CN117466547A - Method for reducing tin penetration of float cover plate glass for electronic information display - Google Patents
Method for reducing tin penetration of float cover plate glass for electronic information display Download PDFInfo
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- CN117466547A CN117466547A CN202311350621.8A CN202311350621A CN117466547A CN 117466547 A CN117466547 A CN 117466547A CN 202311350621 A CN202311350621 A CN 202311350621A CN 117466547 A CN117466547 A CN 117466547A
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- glass
- ion exchange
- tin
- information display
- electronic information
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 230000035515 penetration Effects 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000005357 flat glass Substances 0.000 title abstract description 11
- 239000011521 glass Substances 0.000 claims abstract description 90
- 238000005342 ion exchange Methods 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 229910001432 tin ion Inorganic materials 0.000 claims abstract description 16
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Inorganic materials [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims abstract description 9
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- -1 alkaline earth metal calcium nitrate Chemical class 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 11
- 239000011575 calcium Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 8
- 150000002500 ions Chemical group 0.000 claims description 7
- 239000006059 cover glass Substances 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 4
- 229910001415 sodium ion Inorganic materials 0.000 claims description 4
- 239000005329 float glass Substances 0.000 abstract description 11
- 229910001413 alkali metal ion Inorganic materials 0.000 abstract description 5
- 238000005452 bending Methods 0.000 abstract description 3
- 230000002411 adverse Effects 0.000 abstract description 2
- 239000005341 toughened glass Substances 0.000 abstract description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 11
- 238000005530 etching Methods 0.000 description 10
- 239000007788 liquid Substances 0.000 description 9
- 230000007547 defect Effects 0.000 description 8
- 229910021645 metal ion Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005496 tempering Methods 0.000 description 5
- 238000006124 Pilkington process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 238000004876 x-ray fluorescence Methods 0.000 description 2
- 238000012952 Resampling Methods 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical group [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- 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
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 invention relates to a method for reducing tin penetration of float cover plate glass for electronic information display, which comprises the steps of firstly immersing a float glass raw sheet into a salt solution containing alkaline earth metal calcium nitrate, wherein the temperature of the salt solution is about 560-565 ℃, and the ion exchange time is about 30-60 min, so that alkaline earth metal ions and tin ions are subjected to full ion exchange reaction; and cooling the glass to room temperature, then carrying out a second ion exchange reaction, putting the glass into a salt solution containing another alkali metal sodium nitrate, wherein the temperature of the salt solution is about 400-450 ℃, and the ion exchange time is about 30-60 min, so that alkali metal ions and tin ions carry out a full ion exchange reaction. The invention greatly reduces the tin penetration of the float cover plate glass, reduces the warp of the toughened glass, improves the Vickers hardness of the glass, effectively reduces the adverse changes of the surface components and the performances of the glass, and reduces the iridescence and the bending phenomenon of the cover plate glass after the toughening.
Description
Technical Field
The invention relates to the field of float glass production and manufacturing, in particular to a method for reducing tin penetration of float cover plate glass for electronic information display.
Background
The float glass production process is that molten and clarified glass liquid flows into a tin bath through a flow channel, the molten glass liquid is flattened on the tin liquid surface, polished, thinned and formed, and the molten glass is subsequently subjected to production processes such as annealing, cutting and the like. The glass formed by the float process has higher flatness and good polishing effect, and the float process has great advantages for producing glass with larger size and different thickness. Along with the wide application of glass in the electronic information display industry, the requirements on the quality of the glass are higher and higher, and defects of cover plate glass used in the electronic information display industry mainly comprise bubbles, stones, stripes, knots, tin defects and the like, and the tin defects are the main problems of unqualified glass quality in the quality detection of float glass. Tin defects are unavoidable in float glass and can only be reduced by controlling the oxidation of the tin liquid.
