CN115432945B - Chemical strengthening method for improving weather resistance of nano microcrystalline glass - Google Patents
Chemical strengthening method for improving weather resistance of nano microcrystalline glass Download PDFInfo
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- CN115432945B CN115432945B CN202211214657.9A CN202211214657A CN115432945B CN 115432945 B CN115432945 B CN 115432945B CN 202211214657 A CN202211214657 A CN 202211214657A CN 115432945 B CN115432945 B CN 115432945B
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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
- C03C21/002—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 perform ion-exchange between alkali ions
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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 provides a chemical strengthening method for improving weather resistance of NaNO microcrystalline glass, which mainly relates to an ion exchange technology of NaNO microcrystalline glass, wherein glass is completely immersed in a salt bath for chemical strengthening, and the salt bath is NaNO with the purity of more than industrial grade 3 Compounding fluxing agent with purity over industrial grade and LiNO 3 . The one-step ion exchange chemical strengthening method can effectively improve the strength and weather resistance of the glass ceramics, and ensure the comprehensive performance of the glass when the glass is applied under the conditions facing complex climates such as mobile phones, vehicles and the like.
Description
Technical Field
The invention mainly relates to a nano microcrystalline glass ion exchange technology, in particular to a chemical strengthening method for improving weather resistance of nano microcrystalline glass.
Background
Consumer electronic devices and display devices (e.g., smartphones, tablets, electronic readers, and notebooks, etc.) often incorporate chemically strengthened glass articles for use as cover glass. In order to improve the shatter resistance of glass, strengthened nano microcrystalline glass is developed and becomes a standard of high-end consumer electronic equipment and display equipment. The nano microcrystalline glass is a multiphase composite material with a glass phase and a microcrystalline phase, which is formed by nuclear crystallization heat treatment. Meanwhile, the glass and ceramic material has the excellent properties of high optical transparency, good mechanical stability and customizable optical properties. Some practical and potential applications involve long-term use in high temperature and humidity and thermal cycling environments, and much work has been done around the direction of the impact of the manufacturing process and the application environment. The application range of the microcrystalline glass is continuously expanded, and the influence relationship of components, crystallization process and environmental parameters (temperature, strain and the like) on the structure, the performance and the application of the microcrystalline glass is required to be considered and more researches are carried out. The application environments of fields such as electronics, instruments, medicine and the like have complicated temperature and humidity changes, and with the deep development of the fields in the application of glass ceramics, the requirement is put forward on the research on the weather resistance of the glass ceramics. The microcrystalline glass for the mobile phone cover plate has high impact strength and high resistanceThe scraping performance is good, and the optical performance is adjustable, and the adoption of glass ceramics for mobile phone cover plate materials is becoming a trend at present. For the glass ceramics for the mobile phone cover plate, the glass ceramics also face complex use environments and are easy to be stained with water vapor, sweat stain, oil stain and the like, so that weather resistance is an important performance for the glass ceramics for the mobile phone cover plate. Compared with the matrix glass, the lithium aluminum silicon microcrystalline glass has the advantages that the silicon dioxide phase part is consumed into crystals, the network structure of the glass is destroyed, and the glass is more easily corroded by water. Li at the glass surface after chemical strengthening + Is replaced by Na + Due to Na + Weather resistance ratio of ions Li + The weatherability is poor, so that the weatherability of the glass becomes worse.
The existing chemical strengthening treatment method has complex process procedures, and most of the existing chemical strengthening treatment methods cannot balance strength and weather resistance. Such as CN202180006588.X, by controlling the content of lithium silicate and lithium phosphate, the glass is heat treated at 450-800 deg.C to chemical strengthening. CN201980072676.2, treating a lithium-containing glass substrate with two salt baths to obtain chemically strengthened glass ceramics; controlling the sodium nitrate content of the first salt bath and the lithium nitrate content of the second salt bath; controlling the temperature of the two salt baths to be 350-520 ℃; the time of the two salt baths is controlled, and the main purpose is to reduce surface defects. CN201911367307.4 is also two strengthening processes, the salt bath system is a potassium-sodium system, the temperature and time of the two processes are mainly controlled, and a heat dissipation process is arranged between the two strengthening processes. Mainly improves the anti-falling performance of the microcrystalline glass. None of the above relates to the problem of the balance of strength and weather resistance of glass ceramics. CN202110739360.3 strengthens glass by two-stage ion exchange, wherein the first stage ion exchange uses sodium ion to exchange lithium ions, and the strengthening time is long; the secondary reverse strengthening uses not more than 200ppm of lithium salt, and the treatment time is short. The proposal reduces sodium ions on the surface of the strengthened glass ceramic, can improve the environmental durability to a certain extent, but still uses two methods and has relatively complex operation.
