CN117819828A - Low-haze glass and preparation method and application thereof - Google Patents
Low-haze glass and preparation method and application thereof Download PDFInfo
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- CN117819828A CN117819828A CN202311547836.9A CN202311547836A CN117819828A CN 117819828 A CN117819828 A CN 117819828A CN 202311547836 A CN202311547836 A CN 202311547836A CN 117819828 A CN117819828 A CN 117819828A
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- 239000011521 glass Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000005530 etching Methods 0.000 claims abstract description 66
- 238000005498 polishing Methods 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000013067 intermediate product Substances 0.000 claims abstract description 25
- 239000005354 aluminosilicate glass Substances 0.000 claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 34
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000008103 glucose Substances 0.000 claims description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 6
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000002313 adhesive film Substances 0.000 claims description 5
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 239000001506 calcium phosphate Substances 0.000 claims description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 3
- 235000011010 calcium phosphates Nutrition 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 3
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000003270 potassium fluoride Nutrition 0.000 claims description 3
- 239000011698 potassium fluoride Substances 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 3
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 3
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 3
- 238000007517 polishing process Methods 0.000 claims description 2
- 239000001166 ammonium sulphate Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 30
- 230000003287 optical effect Effects 0.000 abstract description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003848 UV Light-Curing Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000005329 float glass Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 241001268993 Heterochrosis Species 0.000 description 1
- 238000006124 Pilkington process Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Theoretical Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to the field of glass products, and discloses low-haze glass and a preparation method and application thereof. The method comprises the following steps: (1) Polishing the aluminosilicate glass in the presence of a polishing solution to obtain an intermediate product I; (2) Performing first etching on the intermediate product I in an etching solution I to obtain an intermediate product II; the conditions of the first etching include: etching thickness of 1-2 μm; the difference in height of the irregularities on the surface of the intermediate product II in any 40 μm by 40 μm range is not more than 0.25 μm; (3) Performing second etching on the intermediate product II in etching solution II to obtain the low-haze glass; the conditions of the second etching include: etching thickness is 30-80 μm; the low-haze glass prepared by the method has better optical uniformity, and the yield in preparing low-haze glass products by using float silica-alumina glass is greatly improved.
Description
Technical Field
The invention relates to the field of glass products, in particular to low-haze glass and a preparation method and application thereof.
Background
The anti-dazzle display protective glass product is manufactured by adopting a chemical etching process, a spraying process and the like, and the anti-dazzle treated protective glass has excellent anti-dazzle performance, and is clearer in image quality and clearer in visual effect when applied to the display field. At present, the main reference technical indexes for detecting the quality of the anti-dazzle glass are the optical performance, and the main technical indexes include glossiness, haze, light transmittance, definition and the like.
The higher the haze, the lower the glossiness, transparency and imaging degree of the protective glass, and as the requirement of high-grade automobile on vehicle-mounted display definition is higher and higher, the low-haze product is more and more favored by customers.
The glass has higher physical and chemical properties except optical properties, so that the alkali metal content and aluminum content of the glass body in the composition of the glass body can be controlled within a certain range (wherein the alkali metal content is not more than 7wt% and the aluminum oxide content is at least 7 wt%), in the production process of the glass, the productivity of the float process is higher, the cost is lower, and the competition of product application is obvious, but in the actual production process, compared with the overflow method, the pulling amount of the float glass is at least 10 times that of the ordinary overflow method, and the glass discharge amount is large; and the viscosity of the aluminum-silicon glass is at least 100 ℃ higher than that of the common soda-lime glass, the melting and molding viscosity is higher, microscopic unevenness is easy to appear on the surface of the glass in the melting and molding process, the optical uniformity of the anti-dazzle protection glass product is poor, and the poor is rapidly increased along with the decrease of the haze.
