CN108585530A - A kind of glass etching liquid and preparation method thereof - Google Patents
A kind of glass etching liquid and preparation method thereof Download PDFInfo
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- CN108585530A CN108585530A CN201810359967.7A CN201810359967A CN108585530A CN 108585530 A CN108585530 A CN 108585530A CN 201810359967 A CN201810359967 A CN 201810359967A CN 108585530 A CN108585530 A CN 108585530A
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- etching liquid
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses a kind of glass etching liquids and preparation method thereof, and according to the mass fraction, the glass etching liquid includes following components：0 30 parts of phosphatase 11,10 40 parts of nitric acid, 10 20 parts of sulfuric acid, 5 20 parts of hydrochloric acid, 5 15 parts of ammonium acid fluoride, 26 parts of nano fluoride, 2 10 parts of surfactant, 15 parts of potassium bichromate, 5 10 parts of polyvinylpyrrolidone, 0 50 parts of water.The present invention does not use hydrofluoric acid, greatly reduces the toxicity of etching solution, is good for the environment；The etching solution of the present invention is more safe and reliable in actual production and operating process, and the etching solution of the present invention can recycle after filtration, and etch-rate is highly stable, and etching quality is good, and yields is up to 96% or more.
Description
Technical field
The present invention relates to glass thinning technical fields, and in particular to a kind of glass etching liquid and preparation method thereof.
Background technology
In recent years, it is required for using liquid crystal display on smart mobile phone, tablet computer, laptop and ultra-thin television
Screen, and liquid crystal display is between liquid crystal is maintained at glass, manufacturer wish further to mitigate the thickness of display device and
Weight, may require that processing after glass substrate have very thin thickness, thickness usually only 0.4mm~0.6mm of touch screen, by
In the limitation of glass substrate production technology, the glass substrate produced is thicker.In order to achieve the purpose that make glass substrate thinning, glass
Glass substrate is etched into as important problem.
Etching solution on existing market is very fast to the etch-rate of glass substrate, and etch quantity is not easily controlled, cannot be fine
Substrate thickness is controlled, what is had can not effectively dissolve silicate, and some will produce stronger ionization, generate excessive
Hydrofluoric acid, etch-rate can be caused not easy to control, etching solution will produce a large amount of bubbles sometimes, reduce etch-rate.
It is therefore desirable to be able to more precisely, efficiently grinding or etching glass substrate lapping liquid or etching solution, can have
Effect removal is attached to the impurity of glass baseplate surface, to improve product qualification rate and yields, while can be to glass substrate
The control of thickness provides accurate ensure.
In addition, usually contain hydrofluoric acid in existing frequently-used etching solution, lead to that there is some negative issues, such as glass
It is reacted with hydrofluoric acid, fluosilicic acid can be generated, with the progress of reaction, fluosilicic acid concentration increases in etching solution, is more than that fluosilicic acid is molten
After solution degree critical point, fluosilicic acid white crystals, meeting isolation glass and hydrofluoric acid are formed in glass edge, influences to crystallize region
The progress of etching process, and then cause different zones glass etching degree inconsistent, influence product final performance.And etching solution
Etch-rate it is unstable and utilization rate is relatively low.Furthermore fluosilicic acid crystalline solid can influence appearance with the increase of volume, and
Conventional cleaning can not be disposed, including common acidity, alkalinity, neutral cleaning solution, alcohol wipe etc. can not clean fluorine
Silicic acid.And hydrofluoric acid is a kind of strong acid of high harm, also known as " rotten bone acid ", and the hydrofluoric acid of high concentration has intense stimulus to skin
Property and corrosivity, can causing death, the hydrofluoric acid after use is difficult to handle, and is easy pollution environment.
Invention content
In view of the problems of the existing technology, the present invention provides a kind of glass etching liquids and preparation method thereof.
The present invention uses following technical scheme：
A kind of glass etching liquid, according to the mass fraction, including following components：
Preferably, according to the mass fraction, the glass etching liquid is composed of the following components：0-30 parts of phosphatase 11, nitric acid 10-
40 parts, 10-20 parts of sulfuric acid, 5-20 parts of hydrochloric acid, 5-15 parts of ammonium acid fluoride, 2-6 parts of nano fluoride, 2-10 parts of surfactant,
1-5 parts of potassium bichromate, 5-10 parts of polyvinylpyrrolidone, 0-50 parts of water.Optionally, the glass etching liquid is by following components group
At：5-30 parts of phosphatase 11,15-30 parts of nitric acid, 15-20 parts of sulfuric acid, 10-20 parts of hydrochloric acid, 5-10 parts of ammonium acid fluoride, nano fluoride
2-6 parts, 2-8 parts of surfactant, 1-5 parts of potassium bichromate, 5-10 parts of polyvinylpyrrolidone, 5-30 parts of water.