Disclosure of Invention
The invention aims to provide a chemical strengthening method for improving the weather resistance of nano microcrystalline glass, which solves the technical problem of how to improve the strength of the microcrystalline glass after chemical strengthening and improve the weather resistance of the nano microcrystalline glass after ion exchange with low cost in the prior art.
The invention discloses a chemical strengthening method for improving weather resistance of NaNO microcrystalline glass, which is characterized in that glass is completely immersed in a salt bath for chemical strengthening, and only one-step strengthening is carried out, wherein the salt bath is NaNO with the purity of more than industrial grade 3 Compounding LiNO with purity above industrial grade 3 And a fluxing agent.
Working principle: ion exchange is a chemical diffusion and is an interdiffusion, the tendency of ion exchange is determined by the equilibrium constant K, for the same nano microcrystalline glass composition, na on the glass surface + The concentration is determined by the equilibrium constant K, the greater K, the Na on the glass surface + The higher the concentration, the poorer the weatherability, and K is related to the ratio of the organisms to the reactants, i.e
a g 、a S The activity of A ions in glass and molten salt respectively
b g 、b S The activity of B ion in glass and molten salt respectively
The greater the K value, the more complete the ion exchange reaction, the activity of the molten salt is represented by the formula
Activity of a\b ions in molten salt:
a S =a A γ A
b S =a B γ B
a A 、a B- coefficient of activity of ion A or ion B
γ A 、γ B Mole fraction of ions A or B
For binary system molten salt, the activity coefficient is
A' - - - -component interaction energy in molten salt
γ i -mole fraction of-i ions;
r- -gas constant
T- -absolute temperature
In many glasses, the ionic activity ratio is related to the ionic mole fraction, i.e
When Li in salt bath + When the concentration is increased, the equilibrium constant K can be reduced, thereby reducing Na on the surface of the glass + Concentration, thereby improving weatherability of the glass. However, the ion exchange enhancement principle (4) shows that the glass surface Na + The higher the concentration, the greater the stress generated.
In- - - - - - - - - - [ sigma ] C Compressive stress on the glass surface;
e modulus of elasticity of glass
Poisson's ratio of v- -glass
Delta V changes in volume after exchange
V ion volume before exchange
Glass surface Na + The concentration is reduced, and the stress on the surface of the glass is reduced, so that the strength of the glass is reduced.
The salt bath proportion is designed, and Li in salt bath with qualified weather resistance is obtained through experiments + Initial concentration, then gradually increase Li + Concentration, the activity of ions is changed through the coordination of fluxing agent, and Li with qualified strength is obtained + The upper limit concentration, thereby realizing the problem of weather resistance and strength balance.
Further, the salt bath lithium ion concentration is 200-1000ppm, preferably 300-700ppm.
Further, the flux concentration is not more than 1000ppm.
Further, the fluxing agent is one or more of calcium oxide, magnesium oxide, fluorite and aluminum oxide.
Further, the salt bath temperature is 350-550 ℃.
Further, the temperature of the salt bath is 380-450 DEG C
Further, the salt bath operation time is 1-24h.
Further, the salt bath operation time is 3-10h.
The second purpose of the invention is to protect the application of the chemical strengthening method for improving the weather resistance of the nano microcrystalline glass, which is used for improving the weather resistance of the nano microcrystalline glass after chemical strengthening.
The third purpose of the invention is to protect the nano microcrystalline glass which is prepared by the method, and the weather resistance of the nano microcrystalline glass reaches more than 89%, and meanwhile, the bending strength is ensured to reach more than 700 MPa.