However, in order to solve the problem of poor optical uniformity of low haze glass products, many problems still remain in the prior art, such as: firstly, the problem that the uniformity of formed glass liquid needs to be improved due to poor optics is solved, the improvement of the uniformity of the glass liquid mainly depends on a forming channel and a stirring device, the fixed investment is too large, the manufacturing cost of a product is improved by more than 50%, and the competitiveness of the product is directly affected; secondly, because the characteristics of float glass can not effectively promote glass forming and temperature control processes, only batch selection verification can be carried out on products at last, but the optical bad proportion can not be effectively promoted and ensured, a large amount of complaints are caused, and stable supply is not possible.
Disclosure of Invention
The invention aims to solve the problem of poor optical uniformity of low-haze glass in the prior art.
In order to achieve the above object, a first aspect of the present invention provides a method of preparing a low haze glass, the method comprising:
(1) Polishing the aluminosilicate glass in the presence of a polishing solution to obtain an intermediate product I; the conditions of the polishing treatment include: polishing thickness is 10-20 μm; the polishing solution is selected from at least one of solution A, solution B and solution C;
(2) Performing first etching on the intermediate product I in an etching solution I to obtain an intermediate product II; the conditions of the first etching include: etching thickness of 1-2 μm; the difference in height of the irregularities on the surface of the intermediate product II in any 40 μm by 40 μm range is not more than 0.25 μm;
(3) Performing second etching on the intermediate product II in etching solution II to obtain the low-haze glass; the conditions of the second etching include: etching thickness of 30-80 μm ；
Based on the total mass of the solution A, the solution A contains 2-8wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 1-5wt% of nitric acid and 75-95wt% of water;
based on the total mass of the solution B, the solution B contains 3-10wt% of ammonium bifluoride, 10-30wt% of sulfuric acid and 60-87wt% of water;
based on the total mass of the solution C, the solution C contains 2-13wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 3-8wt% of phosphoric acid and 71-93wt% of water.
Preferably, the conditions of the polishing treatment further include: the polishing rate is 2-4 μm/min.
Preferably, the polishing solution is a C solution.
Preferably, the thickness of the aluminosilicate glass is 0.3-1.8mm.
More preferably, the thickness of the aluminosilicate glass is 1.0-1.5mm.
Further preferably, the thickness of the tin-impregnated layer of the tin face of the aluminosilicate glass is not more than 15 μm.
Preferably, in step (2), the etching solution I contains 18 to 26wt% of ammonium bifluoride, 7 to 11wt% of citric acid, 2 to 5wt% of barium sulfate, 2 to 6wt% of bentonite, 8 to 15wt% of ferric trichloride, 8 to 15wt% of potassium nitrate, 5 to 9wt% of potassium fluoride, 3 to 6wt% of hydrofluoric acid and 7 to 44wt% of water based on the total mass of the etching solution I.
Preferably, in the step (2), the etching solution I contains 25 to 30wt% of ammonium bifluoride, 8 to 12wt% of ammonium fluoride, 5 to 10wt% of magnesium fluoride, 20 to 25wt% of oxalic acid, 2 to 3wt% of calcium phosphate, 4 to 6wt% of ammonium sulfate, 5 to 10wt% of sodium hexametaphosphate and 4 to 31wt% of water based on the total mass of the etching solution I.
Preferably, in step (3), the etching solution II is selected from at least one of a C solution and a D solution; the solution D contains 5-20wt% of hydrofluoric acid, 2-15wt% of sulfuric acid, 5-20wt% of ammonium bifluoride, 1-5wt% of glucose and 40-87wt% of water based on the total mass of the solution D.
Preferably, the method further comprises: before the step (1), coating a protective material on the tin surface of the aluminosilicate glass.
More preferably, the protective material is at least one selected from acid-fast ink, UV-curable ink, UV-adhesive film.
Further preferably, the thickness of the coating protecting material is 15-70 μm.
A second aspect of the invention provides a low haze glass prepared by the method of the first aspect.
