CN111847894B - Preparation process of glass with scratch-resistant crystal diamond flash point effect - Google Patents
Preparation process of glass with scratch-resistant crystal diamond flash point effect Download PDFInfo
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- CN111847894B CN111847894B CN202010652465.0A CN202010652465A CN111847894B CN 111847894 B CN111847894 B CN 111847894B CN 202010652465 A CN202010652465 A CN 202010652465A CN 111847894 B CN111847894 B CN 111847894B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
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- 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
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Abstract
The invention belongs to the technical field of etched glass, and particularly relates to a preparation process of glass with scratch-resistant crystal diamond flash point effect, which comprises the following steps: the invention relies on the etching effect of fluoride on glass, and the etching effect and the glass surface generate multi-stage chemical reaction in acid liquor with certain concentration and variety to generate a nano-scale diamond-shaped microcrystal particle attachment layer which is uniformly distributed on the whole glass surface, thereby realizing the visual effect of cash light scintillation when the glass is exposed to light, and simultaneously having excellent performances of anti-reflection light, anti-scratch, anti-dust, anti-fingerprint and the like.
Description
Technical Field
The invention belongs to the technical field of chemical etching of scratch-resistant crystal diamond flash point effect glass, and particularly relates to a preparation process of the scratch-resistant crystal diamond flash point effect glass.
Background
Along with the improvement of the living standard of people, the requirements of people on the aspects of furniture decoration, business space partition and the like are also improved, the requirements of glass with the scratch-resistant crystal diamond flash point effect are greatly improved, but the purpose of realizing the crystal diamond flash point effect on the surface of the glass is generally realized by adopting a process of combining spray resin and metal flash powder in the production field of decorative glass, and the crystal diamond flash point effect glass realized by the physical spray coating process has the defects of easy aging, easy scratch, poor adhesive force, short service life and the like.
Disclosure of Invention
The invention aims to provide a preparation process of glass with a scratch-resistant crystal diamond flash point effect, developed scratch-resistant crystal diamond flash point effect glass products have a cash light flashing effect when exposed to light, different dazzling crystal diamond flash point visual effects are shown at different viewing angles, the product has excellent performances of reflection resistance, scratch resistance, dust resistance, fingerprint resistance and the like, can be widely applied to the fields of architectural decoration glass, high-end business space partitions, bath rooms, high-grade furniture, glass wall paintings and the like, and meets different requirements of people on glass decoration products.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation process of glass with scratch-resistant crystal diamond flash point effect comprises the following steps:
1) Preparing a glass etching solution according to the following percentage: NH (NH) 4 HF 2 12-25%、NaF 5-18%、HCL6-18%、HNO 3 5-15%、K 2 HPO 3 3-8%、NaNO 3 3-6%、(NH 4 ) 2 SiF 6 0.5-1.0 percent of sodium alkyl benzene sulfonate, 0.3-0.8 percent of sodium alkyl benzene sulfonate, 5-8 percent of viscosity regulator and H 2 O15-28%；
2) Carrying out silk-screen laminating protection on the surface of the glass original sheet which does not need to be etched by using etching-resistant ink;
3) Cleaning one surface of a glass original sheet to be etched with a pretreatment solution, and putting the glass original sheet into an etching solution in a wet state for soaking type etching treatment;
4) Controlling the temperature of the etching solution to be 18-25 ℃, soaking and etching for 5-8 minutes, taking out the etched glass from the etching solution after reaching the soaking and etching time, then cleaning the etched glass by pure water, and air-drying or drying the glass to obtain the scratch-resistant crystal diamond flash point effect glass product.
Further, in the step 1), after the raw materials are sequentially added into the glass etching solution according to the formula of the etching solution during preparation, the glass etching solution is stirred until the glass etching solution is in a uniform and stable supersaturated solution state, wherein the supersaturated solution refers to a solution which is not precipitated when the concentration of solute in the solution exceeds the solubility of the solute at a certain temperature and under a certain pressure, and the phenomenon is called a supersaturation phenomenon, wherein the supersaturated solution is unstable, and if the solution is stirred, the solution is vibrated, the wall of a container is rubbed, or solid seed crystals are put into the solution, excessive solute in the solution is immediately crystallized and precipitated, and the glass etching solution is kept stand and aged for 36 to 72 hours at the normal temperature.
