CN116081955A - Frosting composition, frosting liquid, flash sand effect high-alumina glass, and preparation method and application thereof - Google Patents
Frosting composition, frosting liquid, flash sand effect high-alumina glass, and preparation method and application thereof Download PDFInfo
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- CN116081955A CN116081955A CN202211733255.XA CN202211733255A CN116081955A CN 116081955 A CN116081955 A CN 116081955A CN 202211733255 A CN202211733255 A CN 202211733255A CN 116081955 A CN116081955 A CN 116081955A
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- 239000011521 glass Substances 0.000 title claims abstract description 188
- 239000000203 mixture Substances 0.000 title claims abstract description 125
- 239000007788 liquid Substances 0.000 title claims abstract description 116
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 230000000694 effects Effects 0.000 title claims abstract description 70
- 239000004576 sand Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 98
- 238000000034 method Methods 0.000 claims abstract description 62
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims abstract description 40
- 229910001618 alkaline earth metal fluoride Inorganic materials 0.000 claims abstract description 40
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 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 abstract description 26
- 230000003746 surface roughness Effects 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 15
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 15
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims description 68
- 238000005498 polishing Methods 0.000 claims description 63
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 48
- 239000000126 substance Substances 0.000 claims description 37
- 230000002378 acidificating effect Effects 0.000 claims description 35
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 28
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 26
- 239000002253 acid Substances 0.000 claims description 25
- 238000010306 acid treatment Methods 0.000 claims description 24
- 239000005338 frosted glass Substances 0.000 claims description 19
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 14
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 14
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 14
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 14
- 235000013024 sodium fluoride Nutrition 0.000 claims description 14
- 239000011775 sodium fluoride Substances 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- 235000003270 potassium fluoride Nutrition 0.000 claims description 13
- 239000011698 potassium fluoride Substances 0.000 claims description 13
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 7
- 239000004973 liquid crystal related substance Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000000873 masking effect Effects 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 42
- 230000008569 process Effects 0.000 abstract description 36
- 239000002245 particle Substances 0.000 abstract description 17
- 239000011256 inorganic filler Substances 0.000 abstract description 8
- 229910003475 inorganic filler Inorganic materials 0.000 abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000009827 uniform distribution Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 34
- 239000000243 solution Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 15
- 238000005530 etching Methods 0.000 description 14
- 238000009826 distribution Methods 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 9
- 229910052783 alkali metal Inorganic materials 0.000 description 8
- 150000001340 alkali metals Chemical class 0.000 description 8
- 229940104869 fluorosilicate Drugs 0.000 description 7
- 238000010998 test method Methods 0.000 description 7
- 230000036961 partial effect Effects 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 5
- -1 ammonium ions Chemical class 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 229910001413 alkali metal ion Inorganic materials 0.000 description 3
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 3
- 150000001342 alkaline earth metals Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000000670 limiting effect Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- 238000003541 multi-stage reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 206010044038 Tooth erosion Diseases 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 201000009310 astigmatism Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000003841 chloride salts Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 229910001504 inorganic chloride Inorganic materials 0.000 description 1
- 239000006194 liquid suspension Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
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- 230000002829 reductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
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- 235000019698 starch Nutrition 0.000 description 1
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Images
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
-
- 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
- C03C15/02—Surface treatment of glass, not in the form of fibres or filaments, by etching for making a smooth surface
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The application relates to a frosting composition, which comprises the following components in parts by weight: 25-30 parts of ammonium bifluoride, 2-6 parts of alkali metal fluoride, 2-6 parts of alkaline earth metal fluoride, 2-3 parts of sodium sulfate, 2-5 parts of ammonia sulfate, 15-20 parts of sulfuric acid, 8-12 parts of nitric acid, 5-10 parts of acetone and 15-30 parts of water. The frosting liquid prepared from the frosting composition can be free of chloride and inorganic filler, fluoride can be adopted, the proportion of each component can be finely controlled, and crystal educts with smaller particles and uniform distribution can be obtained when the frosting liquid is used for the frosting process of high-alumina glass, so that the high-alumina glass product with the flash sand effect is prepared, and the glass product has smaller surface roughness and higher haze. In addition, the frosting process has higher efficiency, low replacement frequency, no chlorine-containing wastewater and less environmental pollution.
Description
Technical Field
The application relates to the technical field of glass surface treatment, in particular to frosting composition, high-alumina glass with a flash sand effect and a preparation method thereof.
Background
The frosted glass has the advantages of high astigmatism, dirt resistance, fine hand feeling and the like, and is widely applied to products such as front covers, rear covers, battery rear covers, vehicle-mounted products and the like of high-end mobile phones. Most of high-end smart phone rear covers in China adopt frosting liquid etching technology to obtain glass with a flash sand effect, but the haze of glass products after the existing frosting treatment is low, the size of particles on the surfaces of the products is large, and the hand feeling of users is affected.
Disclosure of Invention
Based on this, the object of the present application includes providing a frosting composition, which can be used for processing high-alumina glass and producing a flash sand table high-alumina glass having smaller surface roughness and higher haze by adjusting the weight percentage of ammonium bifluoride, alkali metal fluoride, alkaline earth metal fluoride, etc., without using inorganic filler and chloride. The application also provides the flash sand effect high-alumina glass and the preparation method thereof.
In a first aspect of the present application, there is provided a frosting composition comprising, in parts by weight: 25-30 parts of ammonium bifluoride, 2-6 parts of alkali metal fluoride, 2-6 parts of alkaline earth metal fluoride, 2-3 parts of sodium sulfate, 2-5 parts of ammonia sulfate, 15-20 parts of sulfuric acid, 8-12 parts of nitric acid, 5-10 parts of acetone and 15-30 parts of water;
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride;
the alkaline earth metal fluoride includes one or both of calcium fluoride and magnesium fluoride.
In some embodiments, the frosting composition has one or more of the following features:
the weight ratio of the alkali metal fluoride to the alkaline earth metal fluoride is (1-2.5): 1;
the ratio of the weight of ammonium bifluoride to the sum of the weights of alkali metal fluoride and alkaline earth metal fluoride is (2-5) 1;
the total weight of the frosting composition is 100 parts.
In some embodiments, the frosting composition comprises, by weight: 26 to 29 parts of ammonium bifluoride, 4 to 6 parts of alkali metal fluoride, 2 to 4 parts of alkaline earth metal fluoride, 2.5 to 3 parts of sodium sulfate, 3.5 to 5 parts of ammonia sulfate, 17 to 20 parts of sulfuric acid, 9 to 12 parts of nitric acid, 7 to 9 parts of acetone and 16 to 28 parts of water.
In a second aspect of the present invention, there is provided a frosting liquid obtained by aging a mixed liquid comprising the frosting composition according to the first aspect.
In some embodiments, the frosting liquid meets one or both of the following characteristics:
The frosting liquid is prepared by adopting a method comprising the following steps: mixing the components of the frosting composition, standing and curing for 24-54 hours at 20-25 ℃ to prepare the frosting liquid;
the pH value of the frosting liquid is 0.5-2.