Compared with the prior art, the invention has the following beneficial effects:
1. the one-step ion exchange chemical strengthening method can effectively improve the strength and weather resistance of the glass ceramics, and ensure the comprehensive performance of the glass when the glass is applied under the conditions facing complex climates such as mobile phones, vehicles and the like;
2. compared with the traditional two-step method, the one-step ion exchange chemical strengthening method has the advantages of simple process steps, convenient design of continuous production lines, low cost and high efficiency;
3. the invention adopts the fluxing agent to match with the salt bath for chemical strengthening, can reduce the treatment temperature, and is energy-saving and environment-friendly.
4. The invention adopts a one-step ion exchange chemical strengthening method to obtain nano microcrystalline glass, the weather resistance of which is more than 89 percent, and the bending strength of which is more than 700 MPa.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments.
Preparing a glass sheet: li is mixed with 2 0-Al 2 O 3 -SiO 2 Grinding and polishing after glass crystallization to form the specification: 149 x 72 x 0.7mm glass sheet, and then fully immersing the glass sheet in a salt bath for chemical strengthening.
Flexural Strength test: bending strength experiments were performed using a four-point bending tester, parameters: the upper span is 20mm, the lower span is 40mm, and the pressing speed is 10mm/min.
Weather resistance test: double 85 experiments were performed using a high temperature and high humidity test chamber, parameters: the humidity is 85%, the temperature is 85 ℃, the time is 14 days, and the surface state of the glass after double-85 experiments is observed. The transmittance of the glass after double 85 experiments was tested using a spectrophotometer to characterize weatherability, test wavelength range 380nm-780nm.
Example 1
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the main body of the salt bath is NaNO 3 Added LiNO 3 The concentration is 500ppm, the added fluxing agent is fluorite, the concentration is 200ppm, the salt bath temperature is 450 ℃, and the treatment time is 8 hours.
And the bending strength of the obtained nano microcrystalline glass is 770MPa. The glass surface state after double 85 experiments is good, and the light transmittance is 91%.
Example 2
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the main body of the salt bath is NaNO 3 Added LiNO 3 The concentration was 200ppm, and the flux added was magnesium oxide, aluminum oxide, and 500ppm. The salt bath temperature is 450 ℃ and the treatment time is 8 hours.
The bending strength of the obtained nano microcrystalline glass is 780MPa, and the surface state is good and the light transmittance is 90% after double-85 experiments.
Example 3
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the main body of the salt bath is NaNO 3 Added LiNO 3 The concentration was 600ppm, and the added flux was magnesium oxide, aluminum oxide, and 400ppm. The salt bath temperature is 450 ℃, and the treatment is carried out8h.
The bending strength of the obtained nano microcrystalline glass is 750MPa, and the surface state is good and the light transmittance is 92% after double-85 experiments.
As can be seen from examples 1-3, liNO was added at a suitable concentration 3 And after the fluxing agent, the microcrystalline glass with both strength and weather resistance can be obtained after chemical strengthening.
Comparative example 1
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the main body of the salt bath is NaNO 3 Added LiNO 3 The concentration was 0ppm without flux. The salt bath temperature is 450 ℃ and the treatment time is 8 hours.
The bending strength of the obtained nano microcrystalline glass is 800MPa, the surface of the glass is atomized after 14 days of double 85 treatment, the light transmittance is reduced to 64%, and the use requirement is not met.
Comparative example 2
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the salt bath main body is NaNO 3 Added LiNO 3 The concentration was 200ppm without fluxing agent. The salt bath temperature is 450 ℃ and the treatment time is 8 hours.
The bending strength of the obtained nano microcrystalline glass 720MPa, and the surface of the glass is atomized after 14 days of double 85 treatment, so that the light transmittance is reduced to 84%, and the use requirement is not met.
Comparative example 3
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the salt bath main body is NaNO 3 Added LiNO 3 The concentration was 0ppm, and the flux added was magnesium oxide, aluminum oxide, and the concentration was 500ppm. The salt bath temperature is 450 ℃ and the treatment time is 8 hours.
The bending strength of the obtained nano microcrystalline glass is 810MPa, the surface of the glass is atomized after 14 days of double 85 treatment, the light transmittance is reduced to 66%, and the use requirement is not met.