The appearance defects of float glass caused by tin are generally called tin defects, including tin dust, tin dipping, tin penetration and the like, wherein the tin penetration can change the chemical composition and structure of the tin surface layer of the glass, thereby changing the physical and chemical properties of the float glass. At high temperature, the molten tin reacts with trace oxygen and the like remaining in the atmosphere to be oxidized into Sn 2+ And Sn (Sn) 4+ By Sn 2+ Mainly, a small amount of Sn 4+ And the ions are subjected to ion exchange reaction with alkali metal ions and alkaline earth metal ions in the glass, and the tin ions in the tin liquid enter the lower surface of the glass liquid to cause the change of glass tempering rainbow and tempering effect. The toughened iridescence is that when float glass is thermally processed (such as physical toughening or thermal bending) in a toughening furnace, the SnO on the surface of the float glass is oxidized into SnO 2 The volume of the glass is increased to cause the surface micro-stripes formed by the expansion of the glass surface, the interference phenomenon of light is generated under the irradiation of light, the lower surface of the glass is colored when reflected, and the micro-stripes on the glass surface can be observed under a microscope. Research shows that the tin penetration amount, tin penetration depth and tin penetration ion distribution directly influence the occurrence and severity of float glass tempering iridescence. Furthermore, it is disadvantageous for glassThe mechanical strength, dielectric property and optical property greatly influence the qualification rate of glass products and the deep processing quality of glass, and limit the application range of the glass, which is a main reason that glass products in China are difficult to be used for deep processing in a large amount.
In the early stage of research on tin penetration defects, in the ion exchange phenomenon of the interface between tin liquid and glass liquid, tin ions possibly undergo exchange reaction with calcium ions, potassium ions and sodium ions, but mainly undergo exchange reaction of sodium ions.
Disclosure of Invention
The invention aims to greatly reduce the problem of tin-leaching defect of the cover plate glass of the electronic information display glass produced by the existing float process, and provides a method for reducing tin-leaching of the cover plate glass for electronic information display.
The technical scheme adopted by the invention is as follows:
a method for reducing tin penetration of float cover glass for electronic information display, comprising the steps of:
1) The first ion exchange reaction of the electronic information display glass is alkaline earth metal ion Ca 2+ Exchange with tin ions, the exchange reaction steps are as follows:
firstly, cleaning an electronic information display glass raw sheet, placing the glass raw sheet into a furnace body, preheating the glass raw sheet to 390-420 ℃, then immersing the glass raw sheet into a pure calcium nitrate salt solution, wherein the temperature of the salt solution is about 560-565 ℃, and the ion exchange time is about 30-60 min, so that calcium nitrate ions and tin ions are fully ion-exchanged;
2) The second ion exchange reaction of the electronic information display glass is alkali metal Na + The ion exchange and tin ion exchange reaction steps are as follows:
thoroughly cleaning and drying electronic information display glass after the first exchange reaction, cooling to room temperature, carrying out a second ion exchange reaction, preheating the glass to 300-320 ℃, then placing the glass into a solution containing pure sodium nitrate salt, wherein the temperature of the salt solution is about 400-450 ℃, and the ion exchange time is about 30-60 min, so that sodium nitrate and tin ions carry out full ion exchange reaction;
3) Cleaning to remove residual molten salt on the surface of the electronic information display glass, and drying.
In the technical proposal of the invention, the network exo-body oxide (such as Na 2 O、CaO、K 2 O, etc.) to participate in the network structure, and metal ions are dissociated in the network structure. Other ions having the same valence or chemical properties may be substituted for the metal and alkali metal ions in some glass networks under certain conditions. In the formed exchange area, certain properties of the glass may change. The ion exchange is to immerse oxide glass in molten salt, and ion exchange reaction occurs at high temperature, heat disturbance exists in the glass, ions pass through a glass substrate to cause potential difference of ion flow, so that alkali metal or alkaline earth metal ions in the molten salt are exchanged with network external ions at the surface of the glass, and finally the required glass is obtained. The invention achieves the effect of exchanging tin ions in the tin surface of the glass by using alkali metal ions and alkaline earth metal ions through ion exchange reaction.
