CN113480195A - Preparation method of antibacterial glass - Google Patents
Preparation method of antibacterial glass Download PDFInfo
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- CN113480195A CN113480195A CN202110731755.9A CN202110731755A CN113480195A CN 113480195 A CN113480195 A CN 113480195A CN 202110731755 A CN202110731755 A CN 202110731755A CN 113480195 A CN113480195 A CN 113480195A
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- 239000011521 glass Substances 0.000 title claims abstract description 129
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000012266 salt solution Substances 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005345 chemically strengthened glass Substances 0.000 claims abstract description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 13
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000005341 toughened glass Substances 0.000 claims abstract description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 53
- 239000002994 raw material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000000845 anti-microbial effect Effects 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 238000003426 chemical strengthening reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 239000012459 cleaning agent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 24
- 238000005342 ion exchange Methods 0.000 abstract description 17
- 230000003287 optical effect Effects 0.000 abstract description 4
- 238000000137 annealing Methods 0.000 abstract 1
- 238000002834 transmittance Methods 0.000 description 10
- 230000008569 process Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 241000894006 Bacteria Species 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 238000005452 bending Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 230000005611 electricity Effects 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 6
- 238000005240 physical vapour deposition Methods 0.000 description 6
- 238000005728 strengthening Methods 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- 238000005496 tempering Methods 0.000 description 4
- 101710134784 Agnoprotein Proteins 0.000 description 3
- 239000004599 antimicrobial Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 239000005347 annealed glass Substances 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000029058 respiratory gaseous exchange Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000249 desinfective effect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000012812 general test Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000013003 hot bending Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000006058 strengthened glass Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Images
Classifications
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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
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/005—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to introduce in the glass such metals or metallic ions as Ag, Cu
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The application relates to a preparation method of antibacterial glass, which comprises the following steps: forming a salt solution, wherein the mass ratio of sodium nitrate in the salt solution is 75-90%, the mass ratio of sodium nitrite is 9-23%, the mass ratio of silver nitrate is 0.005-0.5%, the mass ratio of aluminum oxide is 0.5-7%, the mass ratio of silicon oxide is 0.5-5%, and the mass ratio of the rest substances is 0.15-1.5%; immersing the physically tempered glass into a salt solution to chemically strengthen the glass; the chemically strengthened glass is taken out and gradually cooled to room temperature. According to the application, the stress introduction technology and the ion exchange technology are adopted, the annealing glass is strengthened to introduce stress, so that the excellent impact resistance and optical performance of the glass are ensured, and the good antibacterial performance of the glass is also ensured.
Description
Technical Field
The application relates to a preparation method of glass, in particular to a preparation method of antibacterial glass.
Background
Glass is an amorphous inorganic nonmetallic material, and is generally prepared by taking a plurality of organic minerals as main raw materials and adding a small amount of auxiliary raw materials. With the development of glass industrialization and scale, glass with various purposes and various properties comes out in succession, the glass has the characteristics of high light transmittance, high temperature resistance, chemical corrosion resistance and the like, and the properties of radiation resistance, display, shielding, electric heating, strength, scratch resistance, antibiosis and the like can be integrated on the glass after deep processing. Nowadays, glass has become an important material in the fields of daily life, production and science, and is widely applied to the fields of buildings, daily use, art, medical treatment, chemistry, electronic components, instruments, automobiles, rail transit and the like.
Along with the improvement of life quality and protection consciousness, a large amount of bacteria can be generated in glass articles contacted with human beings in daily work and life, the body health is influenced, and even the safety of the human beings is seriously involved. Therefore, the application of the antibacterial glass in the fields of medical and sanitary environments, personal communication, public transportation means, special occasions with high requirements on sterile conditions and the like becomes a trend. The first method is to prepare hydroxyl (-OH) by adopting an organic Coating (CVD) gel method technology, and the antibacterial effect is achieved on the surface of the glass; the second is to adopt the technology of the magnetron sputtering method of the inorganic coating (PVD) to plate TiO2, and the catalytic reaction is carried out under the illumination condition, thus realizing the antibiosis on the glass surface; and thirdly, the ion exchange technology is adopted, and ions with antibacterial property and alkali metal ions on the surface of the glass are used for replacement, so that the antibacterial property is realized on the surface of the glass.