Comparative example 4
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the salt bath main body is NaNO 3 Added LiNO 3 The concentration was 0ppm without flux. The salt bath temperature is 400 ℃ and the treatment time is 8 hours.
The obtained nano microcrystalline glass has the bending strength of 480MPa, has good surface state of glass treated by double-85 treatment for 14 days, has the light transmittance of 89 percent and does not meet the use requirement.
Comparative example 5
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the salt bath main body is NaNO 3 Added LiNO 3 The concentration was 0ppm without flux. The salt bath temperature is 450 ℃ and the treatment time is 4 hours.
The obtained nano microcrystalline glass has 650MPa of bending strength, good surface state of glass treated by double-85 treatment for 14 days, 86% of light transmittance and no use requirement.
Comparative example 6
Immersing the processed glass sheet into salt bath for chemical strengthening, wherein the salt bath main body is NaNO 3 Added LiNO 3 The concentration was 500ppm, and the flux added was magnesium oxide, aluminum oxide, and 1100ppm. The salt bath temperature is 450 ℃ and the treatment time is 8 hours.
The glass transmittance of the obtained nano microcrystalline glass after being subjected to double-85 treatment for 14 days is 81% under the bending strength of 660MPa, and the use requirement is not met.
As can be seen from comparative example 1, no LiNO was added 3 When the glass ceramic is used as a fluxing agent, the strength of the glass ceramic can be improved through chemical strengthening treatment, but the weather resistance requirement on the aspect of light transmittance cannot be met; as seen in comparative example 2, liNO was added alone 3 Has certain benefit on the light transmittance performance, but has a tendency to have a large decrease in intensity even at low concentrations; from comparative example 3, the addition of the flux alone does not improve weather resistance; comparative examples 4 and 5 illustrate that only the adjustment of the chemical strengthening temperature or time does not give a compromise between strength and light transmittance; comparative example 6 shows that an excessive amount of flux adversely affects the strength and weather resistance of the glass-ceramic.
The above is an embodiment exemplified in this example, but this example is not limited to the above-described alternative embodiments, and a person skilled in the art may obtain various other embodiments by any combination of the above-described embodiments, and any person may obtain various other embodiments in the light of this example. The above detailed description should not be construed as limiting the scope of the present embodiments, which is defined in the claims and the description may be used to interpret the claims.
Claims (8)
1. A chemical strengthening method for improving weather resistance of nano microcrystalline glass is characterized by comprising the following steps: the glass is fully immersed in a salt bath for chemical strengthening and only one-step strengthening is carried out, wherein the salt bath is NaNO with the purity of more than industrial grade 3 Compounding flux with Li NO with purity over industrial grade 3 The concentration of the lithium ions in the salt bath is 200-1000ppm, the concentration of the fluxing agent is not more than 1000ppm, and the fluxing agent is one or more of calcium oxide, magnesium oxide, fluorite and aluminum oxide.
2. The chemical strengthening method for improving weatherability of nano glass ceramics according to claim 1, wherein the salt bath lithium ion concentration is 300-700ppm.
3. The chemical strengthening method for improving the weatherability of nano glass ceramics according to claim 1, wherein the salt bath temperature is 350-550 ℃.
4. The chemical strengthening method for improving the weather resistance of nano glass ceramics according to claim 3, wherein the salt bath temperature is 380-450 ℃.
5. The chemical strengthening method for improving the weather resistance of nano glass ceramics according to claim 1, wherein the salt bath operation time is 1-24h.
6. The chemical strengthening method for improving the weather resistance of nano glass ceramics according to claim 5, wherein the salt bath operation time is 3-10h.
7. The method for improving the weather resistance of nano glass ceramics according to any one of claims 1 to 6, wherein the method is used for improving the weather resistance of nano glass ceramics after chemical strengthening.
8. A nano microcrystalline glass is characterized in that the nano microcrystalline glass is obtained by using the chemical strengthening method for improving the weather resistance of the nano microcrystalline glass according to any one of claims 1-6, the weather resistance is represented by using the light transmittance of the glass, the weather resistance of the nano microcrystalline glass is more than 89%, and the bending strength is more than 700 MPa.
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