In the technical scheme of the invention, the glass body contains the following alkali metal and alkaline earth metal oxides: caO, mgO and Na 2 O is not suitable as the first choice for ion exchange because MgO is used as a glass intermediate and the melting temperature of the salt solution is relatively high. Further preliminary experiments show Ca 2+ And Na (Na) + Can be subjected to ion exchange reaction with tin ions, but Na is used for preparing + Mainly. Ca (Ca) 2+ With Sn 2+ The valence states are the same, and ion exchange reaction can be performed. On the other hand Ca 2+ Radius of 0.1nm, na + Radius of 0.102nm, sn 2+ Radius of 0.112nm, sn 4+ Radius of 0.069nm, when Ca 2+ And Na (Na) + Exchange Sn 2+ The radius is similar, but Ca 2+ And Na (Na) + Exchange Sn 4+ And then, carrying out ion exchange on the large-radius metal ions in the salt bath and the small-radius metal ions in the glass surface, and utilizing the volume difference of the large-radius metal ions and the small-radius metal ions to enable the glass surface to be in a compressive stress state, so that the Vickers hardness of the glass can be effectively improved. The method reduces the tin penetration of the glass on one hand and improves the Vickers hardness of the glass on the other hand, thus the inventionEnd use Ca 2+ 、Na + The ion exchange reaction is carried out with tin ions, so that the mixed alkali effect is avoided, and the melting temperature difference of two salt solutions is large, so that the ion exchange reaction is carried out in two steps.
The invention has the beneficial effects that:
the method of the invention greatly reduces the tin penetration of float glass, reduces the warp of glass after tempering, greatly improves the Vickers hardness of the glass, effectively reduces the adverse changes of the surface components and the performance of the glass, and reduces the iridescence and the bending phenomenon of the glass after tempering.
Description of the embodiments
The invention relates to a method for reducing tin penetration of float cover plate glass for electronic information display, which comprises the following steps of firstly using calcium ion exchange, and secondly using sodium ion exchange:
(1) Firstly, preparing cover plate glass of 4 float production lines, cutting the glass into pieces with the size of 3.5cm or less and 3.5cm, putting the pieces into an ultrasonic instrument for cleaning, then flushing the pieces with deionized water, and putting the pieces into an oven for drying for later use;
(2) Respectively carrying out X-ray fluorescence spectrum test on 4 pieces of glass to obtain tin content of about 0.44wt%, wherein specific values are shown in the following table, namely example 1-example 4, and after the test is completed, respectively placing the 4 pieces of glass in a muffle furnace for preheating at 400 ℃;
(3) Heating calcium nitrate to 565 ℃, then placing the glass in a calcium nitrate solution for ion exchange for 30min, taking out the glass for cooling after the exchange is completed, performing ultrasonic cleaning to remove residual molten salt on the surface, and drying;
(4) And (3) heating the dried glass to 300 ℃ again for preheating, putting the preheated glass into a sodium nitrate solution at 420 ℃ for secondary ion exchange for 1h, taking out the glass after the exchange is completed, cooling, cleaning to remove residual molten salt on the surface of the electronic information display glass, and drying.
In order to judge the exchange condition of tin ions in the glass after the ion exchange reaction, the glass is thinned. Firstly, preparing an acid etching solution, measuring the original thickness of the electronic display glass, placing the electronic display glass in the etching solution for a certain time, taking out the thickness of the etched glass, and calculating the etching speed of the electronic display glass. According to the etching speed of the glass, resampling, soaking the glass in etching liquid for different time to achieve the purpose of etching different thicknesses, and accurately etching the glass by the experiment with etching errors of 1 mu m, 3 mu m and 5 mu m, wherein the etching errors are < +/-0.2 mu m. After etching, the tin content was measured using X-ray fluorescence spectroscopy, respectively.