Further, the composition of the pretreatment solution in the step 3) is 15% of sulfuric acid, 8% of hydrofluoric acid and 77% of water.
The mechanism of the invention is as follows: fluoride in the formula of the etching solution is used as a main raw material for etching glass, so that the effect of forming nano-grade frosted particles on the surface of the glass is achieved, and acid solutions of different types and different concentrations, ammonium fluosilicate, sodium nitrate and the like can control the structure and the shape of formed microcrystal particles together, so that the purposes of determining the structure and determining the performance of the structure by components are achieved; the viscosity regulator is used for regulating the viscosity of the liquid medicine, so as to be beneficial to realizing the purpose of uniform etching, and the generated nano-scale microcrystalline diamond particles are uniformly distributed on the surface of the glass, thereby achieving the uniform crystal drilling effect, sodium alkyl benzene sulfonate is used as a surfactant to promote the formation of the frosted particles, the affinity of the liquid medicine and the surface of the glass is enhanced, and the uniform and ordered growth of crystal nuclei is promoted, thereby realizing the purpose of finer and more uniform frosted effect, playing the role of a catalyst, and the strength of the microcrystalline diamond-shaped particles formed on the surface of the glass is large, the adhesive force is strong, so that the glass has excellent scratch resistance.
The invention has the advantages that: the invention adopts a soaking type chemical etching process to manufacture scratch-resistant crystal diamond flash point effect glass, optimizes and innovates the components and content of an etching solution formula, and mixes a proper surface active substance and a viscosity regulator, and generates a multi-stage chemical reaction with the surface of the glass in acid liquor with certain concentration and variety depending on the etching effect of fluoride on the glass to generate a nano-scale diamond-shaped microcrystal particle attachment layer, thereby realizing the crystal diamond flash point etching effect on the surface of the glass, sodium alkyl benzene sulfonate is used as a surface active substance to promote the formation of frosted particles, the affinity of a liquid medicine and the surface of the glass is enhanced, and the uniform and ordered growth of crystal nuclei is promoted, thereby realizing the purpose of finer and more uniform frosted effect, playing the role of a catalyst, and in order to promote the etching solution to realize uniform and consistent chemical reaction on the surface of the glass, the purpose of adding the viscosity regulator is to regulate the degree of the etching solution, maintain the stability and the suspension effect of the supersaturated etching solution, realizing the chemical etching treatment on the surface of the glass, forming nano-scale diamond-shaped diamond particles with the thickness of 25-80nm on the surface of the glass, realizing uniform distribution of the whole glass, uniform visual fingerprint, and uniform distribution, thereby having excellent anti-scratch-resistance and anti-dust-reflection performance on the whole glass surface of the glass.
Drawings
FIG. 1 is a photomicrograph of a scratch resistant diamond flash point effect glass prepared in accordance with the present invention.
FIG. 2 is a microscope photograph of a common frosted glass.
Detailed Description
Example 1
1. Preparing a crystal diamond flash point effect glass etching solution (wt%) according to the following formula: NH 4 HF 2 22.3%、NaF 15.8%、HCL13.6%、HNO 3 11.8%、K 2 HPO 3 4.5%、NaNO 3 3.5%、(NH 4 ) 2 SiF 6 0.6 percent of sodium alkyl benzene sulfonate, 0.3 percent of viscosity regulator, 4.7 percent of H 2 O22.9 percent, adding the raw materials in turn according to the requirements of the etching process, then fully stirring the mixture evenly to form a uniform and stable supersaturated solution state, standing the mixture at the normal temperature for curing for 36 to 72 hours to obtain the etching solution meeting the requirements, and then starting the etching treatment work of the scratch-resistant crystal diamond flash point effect glass of the glass sheet;
2. carrying out silk-screen laminating protection on the surface of the glass original sheet which does not need to be etched by using etching-resistant ink;
3. cleaning the surface of the glass original sheet to be etched with a pretreatment solution, and putting the glass original sheet into an etching solution in a wet state for soaking type etching treatment;
4. controlling the temperature of the etching solution to be 18-25 ℃, and controlling the soaking etching time to be 5-8 minutes;
5. and after the requirement of the soaking etching time is met, the etched glass is taken out of the etching solution in time, then is cleaned by pure water, and is air-dried or dried to obtain the scratch-resistant crystal diamond flash point effect glass product.