A third aspect of the invention provides the use of the low haze glass of the second aspect in a display device.
The low-haze glass prepared by the method provided by the invention has better optical uniformity, and the yield in preparing low-haze glass products by using float silica-alumina glass is greatly improved.
Drawings
FIG. 1 is a graph of the grain surface at various magnification (gloss (G) 121, roughness (Ra) 0.035, haze (H) 3.5, maximum height (Rz) 0.325, average width (Rsm) 15, flash point (spark) 0.78) for the low haze glass prepared in example 1 provided by the present invention;
FIG. 2 is a graph of the grain surface at various magnification (gloss (G): 25, roughness (Ra): 0.4, haze (H): 35, and average width (Rsm): 55) for the low haze glass prepared in example 3 provided by the present invention.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
As previously described, a first aspect of the present invention provides a method of preparing a low haze glass, the method comprising:
(1) Polishing the aluminosilicate glass in the presence of a polishing solution to obtain an intermediate product I; the conditions of the polishing treatment include: polishing thickness is 10-20 μm; the polishing solution is selected from at least one of solution A, solution B and solution C;
(2) Performing first etching on the intermediate product I in an etching solution I to obtain an intermediate product II; the conditions of the first etching include: etching thickness of 1-2 μm; the difference in height of the irregularities on the surface of the intermediate product II in any 40 μm by 40 μm range is not more than 0.25 μm;
(3) Performing second etching on the intermediate product II in etching solution II to obtain the low-haze glass; the conditions of the second etching include: etching thickness of 30-80 μm ；
Based on the total mass of the solution A, the solution A contains 2-8wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 1-5wt% of nitric acid and 75-95wt% of water;
based on the total mass of the solution B, the solution B contains 3-10wt% of ammonium bifluoride, 10-30wt% of sulfuric acid and 60-87wt% of water;
based on the total mass of the solution C, the solution C contains 2-13wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 3-8wt% of phosphoric acid and 71-93wt% of water.
In the present invention, the polishing thickness refers to a thickness obtained by polishing and removing a non-tin surface of the aluminosilicate glass; the etching thickness refers to the thickness removed after etching the non-tin surface of the aluminosilicate glass.
Preferably, the concentration of hydrofluoric acid is 55wt%, the concentration of sulfuric acid is 98wt%, the concentration of hydrochloric acid is 36wt%, the concentration of nitric acid is 68wt%, the concentration of ammonium bifluoride is 95wt%, and the concentration of phosphoric acid is 85wt%.
It should be noted that, in order to ensure uniformity of the polishing solution, the polishing solution may be stirred and/or bubbled with compressed air before use, which is not described herein, and those skilled in the art should not understand the limitation of the present invention.
Preferably, the conditions of the polishing treatment further include: the polishing rate is 2-4 μm/min.
More preferably, the conditions of the polishing process further include: the temperature is 20-35 ℃.
Preferably, the conditions of the first etching and the second etching treatment each independently further include: the temperature is 20-40 ℃.
Preferably, the polishing solution is a C solution.
Preferably, the thickness of the aluminosilicate glass is 0.3-1.8mm.
More preferably, the thickness of the aluminosilicate glass is 1.0-1.5mm.
Further preferably, the thickness of the tin-impregnated layer of the tin face of the aluminosilicate glass is not more than 15 μm.
Preferably, in step (2), the etching solution I contains 18 to 26wt% of ammonium bifluoride, 7 to 11wt% of citric acid, 2 to 5wt% of barium sulfate, 2 to 6wt% of bentonite, 8 to 15wt% of ferric trichloride, 8 to 15wt% of potassium nitrate, 5 to 9wt% of potassium fluoride, 3 to 6wt% of hydrofluoric acid and 7 to 44wt% of water based on the total mass of the etching solution I.