In a third aspect of the present application, a method for preparing a high alumina glass with a flash sand effect is provided, including the following steps:
acid treatment is carried out on the high-alumina glass substrate by using an acid treatment liquid, so as to prepare an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
Performing frosting treatment on the acid-treated glass substrate for 200-300 s by using the frosting liquid according to the second aspect to obtain a frosted glass substrate;
and carrying out chemical polishing treatment on the frosted glass substrate by using the polishing solution, and carrying out ultrasonic cleaning.
In some embodiments, the methods of preparation meet one or more of the following characteristics:
the acidic treatment solution contains 4 g/mL-6 g/mL hydrofluoric acid and 3 g/mL-5 g/mL sulfuric acid;
the polishing solution contains 7-9 g/mL hydrofluoric acid and 55-65 g/mL sulfuric acid;
pre-cleaning the high alumina glass substrate before the acid treatment;
The acid treatment time is 300 s-600 s;
the temperature of the chemical polishing treatment is 40+/-0.5 ℃, and the accumulated treatment time is 100-200 s;
the times of the chemical polishing treatment are 8-13 times, and the treatment time of each time is 10-15 s;
after the chemical polishing treatment is finished, ultrasonic cleaning is carried out at 60+/-0.5 ℃ for 150-200 s.
In a fourth aspect of the application, a high alumina glass with a flash sand effect is provided, and the high alumina glass is prepared by the preparation method in the third aspect.
In some embodiments, the sparkling sand effect high alumina glass has a surface roughness of from 3 μm to 6 μm.
In a fifth aspect of the present application, a glass article is provided, comprising a glass structure, the glass structure being made from the sparkling sand effect high alumina glass of the fourth aspect.
The method does not use chloride salt and inorganic filler, adopts fluoride and finely controls the proportion of each composition, and has proper proportion of alkali metal ions, alkaline earth metal ions and ammonium ions. When the flash sand is used for the frosting process of the high-alumina glass, the erosion speed of the high-alumina glass and the crystal precipitation speed on the surface of the high-alumina glass are balanced, crystal precipitates with smaller particles and uniform distribution can be obtained, the surface roughness of the obtained flash sand effect high-alumina glass product is smaller (for example, only 3-6 μm), and the haze is higher (for example, 90-98%). The frosting composition is matched with an acidic pretreatment process when used in a frosting process, and has higher frosting efficiency on high-alumina glass; the frosting liquid does not contain inorganic filler, has stable composition and low replacement frequency, does not generate chlorine-containing wastewater, and has less environmental pollution.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application and to more fully understand the present application and its advantageous effects, the following brief description will be given with reference to the accompanying drawings, which are required to be used in the description of the embodiments. It is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained from these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic illustration of surface roughness in an embodiment of the present invention.
Detailed Description
In order to facilitate an understanding of the present application, a more complete description of the present application will follow. This application may, however, be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Terminology
Unless otherwise indicated or contradicted, terms or phrases used herein have the following meanings:
herein, "preferred", "better", "preferred" are merely to describe better embodiments or examples, and it should be understood that they do not limit the scope of protection of the present application. If there are multiple "preferences" in a solution, if there is no particular description and there is no conflict or constraint, then each "preference" is independent of the others.
In this application, "further," "still further," "particularly," and the like are used for descriptive purposes and are not to be construed as limiting the scope of the present application.
In the application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise the open technical scheme of the listed characteristics.
In this application, reference is made to a value interval (i.e., a range of values), where the distribution of the values selected within the value interval is considered continuous, and includes two value endpoints (i.e., a minimum value and a maximum value) of the value interval, and each value between the two value endpoints, unless otherwise indicated. When a numerical range merely points to integers within the numerical range, unless expressly stated otherwise, both endpoints of the numerical range are inclusive of the integer between the two endpoints, and each integer between the two endpoints is equivalent to the integer directly recited. When multiple numerical ranges are provided to describe a feature or characteristic, the numerical ranges may be combined. In other words, unless otherwise indicated, the numerical ranges disclosed herein are to be understood as including any and all subranges subsumed therein. The "numerical value" in the numerical interval may be any quantitative value, such as a number, a percentage, a proportion, or the like. "numerical interval" allows to broadly include quantitative intervals such as percentage intervals, proportion intervals, ratio intervals, etc.
The temperature parameter in the present application is not particularly limited, and may be a constant temperature treatment or may vary within a predetermined temperature range. It should be appreciated that the constant temperature process described allows the temperature to fluctuate within the accuracy of the instrument control. Allows for fluctuations within a range such as + -5 ℃, + -4 ℃, + -3 ℃, + -1 ℃, + -0.5 ℃.
High alkali glass, herein Al 2 O 3 Silicate glass of 18% or more.
The frosting treatment, which is also called as sand-blasting, in the present application refers to a process of etching the glass surface by using a frosting composition and precipitating crystals on the surface after pretreating one surface to be frosted with an organic acid aqueous solution of a dilute acid such as citric acid or an inorganic aqueous solution of hydrofluoric acid, sulfuric acid or nitric acid.
High alumina glass with flash sand effect, which is referred to herein as glass with flash sand effect.
High alumina glass (alumina content is more than 18% of the total weight of the glass composition) is widely applied to the fields of consumer electronics and displays due to excellent mechanical properties and light transmittance. However, when the alumina content in the glass structure is high, the difficulty of surface treatment of the high alumina glass is also increased.
Generally, al 2 O 3 Four-coordinated tetrahedra and six-coordinated octahedra are in the network structure of the glass, which on the one hand provides a fairly stable framework structure for the glass and on the other hand is detrimental to the movement of smaller radius ions such as alkali metal ions and alkaline earth metal ions. Therefore, the traditional frosting composition is used for treating the high-alumina glass, the frosting efficiency is low, the precipitated crystal particles are large and unevenly distributed, the roughness of the frosting surface of the glass is more than 500 mu m, and the haze of the product is only 45-60%.
The frosting composition adopted in the prior art mostly contains inorganic fillers such as starch, CMC, titanium pigment, activated carbon and calcium fluoride, and the inorganic fillers have low solubility in acidic aqueous solution, so that the frosting composition is easy to be uneven in components in the production process, the frosting composition needs to be replaced frequently, and more solid wastes are generated to have adverse effects on the environment.
The present application has found, through extensive research, that a frosting composition can better overcome the above problems.
In a first aspect of the present application, there is provided a frosting composition comprising, in parts by weight: 25-30 parts of ammonium bifluoride, 2-5 parts of alkali metal fluoride, 3-6 parts of alkaline earth metal fluoride, 2-3 parts of sodium sulfate, 2-5 parts of ammonia sulfate, 15-20 parts of sulfuric acid, 8-12 parts of nitric acid, 5-10 parts of acetone and 15-30 parts of water;
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride;
the alkaline earth metal fluoride comprises one or two of calcium fluoride and magnesium fluoride;
the total weight of the frosting composition is 100 parts.
The scheme does not use chloride and inorganic filler, adopts fluoride and finely controls the proportion of each component, and has higher erosion efficiency when being used in the frosting process of the high-alumina glass; the method is characterized in that the ratio of alkali metal ions, alkaline earth metal ions and ammonium ions is proper, the method is used for the frosting process of the high-alumina glass, the erosion rate of the glass and the surface crystal precipitation rate of the glass are balanced, crystal precipitates which are smaller in particles and uniformly distributed can be formed on the surface of the high-alumina glass, and the obtained flash sand effect high-alumina glass product is smaller in surface roughness (for example, 3-6 mu m) and higher in haze (for example, 90-98%).