Referring to FIG. 4, which is a schematic structural diagram of the glass surface structure before and after ion exchange in the prior art for strengthening glass by ion exchange, as shown in the figure, when the antibacterial glass is prepared by the third preparation method, the glass is put into KNO3、AgNO3、NaNO3、KOH、Al2O3And SiO2Ion exchange is carried out by the mixed solution, and the ion exchange is carried out in the solutionThe exchange of K + ions with Na + in the glass provides strength and the exchange of Ag + in solution with Na + in the glass provides antibacterial properties, which the applicant has found to be at least a technical problem:
1. exchange of K +, Ag + ions and Na + can be mutually inhibited, so that the glass strength and the antibacterial property can hardly meet the requirements; 2. the method has long exchange time and high required proportion of Ag +, but the transmittance and the strength of the finally prepared antibacterial glass are reduced because the transmittance and the strength of the glass are influenced by silver ion (Ag +) exchange; 3. meanwhile, the whole preparation process has high requirements on the temperature rise and the temperature reduction of the glass, so that the surface of the glass is easy to crack.
Disclosure of Invention
In order to solve the technical problems in the prior art, the embodiment of the application provides a preparation method of antibacterial glass. The specific technical scheme is as follows:
in a first aspect, a method for preparing antibacterial glass is provided, which comprises the following steps: forming a salt solution, wherein the mass ratio of sodium nitrate in the salt solution is 75-90%, the mass ratio of sodium nitrite is 9-23%, the mass ratio of silver nitrate is 0.005-0.5%, the mass ratio of aluminum oxide is 0.5-7%, the mass ratio of silicon oxide is 0.5-5%, and the mass ratio of the rest substances is 0.15-1.5%; immersing the physically tempered glass into a salt solution to chemically strengthen the glass; the chemically strengthened glass is taken out and gradually cooled to room temperature.
In a first possible implementation of the first aspect, the method of forming a salt solution comprises the steps of: weighing raw materials according to the mass ratio of each component in the salt solution, and adding the raw materials into a salt tank of a chemical furnace; setting the heating temperature of the salt tank to 380-; after all the components in the raw materials are liquefied, waiting for 20-40 hours, and uniformly mixing to form a salt solution.
In a second possible implementation of the first aspect, the glass composition comprises: 50-70% of silicon dioxide, 0-18% of aluminum oxide, 8-15% of sodium oxide, 3-7% of magnesium oxide, 1-8% of potassium oxide, 1-8% of calcium oxide, 0.002% or less of iron oxide and 1.5% or less of boron oxide, zinc oxide, cerium oxide and zirconium oxide.
In a third possible implementation manner of the first aspect, the step of preheating the glass before immersing the physically tempered glass in the salt solution further comprises.
With reference to the third possible implementation manner of the first aspect, in a fourth possible implementation manner of the first aspect, the preheating temperature is 230-.
With reference to the first possible implementation manner of the first aspect, in a fifth possible implementation manner of the first aspect, the method for immersing the physically tempered glass into the salt solution includes the steps of placing the glass in a basket of a chemical furnace, and lowering the glass into a salt bath through the basket so that the glass is immersed into the salt solution.
In a sixth possible implementation manner of the first aspect, when the physically tempered glass is immersed in the salt solution, the temperature of the salt solution is 320-500 ℃, and the heat preservation time is 10 minutes-4 hours.
In a seventh possible implementation manner of the first aspect, the method for gradually cooling the chemically strengthened glass comprises the following steps: firstly, placing the chemically strengthened glass at the temperature of 230 ℃ and 300 ℃ and preserving heat for at least 2 hours; then placing the chemically strengthened glass at the temperature of 100-150 ℃, and preserving the heat for at least 1 hour; and finally, placing the chemically strengthened glass at room temperature until the glass is cooled to room temperature.
In an eighth possible implementation manner of the first aspect, the method further includes the following steps: and cleaning the cooled glass.
With reference to the eighth possible implementation manner of the first aspect, in a ninth possible implementation manner of the first aspect, when the glass is cleaned after cooling, the surface of the glass is cleaned sequentially with a citric acid solution, a cleaning agent, and deionized water.
Compared with the prior art, the application has the advantages that:
antimicrobial glass of the present applicationThe preparation method adopts the temperature difference stress introduction technology and the ion exchange technology, firstly strengthens the annealed glass to introduce stress, and ensures that the glass has excellent impact resistance and optical performance. AgNO for glass of physically tempered glass3、NaNO3、NaNO2、Al2O3And SiO2When the mixed solution is subjected to ion exchange, Ag + with positive electricity is formed on the surface of the glass, the Ag + with positive electricity can be adsorbed into bacteria with negative electricity to destroy the charge balance of the bacteria, the respiration and the reproduction of the bacteria are influenced, and the sterilization purpose is achieved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic flow chart illustrating steps of a method for manufacturing an antimicrobial glass according to an embodiment of the present disclosure.