Preferably, in the step (2), the etching solution I contains 25 to 30wt% of ammonium bifluoride, 8 to 12wt% of ammonium fluoride, 5 to 10wt% of magnesium fluoride, 20 to 25wt% of oxalic acid, 2 to 3wt% of calcium phosphate, 4 to 6wt% of ammonium sulfate, 5 to 10wt% of sodium hexametaphosphate and 4 to 31wt% of water based on the total mass of the etching solution I.
It should be noted that, in the present invention, etching solutions I of different formulations (types and/or ratios) may be selected according to different market demands; by adopting the etching solution I provided by the invention and combining specific polishing treatment and etching treatment, glass products with good glossiness uniformity, high product yield and haze values meeting different market demands can be obtained; the low haze glass of the present invention can be obtained by those skilled in the art based on the formulations and process parameters provided herein, and the following examples of the present invention are given by way of illustration of the preparation of the low haze glass of the present invention. The present invention is not described in detail in relation to all the formulations and process parameters, and the person skilled in the art should not be construed as limiting the invention.
Preferably, in step (3), the etching solution II is selected from at least one of a C solution and a D solution; the solution D contains 5-20wt% of hydrofluoric acid, 2-15wt% of sulfuric acid, 5-20wt% of ammonium bifluoride, 1-5wt% of glucose and 40-87wt% of water based on the total mass of the solution D.
Preferably, the glucose is an aqueous glucose solution having a concentration of 90-95 wt%.
It should be noted that, in order to ensure uniformity of etching, the etching solution I and the etching solution II may be stirred and/or bubbled with compressed air before use, which is not described herein, and those skilled in the art should not understand the limitation of the present invention.
In order to meet the product quality requirement, the low haze product needs air surface treatment, the tin surface needs protection treatment, and preferably, the method further comprises: before the step (1), coating a protective material on the tin surface of the aluminosilicate glass.
More preferably, the protective material is at least one selected from acid-fast ink, UV-curable ink, UV-adhesive film.
In the invention, the acid-resistant ink is AG glass protection ink, the UV curing ink is UV curing acid-resistant ink, and the UV adhesive film is UV acid-resistant and alkali-resistant protection film, so that the acid-resistant ink is not particularly required to resist 10wt% hydrofluoric acid for 15-30min, and manufacturers and models can not be specified on the premise of ensuring the product quality of the protection material.
Further preferably, the thickness of the coating protecting material is 15-70 μm.
As previously described, a second aspect of the present invention provides a low haze glass prepared by the method of the first aspect.
As previously described, a third aspect of the present invention provides the use of the low haze glass of the second aspect in a display device.
The invention will be described in detail below by way of examples and is not thereby limited. Unless otherwise indicated, all of the experimental apparatus, reagents and materials involved in the examples below were commercially available, and all of the reagents were analytically pure.
In the following examples, the concentration of hydrofluoric acid was 55wt%, the concentration of sulfuric acid was 98wt%, the concentration of hydrochloric acid was 36wt%, the concentration of nitric acid was 68wt%, the concentration of ammonium bifluoride was 95wt%, the concentration of phosphoric acid was 85wt%, and glucose was an aqueous glucose solution having a concentration of 95wt%, unless otherwise specified.
Example 1
This example illustrates the low haze glass of the present invention according to the process parameters in table 1 and prepared as follows.
The method for preparing the low haze glass comprises the following steps:
pretreatment: coating a 50 mu m UV adhesive film on the tin surface of the aluminum silicon glass; the thickness of the aluminum silicon glass is 1.1mm; the thickness of the tin-impregnated layer of the tin surface of the aluminum silicon glass is 10 mu m;
step one: polishing the aluminosilicate glass in the presence of a polishing solution to obtain an intermediate product I;
step two: performing first etching on the intermediate product I in an etching solution I to obtain an intermediate product II;
step three: and performing second etching on the intermediate product II in etching solution II to obtain the low-haze glass.