The ammonium bifluoride in the frosting liquid composition provides ammonium bifluoride ions and fluoride ions, and the ammonium bifluoride content in the frosting liquid composition is controlled in a proper range, so that the high-alumina glass with a low surface roughness and a high flash sand effect can be obtained, and the frosting treatment efficiency is improved. If in the frosting liquid compositionAmmonium bifluoride content above the proper range may lead to the formation of large amounts (NH 4 ) 2 SiF 6 Grow into large crystals, affecting roughness; if the ammonium bifluoride content in the frosting liquid composition is below the proper range, the alkali metal fluoride and alkaline earth metal fluoride may be caused to grow slowly, and the ammonium bifluoride amount is small (NH 4 )2SiF 6 The formation rate is too slow, so that the glass is etched without forming a crystal protection layer, and the frosting effect cannot be achieved.
In the frosting composition, the calculation method of the weight parts of sulfuric acid is that sulfuric acid H in dilute sulfuric acid (less than or equal to 70 wt%) 2 SO 4 Solute meter.
In the frosting composition, the sulfuric acid weight part is calculated by nitric acid HNO in dilute nitric acid (less than or equal to 31.68 wt%) 3 Solute meter.
In some embodiments, the frosting composition comprises 25-30 parts by weight of ammonium bifluoride, 25-29 parts by weight of ammonium bifluoride, 26-29 parts by weight of ammonium bifluoride, and one or two of the following ranges by weight: 25 parts, 25.5 parts, 26 parts, 26.5 parts, 27 parts, 27.5 parts, 28 parts, 28.5 parts, 29 parts, 29.5 parts, 30 parts, etc.
When the surface of the high-alumina glass is subjected to frosting treatment, part of alkali metal fluoride and silicon which is corroded and dissociated in the glass are subjected to multi-step reaction to finally form fluorosilicate for crystallization on the surface of the glass. The alkali metal fluoride content in the frosting liquid composition is controlled in a proper range, so that the high-alumina glass with the flash sand effect, which has small precipitated crystal particles and uniform distribution, can be obtained. If the alkali metal fluoride content in the frosting liquid composition is higher than the proper range, stacking of alkali metal fluorosilicate crystals and larger roughness of the glass surface may be caused; if the alkali metal fluoride content in the composition of the frosting liquid is lower than the proper range, the precipitation speed of alkali metal fluorosilicate crystals may be slow, and the distribution uniformity of the precipitates on the glass surface may be poor.
In some embodiments, the frosting composition comprises 2-6 parts by weight of alkali metal fluoride, further 3-6 parts by weight, further 4-6 parts by weight, and further one or two of the following ranges: 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, etc.
In some embodiments, the alkali metal fluoride comprises 2-3 parts by weight of potassium fluoride and 2-3 parts by weight of sodium fluoride.
The alkaline earth metal fluoride content in the frosting liquid composition is controlled in a proper range, so that the high-alumina glass with small precipitated crystal particles and fine hand feeling and a flash sand effect is obtained. If the alkaline earth metal fluoride content in the frosting liquid composition is higher than the proper range, more alkaline earth metal fluoride can be generated, the crystal particle size is large, and the roughness is large; if the alkali earth metal fluoride content in the frosting liquid composition is below the proper range, it may cause an increase in the fluoride percentage of alkali metal indirectly, a stacking of a large number of polycrystal, and a small number of maldistribution of crystal.
In some embodiments, the frosting composition comprises 2-6 parts by weight of alkaline earth metal fluoride, further 2-5 parts by weight, further 2-4 parts by weight, and further one or two of the following ranges: 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, etc.
In some embodiments, the alkaline earth metal fluoride comprises 1-2 parts by weight of magnesium fluoride and 1-2 parts by weight of calcium fluoride.
In some embodiments, the alkaline earth metal fluoride comprises 1-2 parts of magnesium fluoride according to parts by weight, and can be selected from the following ranges: 1 to 1.5 parts or 1.5 to 2 parts.
In some embodiments, the alkaline earth metal fluoride comprises 1-2 parts of calcium fluoride according to parts by weight, and can be selected from the following ranges: 1 to 1.5 parts or 1.5 to 2 parts.
The action of sodium sulfate provides free Na + And replenishing the alkali metal consumed in the frosting liquid. The sodium sulfate in the frosting liquid composition containsThe control of the amount in a proper range is beneficial to prolonging the service life of the frosting liquid. If the sodium sulfate content in the frosting liquid composition is higher than the proper range, it may cause an increase in the amount of RF, and stacking of crystals; if the sodium sulfate content in the composition of the frosting liquid is below the proper range, the use cycle of the frosting liquid may be shortened.
In some embodiments, the frosting composition comprises 2-3 parts by weight of sodium sulfate, further 2.2-3 parts by weight, further 2.5-3 parts by weight, and further one or two of the following ranges by weight: 2 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts, 2.9 parts, 3 parts, etc.
The action of ammonia sulfate supplements NH in the frosting liquid 4 . The ammonia sulfate content in the frosting liquid composition is controlled in a proper range to facilitate the reduction of the ammonia sulfate content (NH 4 )2SiF 6 Is continuously generated. If the ammonia sulfate content in the frosting liquid composition is higher than the proper range, coarse crystals can be caused to influence the roughness; if the ammonia sulfate content in the frosting liquid composition is lower than the proper range, the etching speed may be higher than the crystallization speed, the surface pits may be uneven, and the flatness difference may be large.
In some embodiments, the frosting composition comprises 2-5 parts by weight of ammonia sulfate, further 3-5 parts by weight, further 3.5-5 parts by weight, and further one or two of the following ranges by weight: 2 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts, 2.9 parts, 3 parts, 3.1 parts, 3.2 parts, 3.3 parts, 3.4 parts, 3.5 parts, 3.6 parts, 3.7 parts, 3.8 parts, 3.9 parts, 4 parts, 4.1 parts, 4.2 parts, 4.3 parts, 4.4 parts, 4.5 parts, 4.6 parts, 4.7 parts, 4.8 parts, 4.9 parts, 5 parts, etc.
The sulfuric acid provides an acidic environment for the frosting liquid, so that the surface structure of the high-alumina glass is easily damaged by hydrofluoric acid in a short time. Controlling the sulfuric acid content in the frosting liquid composition in a proper range is beneficial to balancing etching and frosting. If the sulfuric acid content in the frosting liquid composition is higher than the proper range, the etching speed may be too high, and the frosting is not finished; if the sulfuric acid content in the frosting liquid composition is lower than the proper range, local etching and local frosting of the high alumina glass may be caused.
In some embodiments, the frosting composition comprises, by weight, 15-20 parts of sulfuric acid, further 16-20 parts, further 17-20 parts, and further one or two of the following ranges: 15 parts, 15.5 parts, 16 parts, 16.5 parts, 17 parts, 17.5 parts, 18 parts, 18.5 parts, 19 parts, 19.5 parts, 20 parts, etc.