Further, the H in the phosphoric acid3PO4Mass percentage be 10~30%；HNO in the nitric acid3's
Mass percentage is 10~40%；H in the sulfuric acid2SO4Mass percentage be 10~30%；In the hydrochloric acid
The mass percentage of HCl is 10~30%.
It is further preferred that the HNO in the nitric acid3Mass ratio with the HCl in hydrochloric acid is 5~8.
Further, the nano fluoride is nano calcium fluoride and/or nanometer sodium fluoride.
It is further preferred that the grain size of the nano fluoride is 5-100nm.
Further, the surfactant is nonionic surfactant and anion surfactant.
It is further preferred that the mass ratio of the nonionic surfactant and anion surfactant is 1：0.5~
2。
It is further preferred that the nonionic surfactant is octyl phenol polyoxyethylene ether and/or polyoxyethylene nonyl phenyl second
Alkene ether.
It is further preferred that the anion surfactant be lauryl sodium sulfate, neopelex and
At least one of dioctyl succinate disulfonate acid.
A kind of preparation method of glass etching liquid, includes the following steps：
(1) reaction is added in water, phosphoric acid, nitric acid, sulfuric acid, hydrochloric acid, ammonium acid fluoride, potassium bichromate, polyvinylpyrrolidone
It is stirred evenly in device, obtains component A；
(2) nano fluoride, surfactant are added in reactor and are stirred evenly, obtain B component；
(3) B component is added in component A, stirs evenly and can be obtained the glass etching liquid.
Further, the stir speed (S.S.) in step (1) is 100-500 revs/min；Stir speed (S.S.) in step (2) is 500-
2000 revs/min；Stir speed (S.S.) in step (3) is 100-1000 revs/min.
Beneficial effects of the present invention：
(1) present invention does not use hydrofluoric acid, greatly reduces the toxicity of etching solution, is good for the environment；
(2) etching solution of the invention is more safe and reliable in actual production and operating process, and the erosion of the present invention
Carving liquid can recycle after filtration；
(3) etching solution etch-rate of the invention is highly stable, and etching quality is good, and to glass baseplate, good damage is hindered invariably, good
Product rate is up to 96% or more.
Specific implementation mode
In order to preferably explain the present invention, it is described further in conjunction with following specific examples, but the present invention is unlimited
In specific embodiment.
Embodiment 1
A kind of glass etching liquid, according to the mass fraction, including following components：
H in the phosphoric acid3PO4Mass percentage be 20%；HNO in the nitric acid3Mass percentage be
30%；H in the sulfuric acid2SO4Mass percentage be 20%；The mass percentage of HCl in the hydrochloric acid is
15%.
The grain size of the nano calcium fluoride is 5-30nm.
The surfactant is octyl phenol polyoxyethylene ether and lauryl sodium sulfate.
Embodiment 2
A kind of glass etching liquid, according to the mass fraction, including following components：
H in the phosphoric acid3PO4Mass percentage be 15%；HNO in the nitric acid3Mass percentage be
15%；H in the sulfuric acid2SO4Mass percentage be 15%；The mass percentage of HCl in the hydrochloric acid is
15%.
The grain size of the nano calcium fluoride is 10-50nm.
The surfactant is octyl phenol polyoxyethylene ether and lauryl sodium sulfate.
Embodiment 3
A kind of glass etching liquid, according to the mass fraction, including following components：
H in the phosphoric acid3PO4Mass percentage be 20%；HNO in the nitric acid3Mass percentage be
30%；H in the sulfuric acid2SO4Mass percentage be 30%；The mass percentage of HCl in the hydrochloric acid is
20%.
The grain size of the nano calcium fluoride is 30-70nm.
The surfactant is nonylphenol polyoxyethylene ether and dioctyl succinate disulfonate acid.
Comparative example 1
For this comparative example 1 other than being free of nano calcium fluoride in ingredient, remaining place is same as Example 1.
Comparative example 2
This comparative example 2 is same as Example 1, in addition to calcirm-fluoride (calcirm-fluoride of common grain size, grain size be more than 10 microns)
It substitutes other than nano calcium fluoride.
Comparative example 3
For this comparative example 3 other than being free of surfactant in ingredient, remaining place is same as Example 1.
Comparative example 4
For this comparative example 4 other than being free of nitric acid, potassium bichromate and polyvinylpyrrolidone in ingredient, remaining is local and real
It is identical to apply example 1.
Comparative example 5
This comparative example 5 in addition in ingredient ammonium acid fluoride account for 3 parts, nano calcium fluoride account for 1 part, surfactant account for 1 part, weight chromium
Sour potassium account for 0.5 part, polyvinylpyrrolidone account for other than 3 parts, remaining place it is all same as Example 1.