The remaining examples were carried out using procedures similar to those of example 1, except that the process parameters used in each example were varied, see in particular table 1, unless otherwise specified.
TABLE 1
Example 7
This example was conducted using a procedure similar to example 1, except that in this example, in step one, the polishing treatment conditions were: the polishing rate was 4.5 μm/min; the polishing solution contained 8wt% hydrofluoric acid, 6wt% sulfuric acid, 5wt% hydrochloric acid, 7wt% phosphoric acid and 74wt% water based on the total mass of the polishing solution.
The remainder was the same as in example 1.
The low haze glass S7 was prepared.
Comparative example 1
This comparative example was conducted by following a procedure similar to example 1 except that in this comparative example, in the first step, the polishing solution contained 5wt% of hydrofluoric acid, 3wt% of acetic acid (concentration of 99 wt%) and 92wt% of water based on the total mass of the polishing solution.
The remainder was the same as in example 1.
The low haze glass DS1 was prepared.
Comparative example 2
This comparative example was conducted using a procedure similar to that of example 1, except that in this comparative example, in step two, the conditions of the first etching were: the etching thickness was 4. Mu.m.
The remainder was the same as in example 1.
The low haze glass DS2 is prepared.
Comparative example 3
This comparative example was conducted using a procedure similar to that of example 1, except that in this comparative example, in step three, the conditions of the second etching were: the etching thickness was 4. Mu.m.
The remainder was the same as in example 1.
The low haze glass DS3 was prepared.
Comparative example 4
This comparative example was conducted using a procedure similar to that of example 1, except that in the first step, the comparative example was subjected to polishing treatment by physical polishing, specifically, the physical polishing was conducted as follows:
polishing the aluminosilicate glass in the presence of polishing liquid to obtain an intermediate product I; the conditions of the polishing treatment include: the polishing thickness is 15 mu m, the polishing speed is 3 mu m/min, the polishing temperature is 30-38 ℃, and the pH value is 3-9;
the polishing solution is prepared from the following components in percentage by mass: 1 (model VK-Ce02W, available from Xuancheng Jinrui New Material Co., ltd.) and water.
The remainder was the same as in example 1.
The low haze glass DS4 was prepared.
Test case
1. Gloss uniformity test: adopting a triangular glossiness tester to test the glossiness of the etched surface of the product, wherein each product takes 10.5 inches as an example to measure 9 points, the uniformity is a CPK value of the measured value of 9 points, and the larger the value is, the better the value is;
2. haze value: testing the haze of the product by adopting a haze permeameter;
3. roughness difference: testing the etching surface roughness of the product by adopting a Sanfeng roughness measuring instrument, measuring at least 6 points of each product by taking 10.5 inches as an example, and calculating the difference value between the maximum value and the minimum value, wherein the smaller the value is, the better the value is;
4. product yield: the product yield is mainly measured by an instrument, and after the haze value parameter is confirmed to meet the requirement (not higher than 35), the product is qualified if visual inspection appearance is free of obvious dot/line/block heterochrosis and bad scratch, and 100 pieces of glass are prepared by adopting a corresponding preparation method in each example and comparative example, wherein the product yield=qualified product quantity/100.
The low haze glasses obtained in the examples and comparative examples were subjected to performance testing using the test methods described above, and the results are shown in table 2.
TABLE 2
As can be seen from the results in Table 2, the low haze glass prepared by the method provided by the invention meets the market demand, and meanwhile, the low haze glass has better glossiness uniformity and roughness effects, higher product yield and can effectively reduce the input cost.