The action of nitric acid provides an acidic environment, sulfuric acid is highly oxidizing and exothermic, resulting in elevated temperature to volatilize HF, providing an acidic environment while reducing sulfuric acid concentration. The nitric acid content in the frosting liquid composition is controlled in a proper range, so that the frosting liquid composition is beneficial to the stabilization of the acidic environment and the frosting temperature. If the nitric acid content in the frosting liquid composition is higher than the proper range, the acidity may be increased, and the etching is too fast; if the nitric acid content in the frosting liquid composition is lower than the proper range, the sulfuric acid percentage may be increased, the frosting temperature is increased, and the gas volatilizes.
In some embodiments, the frosting composition comprises 8-12 parts by weight of nitric acid, further can be 9-12 parts by weight, and can be selected from the following one or two ranges in percentage by weight: 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, etc.
Acetone and water can be mutually dissolved in any proportion, which is beneficial to providing more uniform frosting liquid, thereby improving the efficiency of frosting treatment and the uniformity of particle distribution of surface precipitated crystals. If the acetone content in the frosting liquid composition is higher than the proper range, the frosting liquid is possibly sticky, the frosting components move slowly, and the frosting effect is poor; if the acetone content in the frosting liquid composition is lower than the proper range, the frosting liquid suspension effect may be poor, and the frosting components may be settled.
In some embodiments, the frosting composition comprises 5-10 parts by weight of acetone, further 6-10 parts by weight, further 7-9 parts by weight, and one or two of the following ranges: 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts, etc.
The frosting composition forms a frosting liquid after being mixed, stood and cured, and the concentration of each component in the frosting liquid is controlled in a proper range, so that the efficiency of frosting treatment is improved, and better surface roughness is obtained. If the water content in the frosting composition is higher than the proper range, the concentration of ions in the frosting liquid obtained after the frosting composition is kept stand and cured is small, and the solubility of the fluorosilicate separated out in the frosting process is large, so that the proportion of the metal fluorosilicate is unbalanced, the distribution of the precipitate is possibly uneven in the frosting process, and the flash effect is high, so that the haze of the aluminum glass is poor; if the water content in the frosting composition is lower than the proper range, the frosting composition may be kept still and cured to obtain a frosting liquid with stronger acidity or smaller dissolution amount of fluorosilicate, and uneven distribution of precipitate may be caused in the frosting process, so that the surface roughness of the high-alumina glass with high flash sand effect is larger.
In some embodiments, the frosting composition comprises 15-30 parts by weight of water, further 16-29 parts by weight, further 16-28 parts by weight, and one or two of the following ranges: 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts.
In the frosting process, alkali metal fluoride and alkaline earth metal fluoride interact with components in the frosting liquid, ions entering the solution after etching the glass surface in the frosting process, and multi-step reactions occur, and the generated substances comprise K 2 SiF 6 、Na 2 SiF 6 、(NH 4 ) 2 SiF 6 、CaF 2 、MgF 2 NaF, which form crystals or redissolve on the glass surface due to the difference in solubility in acidic aqueous solutions. The proportion of the alkali metal fluoride and the alkaline earth metal fluoride is controlled in a proper range, so that the glass with the flash sand effect, which has smaller surface roughness and lower haze, is favorable to be obtained. If the ratio of alkaline earth metal to alkali metal is higher thanIn a proper range, the precipitation process of alkali metal fluoride is faster and stacked, so that the precipitates on the surface of the glass are thicker and the haze of the glass is poorer; if the ratio of alkaline earth metal to alkali metal is higher than the proper range, the precipitation rate of alkaline earth metal fluoride may be higher than that of alkali metal fluoride, and the crystal precipitate particle size on the surface of the glass is larger, so that the surface roughness of the glass is larger.
In some embodiments, the weight ratio of the alkali metal fluoride to the alkaline earth metal fluoride is (1-3): 1, further may be (1-2): 1, further may be (1.5-2.5): 1, and may be selected from the following ranges consisting of one or two of the following ratios: 1:1, 1.05:1, 1.1:1, 1.15:1, 1.2:1, 1.25:1, 1.3:1, 1.35:1, 1.4:1, 1.45:1, 1.5:1, 1.55:1, 1.6:1, 1.65:1, 1.7:1, 1.75:1, 1.8:1, 1.85:1, 1.9:1, 1.95:1, 2:1, 2.05:1, 2.1:1, 2.15:1, 2.2:1, 2.25:1, 2.3:1, 2.35:1, 2.4:1, 2.45:1, 2.5:1, 2.6:1, 2.7:1, 2.8:1, 2.9:1, 3:1, etc.
The ammonium bifluoride can provide more fluoride ions in the frosting composition, and the ratio of the weight of the ammonium bifluoride in the frosting composition to the sum of the weights of the alkali metal fluoride and the alkaline earth metal fluoride is controlled in a proper range, so that the frosting particle size is controlled. If the ratio of the weight of ammonium bifluoride to the sum of the weights of alkali metal fluoride and alkaline earth metal fluoride in the frosting composition is higher than the proper range, it may result in the formation of (NH 4) 2SiF 6 Excessive amount of particles has large particle size; if the ratio of the weight of ammonium bifluoride to the sum of the weights of alkali metal fluoride and alkaline earth metal fluoride in the frosting composition is below the proper range, uneven crystal frosting and local frosting stacking may result;
In some embodiments, the ratio of the weight of ammonium bifluoride to the sum of the weights of alkali metal fluoride and alkaline earth metal fluoride in the frosting composition is (2-5): 1; further, 1 may be (2.5 to 5), and further, 1 may be (2.6 to 4.4), and may be selected from the following ranges consisting of one or two of the following ratios: 2:1, 2.1:1, 2.2:1, 2.3:1, 2.4:1, 2.5:1, 2.6:1, 2.7:1, 2.8:1, 2.9:1, 3:1, 3.1:1, 3.2:1, 3.3:1, 3.4:1, 3.5:1, 3.6:1, 3.7:1, 3.8:1, 3.9:1, 4:1, 4.1:1, 4.2:1, 4.3:1, 4.4:1, 4.5:1, 4.6:1, 4.7:1, 4.8:1, 4.9:1, 5:1.
The alkali metal fluoride in the frosting composition, wherein the proportion of potassium fluoride and sodium fluoride is controlled in a proper range, helps to obtain a product with smaller surface roughness and higher haze. If the proportion of potassium fluoride and sodium fluoride in the alkali metal fluoride is higher than the proper range, crystal stacking may be caused, and the flatness of the frosted surface may be lowered; if the proportion of potassium fluoride and sodium fluoride in the alkali metal fluoride is below the proper range, uneven crystal distribution may be caused, thereby affecting the frosting effect.
In some embodiments, the frosting composition comprises 100 parts by weight of the total weight of the frosting composition.
In some embodiments, the weight ratio of potassium fluoride to sodium fluoride in the alkali metal fluoride is (0.5 to 1.5): 1, more preferably (0.75 to 1.5): 1, still more preferably (1 to 1.5): 1, and further preferably one or two of the following ranges may be selected as the weight ratio: 0.5:1, 0.55:1, 0.6:1, 0.65:1, 0.75:1, 0.8:1, 0.85:1, 0.9:1, 0.95:1, 1.0:1, 1.05:1, 1.1:1, 1.15:1, 1.2:1, 1.25:1, 1.3:1, 1.35:1, 1.4:1, 1.45:1, 1.5:1, etc.