Fig. 2 is a stress-stress layer graph after the antibacterial glass of an embodiment of the present application is subjected to a stress introducing technique.
FIG. 3 is a schematic structural view of the surface structure of a glass according to an embodiment of the present application before and after ion exchange.
FIG. 4 is a schematic structural view of the glass surface structure before and after ion exchange in the case of strengthening glass by the conventional ion exchange technique.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, embodiments of the present application.
In an embodiment of the present application, please refer to fig. 1, which is a schematic flow chart illustrating steps of a method for manufacturing an antimicrobial glass according to an embodiment of the present application, and as shown in the figure, the method 1 for manufacturing an antimicrobial glass includes the following steps 101 to 103, wherein:
Specifically, the raw materials are weighed according to the mass ratio of each component in the salt solution, wherein NaNO is375-90% by mass of NaNO29-23% of AgNO30.005-0.5% of Al2O30.5-7% of SiO2The mass ratio of the components is 0.5-5 percent, and the mass ratio of the rest components is 0.15-1.5 percent.
Then, the raw materials are added into a salt tank of a chemical furnace, the heating temperature of the salt tank is set to 380-.
After all the components in the raw materials are liquefied, waiting for at least 20-40 hours to uniformly mix the components to form a salt solution, reducing the mass ratio of Ag & lt + & gt in the salt solution prepared in the way, and adding Al2O3And SiO2And the catalyst and the adsorbent can realize rapid ion exchange in the subsequent step, and avoid the problem of light transmittance reduction caused by the interference of impurity ions (Ag +).
And 102, chemically strengthening. And immersing the physically tempered glass into a salt solution to chemically strengthen the glass.
Specifically, setting physical tempering parameters, selecting glass, and performing physical tempering on the glass, wherein the physical tempering parameters comprise: the preheating temperature is 550-620 ℃, the preheating time is 30-300s, the toughening temperature is 640-750 ℃, the toughening time is 30-200s, the toughening air pressure is 1000-15000KPa, the air distance is 10-50mm, and the cooling time is 30-300 s. The glass comprises the following components: 50-70% of silicon dioxide, 0-18% of aluminum oxide, 8-15% of sodium oxide, 3-7% of magnesium oxide, 1-8% of potassium oxide, 1-8% of calcium oxide, 0.002% or less of iron oxide, 1.5% or less of boron oxide, zinc oxide, cerium oxide and zirconium oxide, wherein the internal molecular structure of the glass is alundum.
After tempering is completed, the surface of the glass is wiped clean by using absolute alcohol, the glass is loaded into a hanging basket of a chemical furnace, the hanging basket is lifted into a preheating box of the chemical furnace, the preheating temperature of the preheating box is set to be 230-300 ℃, and the preheating time is at least 2 hours, so that a stress technology is introduced into the glass to ensure that the impact resistance and the optical performance of the glass are excellent, as shown in fig. 2, the stress-stress layer curve diagram is obtained after the stress technology is introduced into the antibacterial glass in one embodiment of the application. In this embodiment, the preheating temperature can be set to 230 ℃, 250 ℃, 280 ℃ or 300 ℃, but is not limited thereto, and the specific preheating temperature can be selected according to the actual production requirements (glass size and thickness).
After preheating, the basket is lowered into the salt bath to immerse the glass in the salt solution, the cover of the bath is closed, and the glass is kept in the salt solution at 500 ℃ for 10 minutes to 4 hours at 320-. In this embodiment, the temperature of the salt solution may be 320 ℃, 400 ℃, 440 ℃ or 500 ℃, and the holding time may be 10 minutes, 2 hours, 3 hours or 4 hours, but is not limited thereto, and the specific temperature and holding time of the salt solution may be selected according to the actual production requirements (the mass ratio of the components of the salt solution, the size and thickness of the glass).
And step 103, gradually cooling. The chemically strengthened glass is taken out and gradually cooled to room temperature.
Specifically, after the chemical strengthening is completed, the cover is opened, the basket is lifted to the preheating box of the chemical furnace, the basket drives the chemically strengthened glass to enter the preheating box, the temperature of the preheating box is set to be 230-.
After the first cooling and heat preservation is completed, the temperature of the preheating box is set to be 150 ℃., the second cooling and heat preservation is performed on the chemically strengthened glass at 150 ℃., the heat preservation time is at least 1 hour, so as to ensure that the temperature of the glass is reduced to 150 ℃.,. in this embodiment, the temperature of the preheating box may be 100 ℃, 120 ℃, 140 ℃ or 150 ℃, but is not limited thereto.