The invention exemplarily provides the grain surface diagrams of the low-haze glass prepared in the embodiment 1 (figure 1) and the embodiment 3 (figure 2) under different magnification, and further illustrates that products with different roughness and haze values and high optical uniformity and yield can be obtained by adopting the method provided by the invention, so that the requirements of different markets are met and the product quality is ensured.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. A method of making a low haze glass, the method comprising:
(1) Polishing the aluminosilicate glass in the presence of a polishing solution to obtain an intermediate product I; the conditions of the polishing treatment include: polishing thickness is 10-20 μm; the polishing solution is selected from at least one of solution A, solution B and solution C;
(2) Performing first etching on the intermediate product I in an etching solution I to obtain an intermediate product II; the conditions of the first etching include: etching thickness of 1-2 μm; the difference in height of the irregularities on the surface of the intermediate product II in any 40 μm by 40 μm range is not more than 0.25 μm;
(3) Performing second etching on the intermediate product II in etching solution II to obtain the low-haze glass; the conditions of the second etching include: etching thickness of 30-80 μm ；
Based on the total mass of the solution A, the solution A contains 2-8wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 1-5wt% of nitric acid and 75-95wt% of water;
based on the total mass of the solution B, the solution B contains 3-10wt% of ammonium bifluoride, 10-30wt% of sulfuric acid and 60-87wt% of water;
based on the total mass of the solution C, the solution C contains 2-13wt% of hydrofluoric acid, 1-7wt% of sulfuric acid, 1-5wt% of hydrochloric acid, 3-8wt% of phosphoric acid and 71-93wt% of water.
2. The method according to claim 1, wherein in step (1), the conditions of the polishing process further comprise: the polishing rate is 2-4 mu m/min;
and/or, the polishing solution is a C solution.
3. A method according to claim 1 or 2, characterized in that the aluminosilicate glass has a thickness of 0.3-1.8mm, preferably 1.0-1.5mm;
and/or the thickness of the tin-impregnated layer of the tin surface of the aluminosilicate glass is not higher than 15 mu m.
4. A method according to any one of claims 1-3, characterized in that in step (2) the etching solution I contains 18-26wt% ammonium bifluoride, 7-11wt% citric acid, 2-5wt% barium sulphate, 2-6wt% bentonite, 8-15wt% ferric trichloride, 8-15wt% potassium nitrate, 5-9wt% potassium fluoride, 3-6wt% hydrofluoric acid and 7-44wt% water, based on the total mass of the etching solution I.
5. A method according to any one of claims 1 to 3, characterized in that in step (2) the etching solution I contains 25 to 30 wt.% ammonium bifluoride, 8 to 12 wt.% ammonium fluoride, 5 to 10 wt.% magnesium fluoride, 20 to 25 wt.% oxalic acid, 2 to 3 wt.% calcium phosphate, 4 to 6 wt.% ammonium sulphate, 5 to 10 wt.% sodium hexametaphosphate and 4 to 31 wt.% water, based on the total mass of the etching solution I.
6. The method according to any one of claims 1 to 5, wherein in step (3), the etching solution II is selected from at least one of a C solution and a D solution; the solution D contains 5-20wt% of hydrofluoric acid, 2-15wt% of sulfuric acid, 5-20wt% of ammonium bifluoride, 1-5wt% of glucose and 40-87wt% of water based on the total mass of the solution D.
7. The method according to any one of claims 1-6, further comprising: before the step (1), coating a protective material on the tin surface of the aluminum silicon glass;
preferably, the protective material is at least one selected from acid-resistant ink, UV-curable ink and UV adhesive film.
8. The method of claim 7, wherein the thickness of the coating protection material is 15-70 μm.
9. A low haze glass made by the method of any one of claims 1-8.
10. Use of the low haze glass according to claim 9 in a display device.
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| CN202311547836.9A CN117819828A (en) | 2023-11-20 | 2023-11-20 | Low-haze glass and preparation method and application thereof |
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| CN202311547836.9A CN117819828A (en) | 2023-11-20 | 2023-11-20 | Low-haze glass and preparation method and application thereof |
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| CN202311547836.9A Pending CN117819828A (en) | 2023-11-20 | 2023-11-20 | Low-haze glass and preparation method and application thereof |
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