Product effect assessment：
Embodiment 1 and the etching solution of comparative example 1-5 are carried out practical etching to produce, temperature control is 25-30 DEG C.
Glass is put into the glass etching liquid obtained in embodiment 1, in total 1000 products of etching, fraction defective 2%,
Yields is 98%.Mean etch rate is about 12 [mus, and etch-rate is very stable, the thickness evenness ＜ after etching
1%.
Glass is put into the glass etching liquid obtained in comparative example 1, in total 20 products of etching, fraction defective 20%,
Yields is 80%.Mean etch rate is about 4 [mus, and etch-rate is unstable, and the thickness evenness after etching is about
9%.
Glass is put into the glass etching liquid obtained in comparative example 2, in total 20 products of etching, fraction defective 20%,
Yields is 80%.Mean etch rate is about 5 [mus, and etch-rate is unstable, and the thickness evenness after etching is about
6%.
Glass is put into the glass etching liquid obtained in comparative example 3, in total 20 products of etching, fraction defective 15%,
Yields is 85%.Mean etch rate is about 6 [mus, and etch-rate is unstable, and the thickness evenness after etching is about
7%.
Glass is put into the glass etching liquid obtained in comparative example 4, in total 20 products of etching, fraction defective 15%,
Yields is 85%.Mean etch rate is about 5 [mus, and etch-rate is unstable, and the thickness evenness after etching is about
7%.
Glass is put into the glass etching liquid obtained in comparative example 5, in total 20 products of etching, fraction defective 10%,
Yields is 90%.Mean etch rate is about 6 [mus, and etch-rate is relatively stablized, and the thickness evenness after etching is about
4%.
As it can be seen that the etching solution of the present invention can still keep higher yields and etching under higher etch-rate
Uniformity.The quality of product can be improved, and greatly saves production time and cost.
Above is only a specific embodiment of the present invention, it is not intended to limit the scope of the invention, every utilization
The equivalent transformation that the present invention makees is applied directly or indirectly in other relevant technical fields, is similarly included in the present invention's
Among scope of patent protection.
Claims (10)
1. a kind of glass etching liquid, which is characterized in that according to the mass fraction, including following components：
2. glass etching liquid according to claim 1, which is characterized in that the H in the phosphoric acid3PO4Mass percentage
It is 10~30%；HNO in the nitric acid3Mass percentage be 10~40%；H in the sulfuric acid2SO4Quality hundred
It is 10~30% to divide content；The mass percentage of HCl in the hydrochloric acid is 10~30%.
3. glass etching liquid according to claim 2, which is characterized in that the HNO in the nitric acid3With the HCl's in hydrochloric acid
Mass ratio is 5~8.
4. glass etching liquid according to claim 1, which is characterized in that the nano fluoride be nano calcium fluoride and/
Or nanometer sodium fluoride.
5. glass etching liquid according to claim 1, which is characterized in that the grain size of the nano fluoride is 5-100nm.
6. glass etching liquid according to claim 1, which is characterized in that the surfactant is non-ionic surface active
Agent and anion surfactant.
7. glass etching liquid according to claim 6, which is characterized in that the nonionic surfactant is octylphenol polyethylene
Ethylene oxide ether and/or nonylphenol polyoxyethylene ether.
8. glass etching liquid according to claim 6, which is characterized in that the anion surfactant is dodecyl
At least one of sodium sulphate, neopelex and dioctyl succinate disulfonate acid.
9. a kind of preparation method of glass etching liquid according to any one of the preceding claims, which is characterized in that including
Following steps：
(1) water, phosphoric acid, nitric acid, sulfuric acid, hydrochloric acid, ammonium acid fluoride, potassium bichromate, polyvinylpyrrolidone are added in reactor
It stirs evenly, obtains component A；
(2) nano fluoride, surfactant are added in reactor and are stirred evenly, obtain B component；
(3) B component is added in component A, stirs evenly and can be obtained the glass etching liquid.
10. the preparation method of glass etching liquid according to claim 9, which is characterized in that the stir speed (S.S.) in step (1)
It is 100-500 revs/min；Stir speed (S.S.) in step (2) is 500-2000 revs/min；Stir speed (S.S.) in step (3) is 100-
1000 revs/min.