The proportion of calcium fluoride and magnesium fluoride in alkaline earth metal fluoride in the frosting composition is controlled in a proper range according to parts by weight, so that a product with smaller precipitated crystal particles and better distribution can be obtained. If the ratio of calcium fluoride to magnesium fluoride in the alkaline earth metal fluoride is higher than the proper range, it is possible to cause the grain size to be larger, and the grain size to be higher than the intended level; if the ratio of calcium fluoride and magnesium fluoride in the alkaline earth metal fluoride is below the proper range, small particle crystals may be caused to stack, thereby affecting haze.
In some embodiments, the weight ratio of the calcium fluoride to the magnesium fluoride in the alkaline earth metal fluoride is 0.5-1.2, may be 0.5-1, may be 0.6-1, and may be selected from one or two of the following ranges: 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, 1.1:1, 1.2:1, etc.
In some embodiments, the frosting composition comprises, in parts by weight: 25-29 parts of ammonium bifluoride, 3-6 parts of alkali metal fluoride, 2-5 parts of alkaline earth metal fluoride, 2.2-3 parts of sodium sulfate, 3-5 parts of ammonia sulfate, 16-20 parts of sulfuric acid, 9-12 parts of nitric acid, 6-10 parts of acetone and 16-29 parts of water; wherein the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride; the alkaline earth metal fluoride includes one or both of calcium fluoride and magnesium fluoride; the total weight of the frosting composition is 100 parts.
In some embodiments, the frosting composition comprises, in parts by weight: 26-29 parts of ammonium bifluoride, 4-6 parts of alkali metal fluoride, 2-4 parts of alkaline earth metal fluoride, 2.5-3 parts of sodium sulfate, 3.5-5 parts of ammonia sulfate, 17-20 parts of sulfuric acid, 9-12 parts of nitric acid, 7-9 parts of acetone and 16-28 parts of water; wherein the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride; the alkaline earth metal fluoride includes one or both of calcium fluoride and magnesium fluoride; the total weight of the frosting composition is 100 parts.
In some embodiments, the frosting composition comprises, in parts by weight: 26-29 parts of ammonium bifluoride, 2-3 parts of potassium fluoride, 2-3 parts of sodium fluoride, 1-2 parts of magnesium fluoride, 1-2 parts of calcium fluoride, 2.5-3 parts of sodium sulfate, 3.5-5 parts of ammonia sulfate, 17-20 parts of sulfuric acid, 9-12 parts of nitric acid, 7-9 parts of acetone and 16-28 parts of water; wherein the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride; the alkaline earth metal fluoride includes one or both of calcium fluoride and magnesium fluoride; the total weight of the frosting composition is 100 parts.
In a second aspect of the present invention, there is provided a frosting liquid obtained by aging a mixed liquid comprising the frosting composition according to the first aspect.
In some embodiments, the frosting liquid is prepared by a method comprising the steps of: and mixing the components of the frosting composition, standing and curing for 24-54 hours at 20-25 ℃ to obtain the frosting liquid.
Curing: the process of reacting the frosting component (alkali metal + alkaline earth metal + ammonium bifluoride + sodium sulfate + ammonium sulfate) with acetone in an acidic environment (sulfuric acid + nitric acid) to form a suspension is also known as aging. The time of standing and curing after the frosting composition is mixed is controlled within a proper range, which is favorable for obtaining the frosting liquid with good uniformity and moderate acidity. If the standing curing time of the frosting composition after mixing is higher than a proper range, a part of components can be settled due to excessively long reaction time, and suspension cannot be formed; if the standing curing time after the mixing of the frosting composition is lower than the proper range, the short reaction time may result in that the components do not reach the frosting component effect, the partial solid components are not uniform in the frosting component, and the frosting effect is affected.
In some embodiments, the components of the frosting composition are mixed and left to stand and cure for 24-54 hours at 20-25 ℃ to prepare the frosting liquid, the left-standing and curing time can be further 24-50 hours, further 30-50 hours, and one or two of the following time intervals can be selected: 24h, 25h, 26h, 27h, 28h, 29h, 30h, 31h, 32h, 33h, 34h, 35h, 36h, 37h, 38h, 39h, 40h, 41h, 42h, 43h, 44h, 45h, 46h, 47h, 48h, 49h, 50h, 51h, 52h, 53h, 54h, etc.
The pH value of the frosting liquid is controlled in a proper range, which is helpful for improving the stability of the frosting liquid and the efficiency of the frosting treatment process. If the pH value of the frosting liquid is higher than a proper range, the surface structure of the high-alumina glass is not damaged locally, and the frosting effect is poor; if the pH value of the frosting liquid is lower than the proper range, the acidity is possibly too high, a uniform crystal layer is not formed, and the etching depth is different, so that uneven frosting and uneven apparent flatness are caused.
In some embodiments, the pH of the frosting liquid is 0.5 to 2.5, further may be 0.5 to 2, further may be 0.5 to 1.5, and may be selected from the following pH or a range of two: 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5.
In a third aspect of the present application, a method for preparing a high alumina glass with a sparkling sand effect is provided, which can prepare a high alumina glass with a sparkling sand effect.
The frosting liquid of the second aspect of the present application can be used in the production method described in the third aspect.
In some embodiments, the method for preparing the flash sand effect high alumina glass comprises the following steps:
s300: acid treatment is carried out on the high-alumina glass substrate by using an acid treatment liquid, so as to prepare an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
S500: performing frosting treatment on the acid-treated glass substrate by using a frosting liquid to prepare a frosted glass substrate;
s700: carrying out chemical polishing treatment on the frosted glass substrate by using polishing solution to obtain a chemically polished glass substrate;
s800: and cleaning the glass substrate subjected to chemical polishing treatment to obtain a glass product with a flash sand effect.
In some embodiments, the method for preparing the flash sand effect high alumina glass comprises the following steps:
s300: acid treatment is carried out on the high-alumina glass substrate by using an acid treatment liquid, so as to obtain an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
S500: performing frosting treatment on the acid-treated glass substrate for 200-300 s by using a frosting solution to obtain a frosted glass substrate;
s700: carrying out chemical polishing treatment on the frosted glass substrate by using polishing solution to obtain a chemically polished glass substrate;
s800: and cleaning the glass substrate subjected to chemical polishing treatment to obtain a glass product with a flash sand effect.
In some embodiments, the method for preparing the flash sand effect high alumina glass comprises the following steps:
s300: acid treatment is carried out on the high-alumina glass substrate for proper time by using acid treatment liquid, so as to obtain an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
S500: performing frosting treatment on the acid-treated glass substrate for 200-300 s by using a frosting solution to obtain a frosted glass substrate;
s700: carrying out chemical polishing treatment on the frosted glass substrate for a proper time by using polishing solution to obtain a chemically polished glass substrate;
s800: and cleaning the glass substrate subjected to chemical polishing treatment to obtain a glass product with a flash sand effect.