(6) In order to investigate whether the temperature of the ion exchange reaction has an influence on the exchange effect, the ion exchange temperature of the first step is relatively high, and the temperature is not suitable to be increased again, and only the ion exchange temperature of the second step is changed. Firstly, 9 pieces of cover glass are prepared, and X-ray fluorescence spectrum is carried out to test tin content, namely about 0.43wt%; and (2) repeating the steps (1), (2) and (3), then carrying out a second ion exchange reaction, wherein the second reaction temperature is 400 ℃, 440 ℃ and 450 ℃ respectively, carrying out an exchange reaction for 1h, taking out glass after the exchange is finished, cooling, carrying out ultrasonic cleaning to remove residual molten salt on the surface, and then drying to measure the tin content on the surface of the glass.
Comparative example 1 is a float produced cover glass raw sheet for electronic information display, and was not subjected to ion exchange treatment. Examples 1 to 4 are cover glasses subjected to two-step ion exchange treatment. Examples 5 to 13 are the surface tin penetration amounts of the glasses after ion exchange at 400 ℃, 440 ℃ and 450 ℃ respectively. Table 1 shows the tin content of the glass and the glass performance index. Table 2 shows the tin penetration of the glass surface before and after the exchange by changing the experimental temperature of the ion exchange in the second step.
Table 1 examples and properties are as follows:
TABLE 2 tin penetration of glass surfaces
The present invention provides a method for reducing tin penetration of float electronic information display glass, and compared with comparative example 1, the tin penetration of the glass surface of examples 1, 2, 3 and 4 is greatly reduced, the warp degree of the tempered glass is greatly reduced, the vickers hardness of the glass is greatly improved, and the influence of ion exchange temperature on the glass is studied, wherein the greater the ion exchange amount is, the progressively reduced tin penetration is as shown in examples 5 to 13 with the increase of temperature.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention in any way; any person skilled in the art can make many possible variations and modifications to the technical solution of the present invention or modifications to equivalent embodiments using the methods and technical contents disclosed above, without departing from the scope of the technical solution of the present invention. Therefore, any simple modification, equivalent substitution, equivalent variation and modification of the above embodiments according to the technical substance of the present invention, which do not depart from the technical solution of the present invention, still fall within the scope of the technical solution of the present invention.
Claims (1)
1. A method for reducing tin penetration of float cover glass for electronic information display, comprising the steps of:
1) The first ion exchange reaction is alkaline earth metal ion Ca 2+ Exchange with tin ions:
cleaning an electronic information display glass raw sheet, placing the glass raw sheet into a furnace body, preheating the glass raw sheet to 390-420 ℃, immersing the glass raw sheet into a pure calcium nitrate salt solution, wherein the temperature of the salt solution is 560-565 ℃, and the ion exchange time is about 30-60 min, so that calcium nitrate ions and tin ions in the glass are fully ion exchanged;
2) The second ion exchange reaction is alkali metal Na + Ion exchange step with tin ion:
thoroughly cleaning and drying electronic information display glass after the first exchange reaction, cooling to room temperature, preheating the glass to 300-320 ℃, then placing the glass into a solution containing pure sodium nitrate salt, wherein the temperature of the solution is 400-450 ℃, and the ion exchange time is about 30-60 min, so that sodium nitrate and tin ions perform full ion exchange reaction;
3) Cleaning to remove residual molten salt on the surface of the electronic information display glass, and drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311350621.8A CN117466547A (en) | 2023-10-18 | 2023-10-18 | Method for reducing tin penetration of float cover plate glass for electronic information display |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311350621.8A CN117466547A (en) | 2023-10-18 | 2023-10-18 | Method for reducing tin penetration of float cover plate glass for electronic information display |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117466547A true CN117466547A (en) | 2024-01-30 |
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ID=89624773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311350621.8A Pending CN117466547A (en) | 2023-10-18 | 2023-10-18 | Method for reducing tin penetration of float cover plate glass for electronic information display |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117466547A (en) |
-
2023
- 2023-10-18 CN CN202311350621.8A patent/CN117466547A/en active Pending
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