And after the second cooling and heat preservation, stopping heating the preheating box, and when the temperature in the preheating box is reduced to be below 100 ℃, reducing the hanging basket from the preheating box to the normal temperature environment, so that the chemically strengthened glass is placed at the room temperature until the glass is cooled to the room temperature.
In one embodiment, the method 1 for manufacturing antibacterial glass further includes a step 104 of cleaning the glass after cooling. Specifically, the glass surface is washed by citric acid solution, then by detergent, and finally by deionized water.
The beneficial effects of the preparation method of the antibacterial glass of the present application will be further explained below by combining with specific experimental data. The specific experimental process is as follows:
experiment process I, preparation of curved glass
The method comprises the following specific steps:
step 1: selecting a piece of plate glass, selecting a part without defects on the surface, and cutting the glass into the size of a product by using a diamond numerical control cutting machine;
step 2: grinding and chamfering the edge of the cut glass by using a numerical control edge grinding machine to form a C-shaped chamfer with uniform upper and lower chamfers;
step 3, corroding the edge area with the ink for glass to form a unique identifier, so as to facilitate tracking and tracing;
and 4, step 4: and (3) placing the glass on a tool according to a certain sequence for hot bending, heating to the softening point of the glass, and utilizing the self-weight forming of the glass to enable the glass to be attached to a mold to obtain the curved glass.
Second experiment Process, strengthened glass
The curved glass prepared in the first experimental process is strengthened according to the preparation method of the antibacterial glass, the existing organic Coating (CVD) gel method technology, the existing inorganic coating (PVD) magnetron sputtering method technology and the existing ion exchange technology, wherein the step of strengthening the curved glass according to the preparation method of the antibacterial glass is shown in the above embodiment, and no further description is given here, and the step of strengthening the curved glass according to the existing CVD gel method technology, the existing PVD magnetron sputtering method technology and the existing ion exchange technology is known to those skilled in the art, so that no further description is given here.
Third experiment procedure, test glass performance
And testing the transmittance, the bending strength (four-point bending test method), the bonding force and the antibacterial capability of the glass strengthened in the second experimental process according to the test methods of standard GJB 503-88 general test method for laminated glass of airplanes, JC 977-2005 chemical toughened glass, GB/T9286-1998G lattice test for paint films of colored paint and varnish, B/T21866-2008 method for antibacterial property test method and antibacterial effect of antibacterial paint (paint film). The test data are as follows:
a first group: the preparation method of the antibacterial glass comprises the following steps: the light transmittance is about 90 percent, the bending strength is about 350Mpa, the bonding force is 0 grade, and the antibacterial property is 99.9 percent;
second group: curved glass strengthened by the existing organic Coating (CVD) gel method technology: the light transmittance is about 75%, the bending strength is about 300Mpa, the bonding force is 2 grades, and the antibacterial property is 90%;
third group: the curved glass reinforced by the existing inorganic coating (PVD) magnetron sputtering method technology comprises the following steps: the light transmittance is about 75%, the bending strength is about 300Mpa, the bonding force is 3 grades, and the antibacterial property is 90%;
and a fourth group: the prior art is that the curved glass after being strengthened by ion exchange technology: the light transmittance is about 80%, the bending strength is about 300Mpa, the adhesive force is 0 grade, and the antibacterial property is 99%.
As shown in the first group of test data, the curved glass strengthened by the preparation method of the antibacterial glass has passed through the test verification standard, and compared with the fourth group of test data, the salt solution prepared again in the application ensures the high strength performance of the curved glass, so that the bending strength of the curved glass is greatly improved, and meanwhile, the light transmittance of the curved glass is also improved to a certain extent, so that the method can be obtained.
First group's test data compares again in second group and third group's test data, and the glass surface antibacterial property after this application is reinforceed is better, and the luminousness is higher to can obtain, the glass surface after this application is reinforceed forms the Ag +, that positive charges are taken to it can destroy bacterium charge balance, reaches the purpose of disinfecting. In addition, the strengthening process combining the existing CVD gel method technology and the existing PVD magnetron sputtering method technology is known, and the strengthened curved glass surface is plated with TiO2Film due to TiO2The film has poor adhesion performance and is easy to fall off when in contact, so that the problems that the curved glass reinforced by the existing CVD gel method technology and the existing PVD magnetron sputtering method technology has poor wear resistance, the antibacterial performance is easy to lose after long-term use and the like are caused.