In some embodiments, the frosting liquid may be selected from the frosting liquids of the second aspect.
The frosting composition is matched with an acidic pretreatment process when used in a frosting process, and has higher frosting efficiency on high-alumina glass; the frosting liquid does not contain inorganic filler, has stable composition and low frequency of replacement, does not generate chlorine-containing wastewater, and has less environmental pollution.
In the traditional technology, concentrated acid is often adopted to pretreat the surface of glass, for example, a mixed solution of sulfuric acid and hydrochloric acid, wherein the concentration of the sulfuric acid is 95-98%, and the concentration of the hydrochloric acid is 32-37%. The concentrated acid has lower efficiency when being used for pretreatment of the high-alumina glass, and cannot well achieve the purpose of preliminarily damaging the surface layer structure of the high-alumina glass substrate.
The acid concentration of the acid pretreatment liquid is in a proper range, so that the efficiency of the subsequent frosting treatment is improved, and the frosting treatment time is reduced by 12-24 hours; if the contents of hydrofluoric acid and sulfuric acid in the acidic pretreatment liquid are higher than the proper range, the inner layer structure of the high-alumina glass can be damaged, so that the etching is uneven after excessive frosting; if the contents of hydrofluoric acid and sulfuric acid in the acidic pretreatment liquid are lower than the proper range, the surface structure of the high-alumina glass is not damaged locally, and partial frosting and partial sanding are not carried out locally. If the content of hydrofluoric acid in the acidic treatment liquid is higher than a proper range, the structural damage to the surface of the high-alumina glass in the pretreatment process may be serious, the uniformity of crystal precipitation distribution of crystals on the surface of the glass after frosting treatment is poor, and further the haze uniformity of the product is poor; if the content of hydrofluoric acid in the acidic pretreatment liquid is lower than the proper range, the corrosion effect of the pretreatment process on the surface of the high-alumina glass is not obvious, and the efficiency of the subsequent frosting treatment process is lower. In some embodiments, the acidic treatment solution contains 4g/mL to 6g/mL of hydrofluoric acid, more preferably 5g/mL to 6g/mL of hydrofluoric acid, still more preferably 5g/mL to 5.5g/mL of hydrofluoric acid.
In some embodiments, the acidic treatment solution contains 3 g/mL-5 g/mL of sulfuric acid, more preferably 4 g/mL-5 g/mL of sulfuric acid, still more preferably 4.5 g/mL-5 g/mL of sulfuric acid.
In some embodiments, the acidic treatment solution contains 4 g/mL-6 g/mL of hydrofluoric acid and 3 g/mL-5 g/mL of sulfuric acid, further may contain 5 g/mL-6 g/mL of hydrofluoric acid and 4 g/mL-5 g/mL of sulfuric acid, and further may contain 5 g/mL-5.5 g/mL of hydrofluoric acid and 4.5 g/mL-5 g/mL of sulfuric acid.
The acid concentration of the polishing solution is in a proper range, which is favorable for removing edges, bulges and sharp parts of the frosted crystal body by chemical polishing; the hand feeling comfort level is improved; if the contents of hydrofluoric acid and sulfuric acid in the polishing liquid are higher than the proper ranges, the generated crystal structure may be damaged; if the contents of hydrofluoric acid and sulfuric acid in the polishing solution are lower than the proper ranges, the edges and corners, bulges and sharp polishing of part of crystals may be incomplete, and the roughness is affected. If the content of hydrofluoric acid in the polishing solution is higher than the proper range, the generated crystal structure may be damaged, so that the frosting effect is poor; if the content of hydrofluoric acid in the polishing solution is lower than the proper range, the edges and corners, bulges and sharp polishing of part of crystals may be incomplete, and the roughness is affected.
In some embodiments, the polishing solution contains 7 g/mL-9 g/mL hydrofluoric acid, more preferably 7.5 g/mL-8.5 g/mL sulfuric acid, and still more preferably 7.5 g/mL-8 g/mL sulfuric acid.
In some embodiments, the polishing solution contains 55 g/mL-65 g/mL sulfuric acid, more preferably 57 g/mL-62 g/mL sulfuric acid, still more preferably 58 g/mL-62 g/mL sulfuric acid.
In some embodiments, the polishing solution contains 7 g/mL-9 g/mL hydrofluoric acid and 55 g/mL-65 g/mL sulfuric acid, more preferably 7.5 g/mL-8.5 g/mL hydrofluoric acid and 57 g/mL-62 g/mL sulfuric acid, still more preferably 7.5 g/mL-8 g/mL hydrofluoric acid and 58 g/mL-62 g/mL sulfuric acid.
In some embodiments, the method for producing a sparkling sand effect high alumina glass further comprises cleaning the high alumina glass substrate prior to the acid treatment.
In some embodiments, the method for preparing the high alumina glass with the flash sand effect further comprises the step of protecting the side surface and the side surface of the glass substrate which do not need etching by acid-resistant ink coating before the acid treatment is carried out.
In some embodiments, the method for preparing the high alumina glass with the flash sand effect further comprises the steps of cleaning and drying the glass substrate after the acid treatment before the frosting treatment is carried out.
In some embodiments, the method for preparing the flash sand effect high alumina glass further comprises ultrasonic cleaning of the frosted glass substrate before chemical polishing.
In some embodiments, the method for preparing the flash sand effect high alumina glass comprises the following steps:
s100: cleaning the high-alumina glass substrate;
s200: protecting one side surface of the glass substrate which does not need etching by an acid-resistant ink coating;
s300: acid treatment is carried out on the high-alumina glass substrate by using an acid treatment liquid, so as to obtain an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
S400: cleaning and drying the glass substrate subjected to acid treatment;
s500: performing frosting treatment on the acid-treated glass substrate for 200-300 s by using a frosting solution to obtain a frosted glass substrate;
s600: ultrasonic cleaning is carried out on the glass substrate subjected to frosting treatment;
s700: carrying out chemical polishing treatment on the frosted glass substrate by using polishing solution to obtain a chemically polished glass substrate;
S800: and cleaning the glass substrate subjected to chemical polishing treatment to obtain a glass product with a flash sand effect.
The time of the acid pretreatment liquid is in a proper range, which is favorable for reducing the frosting time and improving the efficiency; if the time of the acidic pretreatment liquid is higher than the proper range, the inner layer structure of the high-alumina glass can be damaged, so that the etching is uneven after excessive frosting; if the time of the acidic pretreatment liquid is lower than the proper range, the surface structure of the aluminum glass is not damaged locally, and partial frosting and partial sanding are not carried out.
In some embodiments, the time of the acid treatment is 300s to 600s, more preferably 330s to 570s, still more preferably 360s to 540s, and further preferably one or two of the following intervals: 300s, 330s, 360s, 390s, 420s, 450s, 480s, 510s, 540s, 570s, 600s, etc.
The frosting treatment time is in a proper range, so that uniformity of the frosting is facilitated, and proper haze is controlled; if the time of the frosting treatment is higher than the proper range, partial frosting stacking and poor apparent flatness of the product are possible; if the time of the frosting treatment is less than the proper range, the frosting may be uneven, the crystal growth speed may be uneven, and the frosting may be insufficient.