Example 2
1. Preparing a crystal diamond flash point effect glass etching solution (wt%) according to the following formula: NH (NH) 4 HF 2 24.1%、NaF 15.3%、HCL13.6%、HNO 3 12.6%、K 2 HPO 3 4.2%、NaNO 3 3.5%、(NH 4 ) 2 SiF 6 0.5 percent of sodium alkyl benzene sulfonate, 0.3 percent of sodium alkyl benzene sulfonate, 5.1 percent of viscosity regulator and H 2 O20.8 percent, adding the raw materials in turn according to the requirements of the etching process, then fully stirring the mixture evenly, presenting a uniform and stable supersaturated solution state and being in a normal temperature stateStanding and curing for 36-72 hours under the state to obtain the etching solution meeting the requirements, and then starting the etching treatment work of the scratch-resistant crystal diamond flash point effect glass of the glass original sheet;
2. carrying out silk-screen laminating protection on the surface of the glass original sheet which does not need to be etched by using etching-resistant ink;
3. cleaning the surface of the glass original sheet to be etched with a pretreatment solution, and putting the glass original sheet into an etching solution in a wet state for soaking type etching treatment;
4. controlling the temperature of the etching solution to be 18-25 ℃, and controlling the soaking etching time to be 5-8 minutes;
5. and after the requirement of the soaking etching time is met, the etched glass is taken out of the etching solution in time, then the glass is cleaned by pure water and is air-dried or dried to obtain the scratch-resistant crystal diamond flash point effect glass product.
Example 3
1. Preparing a crystal diamond flash point effect glass etching solution (wt%) according to the following formula: NH 4 HF 2 23.8%、NaF 15.2%、HCL14.2%、HNO 3 12.7%、K 2 HPO 3 4.5%、NaNO 3 3.2%、(NH 4 ) 2 SiF 6 0.6 percent of sodium alkyl benzene sulfonate, 0.3 percent of viscosity regulator, 4.5 percent of H 2 O22.0 percent, adding the raw materials in sequence according to the requirements of the etching process, then fully stirring the mixture evenly to present a uniform and stable supersaturated solution state, standing and curing the mixture for 36 to 72 hours at the normal temperature state to obtain the special etching solution meeting the requirements, and then starting the etching treatment work of the scratch-resistant crystal diamond flash point effect glass of the glass original sheet;
2. carrying out silk-screen laminating protection on one side of the glass sheet, which does not need to be etched, by using etching-resistant ink;
3. cleaning the surface of the glass original sheet to be etched with a pretreatment solution, and putting the glass original sheet into an etching solution in a wet state for soaking type etching treatment;
4. controlling the temperature of the etching solution to be 18-25 ℃, and controlling the soaking etching time to be 5-8 minutes;
5. and after the requirement of the soaking etching time is met, the etched glass is taken out of the etching solution in time, then the glass is cleaned by pure water and is air-dried or dried to obtain the scratch-resistant crystal diamond flash point effect glass product.