Priority Applications (1)
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| CN201810359967.7A CN108585530A (en) | 2018-04-20 | 2018-04-20 | A kind of glass etching liquid and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810359967.7A CN108585530A (en) | 2018-04-20 | 2018-04-20 | A kind of glass etching liquid and preparation method thereof |
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| CN201810359967.7A Pending CN108585530A (en) | 2018-04-20 | 2018-04-20 | A kind of glass etching liquid and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981207A (en) * | 2019-12-17 | 2020-04-10 | 安徽凤阳玻璃有限公司 | Preparation method of plate glass with anti-dazzle and anti-reflection functions |
| 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 |
| CN112430815A (en) * | 2020-11-23 | 2021-03-02 | 南通卓力达金属科技有限公司 | Etching solution and preparation method and application thereof |
| CN112662401A (en) * | 2020-11-25 | 2021-04-16 | 重庆臻宝实业有限公司 | Etching solution for low-resistance silicon product and etching method thereof |
| CN113072306A (en) * | 2021-04-08 | 2021-07-06 | 烟台远东精细化工有限公司 | Preparation method of electronic grade mixed acid etching solution |
| CN114075041A (en) * | 2020-08-12 | 2022-02-22 | Oppo广东移动通信有限公司 | Frosting liquid and preparation method thereof, frosted glass and processing method thereof |
| CN114751648A (en) * | 2022-04-01 | 2022-07-15 | 惠州市百时达化工有限公司 | Frosting liquid medicine for high-alumina-silica glass etching surface lattice directional arrangement and process |
| CN116040952A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, glass with crystal-shining pattern and production method thereof |
| CN116040951A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid and preparation method thereof, striped glass and production method thereof |
| CN116040948A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, preparation method thereof, glass with flash crystal effect and production method thereof |
| CN116040949A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, glass with nut patterns and production method thereof |
| CN116144429A (en) * | 2022-12-22 | 2023-05-23 | 湖北兴福电子材料股份有限公司 | Cleaning solution and cleaning method for carbon-containing film |
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| CN101054265A (en) * | 2007-05-09 | 2007-10-17 | 信利半导体有限公司 | Glass etching liquid for flat panel display |
| CN105060727A (en) * | 2015-07-31 | 2015-11-18 | 安徽和润特种玻璃有限公司 | Etching solution for high-transmittance anti-dazzle glass, and preparation method thereof |
| CN107601912A (en) * | 2017-09-19 | 2018-01-19 | 合肥惠科金扬科技有限公司 | A kind of efficient etching solution of TFT LCD displays base plate glass |
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| US20060118759A1 (en) * | 2002-08-26 | 2006-06-08 | Sylke Klein | Etching pastes for titanium oxide surfaces |
| CN101054265A (en) * | 2007-05-09 | 2007-10-17 | 信利半导体有限公司 | Glass etching liquid for flat panel display |
| CN105060727A (en) * | 2015-07-31 | 2015-11-18 | 安徽和润特种玻璃有限公司 | Etching solution for high-transmittance anti-dazzle glass, and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110981207A (en) * | 2019-12-17 | 2020-04-10 | 安徽凤阳玻璃有限公司 | Preparation method of plate glass with anti-dazzle and anti-reflection functions |
| CN111362584B (en) * | 2020-03-21 | 2022-02-18 | 郑州恒昊光学科技有限公司 | High borosilicate glass etching solution 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 |
| CN114075041A (en) * | 2020-08-12 | 2022-02-22 | Oppo广东移动通信有限公司 | Frosting liquid and preparation method thereof, frosted glass and processing method thereof |
| CN112430815A (en) * | 2020-11-23 | 2021-03-02 | 南通卓力达金属科技有限公司 | Etching solution and preparation method and application thereof |
| CN112662401A (en) * | 2020-11-25 | 2021-04-16 | 重庆臻宝实业有限公司 | Etching solution for low-resistance silicon product and etching method thereof |
| CN113072306A (en) * | 2021-04-08 | 2021-07-06 | 烟台远东精细化工有限公司 | Preparation method of electronic grade mixed acid etching solution |
| CN116040952A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, glass with crystal-shining pattern and production method thereof |
| CN116040951A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid and preparation method thereof, striped glass and production method thereof |
| CN116040948A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, preparation method thereof, glass with flash crystal effect and production method thereof |
| CN116040949A (en) * | 2021-10-28 | 2023-05-02 | 比亚迪股份有限公司 | Glass etching liquid, glass with nut patterns and production method thereof |
| CN114751648A (en) * | 2022-04-01 | 2022-07-15 | 惠州市百时达化工有限公司 | Frosting liquid medicine for high-alumina-silica glass etching surface lattice directional arrangement and process |
| CN114751648B (en) * | 2022-04-01 | 2024-02-27 | 惠州市百时达化工有限公司 | Frosting liquid medicine and process for high-alumina silicate glass etched surface lattice directional arrangement |
| CN116144429A (en) * | 2022-12-22 | 2023-05-23 | 湖北兴福电子材料股份有限公司 | Cleaning solution and cleaning method for carbon-containing film |
| CN116144429B (en) * | 2022-12-22 | 2024-04-19 | 湖北兴福电子材料股份有限公司 | Cleaning solution and cleaning method for carbon-containing film |
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