In some embodiments, the time of the frosting treatment is 200 s-300 s, further may be 220 s-300 s, further may be 240 s-300 s, and may be selected from one or two of the following intervals: 200s, 210s, 220s, 230s, 240s, 250s, 260s, 270s, 280s, 290s, 300s, etc.
The time of chemical polishing treatment is in a proper range, which is favorable for polishing edges, bulges and sharpness of crystals after frosting, and the roughness and the flatness are improved; if the time of the chemical polishing treatment is higher than the proper range, the generated crystal structure may be damaged, resulting in poor frosting effect; if the chemical polishing treatment time is less than the proper range, the polishing may be incomplete in the corners, protrusions, and sharpness of a part of the crystal, and the roughness may be affected.
In some embodiments, the temperature of the chemical polishing treatment is 40±0.5 ℃, the cumulative treatment time is 100s to 200s, further 120s to 180s, further 150s to 180s, and further one or two of the following intervals may be selected: 100s, 105s, 120s, 135s, 150s, 165s, 180s, 195s, 200s, etc.
In some embodiments, the number of times of the chemical polishing treatment is 8-13, and the treatment time is 10 s-15 s.
In some embodiments, the method for preparing the high alumina glass with flash sand effect comprises ultrasonic cleaning at 60±0.5 ℃ for 150s to 200s, further 160s to 180s, and further one or two of the following time intervals: 150s, 155s, 160s, 165s, 170s, 175s, 180s, 185s, 190s, 195s, 200s, etc.
In a fourth aspect of the application, a high alumina glass with a flash sand effect is provided, and the high alumina glass is prepared by the preparation method in the third aspect.
In some embodiments, the haze of the flash sand effect high alumina glass is 90% -99%, further may be 90% -98.5%, and may be selected from the following range of one haze or two types: 90%, 90.5%, 91%, 91.5%, 92%, 92.5%, 93%, 93.5%, 94%, 94.5%, 95%, 95.5%, 95.7%, 96%, 96.5%, 97%, 97.4%, 97.5%, 98%, 98.5%, 99%, etc.
In some embodiments, the surface roughness of the flash sand effect high alumina glass is 3-6 μm, and the flash sand effect high alumina glass can be selected from the following one surface roughness or two intervals: 3.1 μm, 3.2 μm, 3.3 μm, 3.4 μm, 3.5 μm, 3.6 μm, 3.7 μm, 3.8 μm, 3.9 μm, 4 μm, 4.1 μm, 4.2 μm, 4.3 μm, 4.4 μm, 4.5 μm, 4.6 μm, 4.7 μm, 4.8 μm, 4.9 μm, 5 μm, 5.1 μm, 5.2 μm, 5.3 μm, 5.4 μm, 5.5 μm, 5.6 μm, 5.7 μm, 5.8 μm, 5.9 μm, 6 μm, etc.
The crystal precipitate with smaller particles and even distribution is formed on the surface of the high-alumina glass product prepared by the preparation method of the high-alumina glass with the flash sand effect, and the surface roughness of the frosted surface of the high-alumina glass product with the flash sand effect is only 3-6 mu m, and the haze can reach 90-98%.
In a fifth aspect of the present application, a glass article is provided, comprising a glass structure, the glass structure being made from the sparkling sand effect high alumina glass of the fourth aspect.
When the glass product with lower surface roughness (3-6 mu m) and higher haze (90-98%) is used for a glass structure, and is applied to the fields of display screens, windows, mobile phone back covers, glassware and the like, the surface of the product is fine and smooth, glare is not easy to generate, and the glass product has better mechanical properties.
In order that the invention may be more readily understood and put into practical effect, the following more particular examples and comparative examples are provided as reference.
Unless otherwise specified, the raw materials used in each of the following tests are commercially available and the performance test methods are as follows:
the testing method comprises the following steps:
haze test method: a beam of parallel light from a standard 'c' light source is vertically irradiated onto a transparent or semitransparent film, sheet or plate, and due to scattering caused by the inside and the surface of the material, part of the parallel light deviates from the incidence direction by more than the percentage of the ratio of the scattered luminous flux Td of 2.5 DEG to the luminous flux T2 transmitted through the material; in the present application, the haze range is a preferable range when the haze range is 90% to 98%.
The method for testing the surface roughness and the flatness comprises the following steps: a surface roughness tester; in the present application, the range of the surface roughness is preferably 3 to 5. Mu.m.
The following are specific examples.
TABLE 1 composition of the frosting compositions of examples 1 to 4 and comparative examples 1 to 3
TABLE 2 composition of the frosting compositions of examples 1 to 4 and comparative examples 1 to 3
Example 1:
preparing a frosting liquid: the respective compositions were mixed and stirred in accordance with the composition of the frosting sand in Table 1, and left to stand at 23℃for curing for 36 hours.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: wherein the acid content is 8g/mol and the sulfuric acid content is 60g/mol in grams per mole.
The whole frosting process of the high-alumina glass comprises the following steps:
s100: cleaning the high-alumina glass substrate;
s200: protecting one side surface of the glass substrate which does not need etching by an acid-resistant ink coating;
s300: acid treatment is carried out on the high-alumina glass substrate for 360s by using an acid treatment liquid, so as to obtain an acid-treated glass substrate; -
S400: cleaning the glass substrate subjected to acid treatment for 60s and drying;
s500: performing frosting treatment on the acid-treated glass substrate for 200-300 s by using a frosting solution to obtain a frosted glass substrate;
s600: ultrasonic cleaning the frosted glass substrate for 60s;
s700: performing chemical polishing treatment (polishing at 40 ℃ for 150s (15 seconds/time, 10 times of polishing)) on the frosted glass substrate by using a polishing solution to obtain a chemically polished glass substrate;
s800: the chemically polished glass substrate was cleaned (60 ℃ C., 180 s) to obtain a glass product having a sparkling sand effect.
The test was carried out on the high alumina glass with the effect of flash sand by the method, and the haze of the high alumina glass product with the effect of flash sand was 90% and the roughness Ra was 6. Mu.m.
Example 2:
preparing a frosting liquid:
the frosting composition in example 2 is shown in table 1, and the method of preparing the frosting liquid is the same as in example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of example 2 is basically the same as that of example 1 except that in step S500, the frosting treatment time is 280S.
The same test method as in example 1 was used to measure 95% haze and 4.2 μm roughness Ra of the high alumina glass product having the effect of flash sand.
Example 3:
preparing a frosting liquid:
the frosting composition in example 3 is shown in table 1, and the method of preparing the frosting liquid is the same as in example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of example 3 is basically the same as that of example 1 except that in step S500, the frosting treatment time is 260S.
The same test method as in example 1 was used to measure 96% haze and 3.8 μm roughness Ra of the high alumina glass product having the effect of flash sand.
Example 4:
preparing a frosting liquid:
the frosting composition in example 4 is shown in table 1, and the method of preparing the frosting liquid is the same as in example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of example 4 is substantially the same as that of example 1, except that in step S500, the frosting treatment time is 240S; in the step S700, the chemical polishing time is 180S (15 seconds/time, 12 times of polishing)
The same test method as in example 1 was used to measure the haze 98% and the roughness Ra 3 μm of the high alumina glass product having the effect of the flash sand, and the surface roughness characterization result of the glass is shown in fig. 1.