In summary, the application provides a preparation method of antibacterial glass, which adopts a temperature difference induced stress technology and an ion exchange technology to firstly strengthen the annealed glass and induce stress, thereby ensuring the excellent impact resistance and optical performance of the glass. AgNO for glass of physically tempered glass3、NaNO3、NaNO2、Al2O3And SiO2When the mixed solution is subjected to ion exchange, Ag + with positive electricity is formed on the surface of the glass, the Ag + with positive electricity can be adsorbed into bacteria with negative electricity to destroy the charge balance of the bacteria, the respiration and the reproduction of the bacteria are influenced, and the sterilization purpose is achieved.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. The preparation method of the antibacterial glass is characterized by comprising the following steps:
forming a salt solution, wherein the mass ratio of sodium nitrate in the salt solution is 75-90%, the mass ratio of sodium nitrite is 9-23%, the mass ratio of silver nitrate is 0.005-0.5%, the mass ratio of aluminum oxide is 0.5-7%, the mass ratio of silicon oxide is 0.5-5%, and the mass ratio of the rest substances is 0.15-1.5%;
immersing the physically tempered glass into the salt solution to chemically strengthen the glass;
and taking out the chemically strengthened glass, and gradually cooling the glass to room temperature.
2. The method of claim 1, wherein the method of forming the salt solution comprises the steps of:
weighing raw materials according to the mass ratio of each component in the salt solution, and adding the raw materials into a salt tank of a chemical furnace;
setting the heating temperature of the salt tank to 380-480 ℃, and heating the raw materials;
after all the components in the raw materials are liquefied, waiting for 20-40 hours, and uniformly mixing to form the salt solution.
3. The method of claim 1, wherein the glass composition comprises: 50-70% of silicon dioxide, 0-18% of aluminum oxide, 8-15% of sodium oxide, 3-7% of magnesium oxide, 1-8% of potassium oxide, 1-8% of calcium oxide, 0.002% or less of iron oxide and 1.5% or less of boron oxide, zinc oxide, cerium oxide and zirconium oxide.
4. The method of claim 1, wherein the step of preheating the glass prior to immersing the physically tempered glass in the salt solution is further included.
5. The method as claimed in claim 4, wherein the preheating temperature is 230 ℃ and 300 ℃ and the preheating time is at least 2 hours.
6. The method of manufacturing antimicrobial glass according to claim 2, wherein the method of immersing the glass that has been physically tempered in the salt solution comprises the steps of placing the glass in a basket of the chemical furnace, lowering the glass into the salt bath through the basket, and immersing the glass in the salt solution.
7. The method for preparing antibacterial glass according to claim 1, wherein the temperature of the salt solution is 320-500 ℃ and the holding time is 10 minutes-4 hours when the glass which is physically tempered is immersed in the salt solution.
8. The method for preparing antibacterial glass according to claim 1, wherein the method for gradually cooling the glass after chemical strengthening comprises the following steps:
firstly, placing the chemically strengthened glass at the temperature of 230-300 ℃, and preserving heat for at least 2 hours;
then placing the glass subjected to chemical strengthening at the temperature of 100-150 ℃, and preserving the heat for at least 1 hour;
and finally, placing the chemically strengthened glass at room temperature until the glass is cooled to room temperature.
9. The method for preparing antibacterial glass according to claim 1, characterized by further comprising the steps of: and cleaning the cooled glass.
10. The method for preparing antibacterial glass according to claim 9, wherein the glass after the cleaning and cooling is finished is cleaned by sequentially adopting a citric acid solution, a cleaning agent and deionized water to clean the surface of the glass.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111417602A (en) * | 2018-07-16 | 2020-07-14 | 康宁股份有限公司 | Glass-ceramic articles having increased crush resistance and methods of making the same |
| CN111807718A (en) * | 2020-07-24 | 2020-10-23 | 江苏铁锚玻璃股份有限公司 | Preparation method of high-light-transmission and high-strength antibacterial glass |
| CN112996759A (en) * | 2018-09-11 | 2021-06-18 | 康宁股份有限公司 | Glass-based articles with improved resistance to cracking |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111417602A (en) * | 2018-07-16 | 2020-07-14 | 康宁股份有限公司 | Glass-ceramic articles having increased crush resistance and methods of making the same |
| CN112996759A (en) * | 2018-09-11 | 2021-06-18 | 康宁股份有限公司 | Glass-based articles with improved resistance to cracking |
| CN111807718A (en) * | 2020-07-24 | 2020-10-23 | 江苏铁锚玻璃股份有限公司 | Preparation method of high-light-transmission and high-strength antibacterial glass |
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