comparative example 5
The procedure is as in example 4 except that "ammonium hexafluorosilicate" is not included.
Comparative example 6
The procedure is as in example 4 except that "calcium fluorosilicate" is not contained.
Example 6
Corning GG6 glass is taken and etched by the etching solutions of examples 1-4 and comparative examples 1-6 respectively to prepare the micro-flash AG effect glass.
The etching method comprises the following specific steps: ultrasonically cleaning glass by using water, then soaking the glass for 60s by using mixed acid (nitric acid and hydrofluoric acid), cleaning the glass by using water, then putting the glass into an etching solution, adjusting the temperature to be 20 ℃, firstly brushing the glass for 20s, then soaking the glass for 90s, then taking out the etched glass, sequentially cleaning the glass by using water, soaking the glass in 4% sulfuric acid aqueous solution for 2min, cleaning the glass by using water, and airing the glass to obtain the micro-flash AG effect glass.
The results of examination of the micro-flash AG effect glasses prepared from the etching solutions of examples 1 to 4 and comparative examples 1 to 6 are shown in Table 1 and FIGS. 1 to 5.
FIG. 1 is a 300-fold electron micrograph of a glass surface obtained by etching in example 4.
FIG. 2 is a 300-fold electron microscopic image of the surface of glass obtained by etching in comparative example 3.
FIG. 3 is a 200-fold electron microscopic photograph of the surface of glass obtained by etching in comparative example 3.
As can be seen from fig. 1-2: the surface of the micro-flash AG effect glass obtained by using the etching solution in the embodiment 4 is provided with crystals, the crystals have a protruding structure, the crystals are connected with each other and uniformly distributed to form uniformly distributed concave-convex textures, the crystals are small, so that the hand feeling is softer, and no leakage point exists on the surface of the glass; whereas the glass surface obtained using the etching solution of comparative example 3 had large crystals and numerous leak points (circled in fig. 2).
As can be seen from FIG. 3, the crystal spacing of the glass surface obtained using the etching solution of comparative example 3 was large and the distribution was not uniform.
FIG. 4 is a photograph showing the edge positions of glass after etching in example 4 and comparative example 3, wherein a is example 4 and b is comparative example 3.
FIG. 5 is an appearance of the glass surface after etching in example 4 and comparative example 3, wherein a is example 4 and b is comparative example 3.
As can be seen from FIG. 4, the AG effect of the invention is stable and uniform, and the edge of the glass has no point penetration phenomenon under the premise of the same light source, the same height and the same shooting angle; in contrast, in comparative example 3, the AG effect is unstable due to the point-like penetration phenomenon (circled part in fig. 4 b) at the edge of the glass.
As can be seen from fig. 5, on the premise of the same light source, the same height and the same shooting angle, the haze of example 4 is significantly better than that of comparative example 3, and the brightness is lower than that of comparative example 3 after etching.
TABLE 1 test results
Figure BDA0003783405920000071
Remarking: detecting the haze and the light transmittance by using a special haze meter; roughness was measured using a roughness instrument; the flash detection method comprises the following steps: the brightness of the glass was observed under the same lighting conditions and compared with comparative example 3.
As can be seen from table 1: the AG effect of the etched glass of examples 1-4 is characterized by high haze, low sparkle, and soft hand.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (10)

1. The etching solution is characterized by comprising the following raw materials in parts by weight: 3-5 parts of ammonium bifluoride, 0.3-2.1 parts of additive, 0.8-1.8 parts of barium sulfate, 0.3-0.9 part of dispersant, 0.2-0.4 part of hydrofluoric acid, 2-3.3 parts of hydrochloric acid and 0.6-1.5 parts of water, wherein the additive is a mixture consisting of ammonium hexafluorosilicate and calcium fluosilicate.
2. The etching solution of claim 1, wherein the weight ratio of ammonium hexafluorosilicate to calcium fluorosilicate is 5-15.
3. The etching solution according to claim 1 or 2, wherein the etching solution further comprises borax, and the weight ratio of barium sulfate to borax is 8-18; preferably, the dispersing agent is starch.
4. The etching solution according to any one of claims 1 to 3, wherein the hydrofluoric acid is an aqueous hydrogen fluoride solution having a mass fraction of 50 to 55 wt%; preferably, the hydrochloric acid is 34-38wt% of hydrochloric acid aqueous solution.
5. A method for preparing an etching solution according to any one of claims 1 to 4, comprising the steps of: mixing the raw materials, sealing and curing at 15-20 deg.C to obtain etching solution; preferably, the time for sealing and curing is more than or equal to 24 hours; preferably, during the curing process, the mixture is stirred for 5-15min every 1-3 h.
6. A micro-flash AG effect glass, which is characterized in that the micro-flash AG effect glass is obtained by etching the glass by using the etching solution of any one of claims 1 to 4.
7. The antiglare AG effect glass of claim 6, wherein the antiglare AG effect glass has a haze of 85 to 90% and a roughness of 2.0 to 2.5 μm.
8. The micro-flash AG effect glass of claim 6 or 7, wherein the surface of the micro-flash AG effect glass has crystalline bodies with a protruding structure, and the crystalline bodies are connected with each other and uniformly distributed to form uniformly distributed concave-convex textures.
9. The micro-flash AG effect glass of any one of claims 6 to 8, wherein the etched glass is at least one of a king panda second generation glass, a Corning GG5 glass, a Corning GG6 glass; preferably, the etching temperature is 16-25 ℃; preferably, the etching method is: brushing in the etching solution for 10-30s, and soaking for 60-110s.
10. Use of a micro-flash AG effect glass according to any one of claims 6-9 in an electronic device; preferably in an electronic device housing.
CN202210936225.2A 2022-08-05 2022-08-05 Etching solution, micro-flash AG effect glass and application thereof Active CN115368023B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432185A (en) * 2011-09-30 2012-05-02 郑州恒昊玻璃技术有限公司 Anti-dazzle glass product etching solution and etching process
CN110563341A (en) * 2019-09-29 2019-12-13 宜昌南玻显示器件有限公司 High-alumina glass frosting liquid and preparation method thereof
CN111362584A (en) * 2020-03-21 2020-07-03 郑州恒昊光学科技有限公司 High borosilicate glass etching solution and preparation method and application thereof
CN112851132A (en) * 2019-11-28 2021-05-28 比亚迪股份有限公司 Etching solution for glass gradual-change frosting and preparation method and application thereof
CN114349360A (en) * 2022-02-23 2022-04-15 Oppo广东移动通信有限公司 Method for preparing glass substrate, glass substrate, housing assembly, and electronic device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432185A (en) * 2011-09-30 2012-05-02 郑州恒昊玻璃技术有限公司 Anti-dazzle glass product etching solution and etching process
CN110563341A (en) * 2019-09-29 2019-12-13 宜昌南玻显示器件有限公司 High-alumina glass frosting liquid and preparation method thereof
CN112851132A (en) * 2019-11-28 2021-05-28 比亚迪股份有限公司 Etching solution for glass gradual-change frosting and preparation method and application thereof
CN111362584A (en) * 2020-03-21 2020-07-03 郑州恒昊光学科技有限公司 High borosilicate glass etching solution and preparation method and application thereof
CN114349360A (en) * 2022-02-23 2022-04-15 Oppo广东移动通信有限公司 Method for preparing glass substrate, glass substrate, housing assembly, and electronic device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王琦: "《无机非金属材料工艺学》", 北京:中国建材工业出版社 *

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