Comparative example 1:
preparing a frosting liquid:
the frosting composition of comparative example 1 is shown in table 1, and the method of preparing the frosting liquid is the same as that of example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of comparative example 1 was substantially the same as in example 1 except that in step S500, the time of the frosting treatment was 240S; in the step S700, the chemical polishing time is 180S (15 seconds/time, 12 times of polishing)
The same test method as in example 1 was used to measure that the haze of the high alumina glass product having the effect of the flash sand was 97% and the roughness Ra was 9.3 μm. The glass product obtained in comparative example 1 has a larger roughness presumably because the alkali earth metal fluoride content in the frosting composition is higher, which is likely to cause stacking of alkali metal fluorosilicate crystals, while the potassium fluoride content is significantly higher than the sodium fluoride content and the magnesium fluoride content is higher, and the proportion of crystal precipitates on the glass surface is unbalanced, which in turn causes a larger roughness of the glass surface.
Comparative example 2:
preparing a frosting liquid:
the frosting composition of comparative example 2 is shown in table 1, and the method of preparing the frosting liquid is the same as that of example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of comparative example 2 was substantially the same as in example 1 except that in step S500, the time of the frosting treatment was 240S; in the step S700, the chemical polishing time is 180S (15 seconds/time, 12 times of polishing)
The same test method as in example 1 was used to measure that the haze of the high alumina glass product having the effect of the flash sand was 60% and the roughness Ra was 3.9 μm. The lower haze of the glass product obtained in comparative example 2 is presumably due to the lower ammonium bifluoride content in the frosting composition, which may result in slow growth of alkali metal fluoride and alkaline earth metal fluoride crystals, ultimately resulting in a larger roughness of the frosted glass product.
Comparative example 3:
preparing a frosting liquid:
the frosting composition of comparative example 3 is shown in table 1, and the method of preparing the frosting liquid is the same as that of example 1.
Acidic treatment liquid: the acidic treatment liquid composition was as shown in Table 2.
Chemical polishing solution: the composition was the same as in example 1.
The whole frosting process of the high-alumina glass comprises the following steps:
the frosting process of comparative example 3 was substantially the same as in example 1 except that in step S500, the time of the frosting treatment was 240S; in the step S700, the chemical polishing time is 180S (15 seconds/time, 12 times of polishing)
The same test method as in example 1 was used to measure that the haze of the high alumina glass product having the effect of the flash sand was 78% and the roughness Ra was 12.2 μm. The lower haze of the glass product obtained in comparative example 2 is presumably due to the lower content of sulfuric acid in the frosting composition, which is only slightly higher than the levels of examples 1 to 4, resulting in the frosting composition being less acidic after standing and curing, which may cause a slower localized erosion of the high alumina glass surface structure, and eventually leading to a significantly increased roughness of the frosted glass product as compared to examples 1 to 4, and a similar decrease in haze.
Furthermore, through experimentation, the inventors have found that when chlorides are used in the frosting composition, the frosting crystals have a larger particle size and an excessive roughness. When acetone is removed from the frosting composition or other solvents with different properties are used, the frosting liquid settles after curing, a suspension cannot be formed, the frosting treatment process is less efficient, and the final glass product has larger roughness and poorer uniformity.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.
Claims (10)
1. The frosting composition is characterized by comprising the following components in parts by weight: 25-30 parts of ammonium bifluoride, 2-6 parts of alkali metal fluoride, 2-6 parts of alkaline earth metal fluoride, 2-3 parts of sodium sulfate, 2-5 parts of ammonia sulfate, 8-20 parts of sulfuric acid, 8-15 parts of nitric acid, 5-10 parts of acetone and 15-30 parts of water;
wherein, the liquid crystal display device comprises a liquid crystal display device,
the alkali metal fluoride comprises one or two of potassium fluoride and sodium fluoride;
The alkaline earth metal fluoride comprises one or two of calcium fluoride and magnesium fluoride;
the total weight of the frosting composition is 100 parts.
2. The frosting composition of claim 1, having one or more of the following characteristics:
the weight ratio of the alkali metal fluoride to the alkaline earth metal fluoride is (1-2.5): 1;
the ratio of the weight of ammonium bifluoride to the sum of the weights of alkali metal fluoride and alkaline earth metal fluoride is (2-5) 1;
the total weight of the frosting composition is 100 parts.
3. The frosting composition according to claim 1 or 2, comprising, in parts by weight: 26 to 29 parts of ammonium bifluoride, 4 to 6 parts of alkali metal fluoride, 2 to 4 parts of alkaline earth metal fluoride, 2.5 to 3 parts of sodium sulfate, 3.5 to 5 parts of ammonia sulfate, 17 to 20 parts of sulfuric acid, 9 to 12 parts of nitric acid, 7 to 9 parts of acetone and 16 to 28 parts of water.
4. A frosting liquid comprising the composition according to any one of claims 1 to 3, which is cured.
5. The masking liquid of claim 4, wherein one or both of the following characteristics are satisfied:
The frosting liquid is prepared by adopting a method comprising the following steps: mixing the components of the frosting composition, standing and curing for 24-54 hours at 20-25 ℃ to prepare the frosting liquid;
the pH value of the frosting liquid is 0.5-2.5.
6. The preparation method of the high-alumina glass with the flash sand effect is characterized by comprising the following steps of:
acid treatment is carried out on the high-alumina glass substrate by using an acid treatment liquid, so as to obtain an acid-treated glass substrate; wherein the high-alumina glass substrate contains 18 to 23 mass percent of Al 2 O 3 ；
Performing frosting treatment on the acid-treated glass substrate for 200s to 300s by using the frosting liquid according to claim 4 or 5 to obtain a frosted glass substrate;
carrying out chemical polishing treatment on the frosted glass substrate by using polishing solution to obtain a chemically polished glass substrate;
and cleaning the glass substrate subjected to chemical polishing treatment to obtain a glass product with a flash sand effect.
7. The method of manufacturing according to claim 6, wherein one or more of the following characteristics are satisfied:
the acidic treatment solution contains 4 g/mL-6 g/mL hydrofluoric acid and 3 g/mL-5 g/mL sulfuric acid;
the polishing solution contains 7-9 g/mL hydrofluoric acid and 55-65 g/mL sulfuric acid;
Pre-cleaning the high alumina glass substrate before the acid treatment;
the acid treatment time is 300 s-600 s;
the temperature of the chemical polishing treatment is 40+/-0.5 ℃, and the accumulated treatment time is 100-200 s;
the times of the chemical polishing treatment are 8-13 times, and the treatment time of each time is 10-15 s;
after the chemical polishing treatment is finished, ultrasonic cleaning is carried out at 60+/-0.5 ℃ for 150-200 s.
8. The high alumina glass with the flash sand effect is characterized by being prepared by adopting the preparation method of claim 6 or 7.
9. The sparkling sand effect high alumina glass according to claim 8, wherein the sparkling sand effect high alumina glass has a surface roughness of 3 μm to 6 μm.
10. A glass article comprising a glass structure prepared using the sparkling sand effect high alumina glass of claim 8 or 9.
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