Examples of the experiments
The relative performance of the scratch resistant diamond flash point effect glass prepared in examples 1-3 before and after chemical etching was tested according to experimental requirements and summarized as follows:
comparison of performance indexes before and after chemical etching of scratch-resistant crystal diamond flash point effect of glass sheet
| Performance of | Original glass before etching | Etching example 1 | Etching example 2 | Etching example 3 |
| Gloss (%) | 110.6 | 60.6 | 61.5 | 61.3 |
| Light transmittance (%) | 96.5 | 42.3 | 41.9 | 41.6 |
| Haze (%) | 0.03 | 50.5 | 49.8 | 49.6 |
| Roughness (mum) | 0 | 3.0 | 3.2 | 3.1 |
| Reflectance (%) | 8.8 | 3.9 | 4.2 | 4.1 |
Claims (1)
1. A preparation process of glass with scratch-resistant crystal diamond flash point effect is characterized by comprising the following steps:
1) Preparing a glass etching solution according to the following mass percent: NH (NH) 4 HF 2 12-25%、NaF 5-18%、HCL6-18%、HNO 3 5-15%、K 2 HPO 3 3-8%、NaNO 3 3-6%、(NH 4 ) 2 SiF 6 0.5-1.0 percent of sodium alkyl benzene sulfonate, 0.3-0.8 percent of sodium alkyl benzene sulfonate, 5-8 percent of viscosity regulator and H 2 15-28% of O, wherein the sum of the mass percentages of the components is 100%, the glass etching solution is prepared by sequentially adding raw materials according to the formula of the etching solution, stirring until the glass etching solution is in a uniform and stable supersaturated solution state, and standing and curing for 36-72 hours at normal temperature;
2) Carrying out silk-screen laminating protection on one side of the glass sheet, which does not need to be etched, by using etching-resistant ink;
3) Cleaning one surface of a glass original sheet to be etched by using pretreatment liquid, and putting the glass original sheet into etching liquid to carry out soaking type etching treatment in a wet state, wherein the pretreatment liquid comprises 15% of sulfuric acid, 8% of hydrofluoric acid and 77% of water;
4) Controlling the temperature of the etching solution to be 18-25 ℃, soaking and etching for 5-8 minutes, taking out the etched glass from the etching solution after reaching the soaking and etching time, then cleaning the glass by pure water, and air-drying or drying the glass to obtain the scratch-resistant crystal diamond flash point effect glass product.
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| CN112321170B (en) * | 2020-12-22 | 2022-08-19 | 郑州恒昊光学科技有限公司 | Glass etching solution and method for simulating ceramic kiln-transmutation ice-patterned glass by using same |
| CN112390537B (en) * | 2020-12-22 | 2022-08-19 | 郑州恒昊光学科技有限公司 | Glass etching solution and method for preparing black glass with silk effect by adopting same |
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| CN116217085A (en) * | 2022-12-06 | 2023-06-06 | 许昌恒昊光学科技有限公司 | Glass etching liquid, manufacturing method of starlight effect on surface of lithium aluminum silicon glass and mobile phone shell |
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| GB470413A (en) * | 1936-02-14 | 1937-08-16 | Gen Electric Co Ltd | Improvements in or relating to the etching of glass |
| SU1675244A1 (en) * | 1989-10-16 | 1991-09-07 | Научно-производственное объединение "Хрусталь" | Solution for obtaining coarse-grain frosted glass surface |
| KR20090109198A (en) * | 2008-04-15 | 2009-10-20 | 주식회사 동진쎄미켐 | Etching and cleaning solution for glass in liquid crystal display device and etching method using the same |
| CN103086609A (en) * | 2011-11-04 | 2013-05-08 | 景志杰 | Glass frosting treatment agent |
| CN107954608A (en) * | 2017-12-14 | 2018-04-24 | 天津美泰真空技术有限公司 | A kind of glass substrate etching solution |
| CN110467354B (en) * | 2019-08-27 | 2021-10-01 | Oppo广东移动通信有限公司 | Frosted glass, preparation method thereof, glass rear cover and electronic equipment |
| CN111362584B (en) * | 2020-03-21 | 2022-02-18 | 郑州恒昊光学科技有限公司 | High borosilicate glass etching solution and preparation method and application thereof |
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