CN110950547A - Method for enhancing GG3 glass surface stress layer - Google Patents
Method for enhancing GG3 glass surface stress layer Download PDFInfo
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- CN110950547A CN110950547A CN201911354857.2A CN201911354857A CN110950547A CN 110950547 A CN110950547 A CN 110950547A CN 201911354857 A CN201911354857 A CN 201911354857A CN 110950547 A CN110950547 A CN 110950547A
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- 239000011521 glass Substances 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 6
- 238000005728 strengthening Methods 0.000 claims abstract description 197
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 84
- 238000005498 polishing Methods 0.000 claims abstract description 63
- 150000003839 salts Chemical class 0.000 claims abstract description 48
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 42
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 42
- 230000006378 damage Effects 0.000 claims abstract description 6
- 229910001415 sodium ion Inorganic materials 0.000 claims description 35
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 13
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 13
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 12
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 7
- 150000007529 inorganic bases Chemical class 0.000 claims description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000000694 effects Effects 0.000 abstract description 14
- 238000002407 reforming Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 6
- 229910001414 potassium ion Inorganic materials 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 238000003426 chemical strengthening reaction Methods 0.000 description 4
- 230000006835 compression Effects 0.000 description 4
- 238000007906 compression Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- -1 salt potassium nitrate Chemical class 0.000 description 3
- 235000004237 Crocus Nutrition 0.000 description 2
- 241000596148 Crocus Species 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000005345 chemically strengthened glass Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000010129 solution processing Methods 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000006058 strengthened glass Substances 0.000 description 1
- 239000005341 toughened glass Substances 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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/005—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents using brushes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B29/00—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents
- B24B29/02—Machines or devices for polishing surfaces on work by means of tools made of soft or flexible material with or without the application of solid or liquid polishing agents designed for particular workpieces
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to a method for enhancing a GG3 glass surface stress layer, and belongs to the technical field of glass surface treatment. In order to solve the problem that the performance of a surface stress layer cannot be improved by the existing GG3 glass, the method for strengthening the surface stress layer of the GG3 glass is provided, and the method comprises the steps of putting the GG3 glass to be strengthened into potassium nitrate molten salt, controlling the temperature to be between 410 and 420 ℃, and carrying out strengthening treatment to form the stress layer on the surface of the GG 3526 glass to obtain the GG3 glass after primary strengthening; polishing the surface of the primary strengthened GG3 glass to damage the stress layer on the surface; and then putting the polished toughened GG3 glass into potassium nitrate molten salt, and performing secondary strengthening treatment under the condition of controlling the temperature to be 380-400 ℃ to obtain corresponding secondarily strengthened GG3 glass. The invention can realize the double effects of reforming better surface compressive stress layer depth DOL and compressive stress CS value.
Description
Technical Field
The invention relates to a method for enhancing a GG3 glass surface stress layer, and belongs to the technical field of glass surface treatment.
Background
With the gradual development and popularization of electronic products, consumers have higher and higher requirements on the quality of the electronic products, and higher requirements and appearance characteristics of display panels, covers and the like. The glass panel or the watch cover is fragile, and the glass panel or the watch cover is not enough in hardness and poor in impact resistance when collided and heavily pressed. Therefore, at present, for products using glass materials, there is a display screen using corning GG3 glass as a display panel or a cover, and the like, as the selection of the glass material. Although the glass has a high theoretical strength, the strength is greatly reduced by damage, and the mechanical strength of the chemically strengthened glass can be prevented from being lost as compared with the non-strengthened glass. Therefore, the rigidity of the display panel such as a watch cover is improved by strengthening, so that the display panel can better meet the market demand.
The glass is strengthened mainly by adopting a chemical strengthening mode, wherein the chemical strengthening is to perform high-temperature chemical strengthening treatment in metal salt to obtain toughened glass. As one of the evaluation methods of chemically strengthened glass, a higher CS value and DOL value are given to glass after strengthening, but there are problems that the concentration of a compressive stress layer cannot be increased or microcracks cannot be generated after chemical strengthening treatment, and strengthening of GG3 glass has been conventionally promoted mainly by primary strengthening, and although certain strengthening performance can be achieved, it is difficult to achieve a requirement for re-promotion, and some of them cannot achieve a breakthrough in a real sense because secondary strengthening is directly performed only to the upper limit of primary strengthening in order to improve the strengthening ability. In addition, many of the conventional methods change the strengthening ability by changing the components of the strengthening solution, and strengthening is generally performed by using a mixed strengthening solution, and some methods alleviate the influence of sodium ions and the like introduced by exchange in the glass by adding silica to a molten potassium nitrate salt in advance, and the purpose of strengthening is achieved by mixing and exchanging sodium and potassium by directly using mixed melting and the like, but the strengthening solution using sodium and potassium mixed exchange cannot be applied to the strengthening treatment of the GG3 glass.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for enhancing a GG3 glass surface stress layer, and solves the problem of how to improve the compressive stress performance of the GG3 glass surface.
The invention aims to realize the technical scheme that the method for strengthening the GG3 glass surface stress layer comprises the following steps:
A. putting GG3 glass to be strengthened into potassium nitrate molten salt, and strengthening under the condition of controlling the temperature to be between 410 and 420 ℃ to form a stress layer on the surface to obtain primary strengthened GG3 glass;
B. polishing the surface of the primary strengthened GG3 glass to damage the stress layer on the surface;
C. and then putting the polished toughened GG3 glass into potassium nitrate molten salt, and performing secondary strengthening treatment under the condition of controlling the temperature to be 380-400 ℃ to obtain corresponding secondarily strengthened GG3 glass.
According to the invention, polishing treatment is carried out on the surface of the GG3 glass after primary strengthening, and the stress layer formed by primary strengthening is destroyed again in the polishing and grinding process correspondingly to destroy the stress layer on the surface of the glass, so that the depth DOL and the value CS of the compressive stress layer on the surface are both reduced to a certain extent after destruction, the balance state of the stress layer is destroyed, and extremely fine microcracks generated in the exchange process of potassium and sodium ions can be also caused, thereby improving the performance of the surface stress layer when subsequent strengthening is facilitated; meanwhile, after polishing the stress failure layer, putting the stress failure layer into pure potassium nitrate molten salt for secondary strengthening, wherein the temperature of the secondary strengthening is lower than that of the primary strengthening, so that K ions (K) in the system are generated+) And Na ion (Na)+) The exchange release is carried out slowly, so that the stress layer adsorbed on the surface can be higher in the exchange process, the dual effects of improving the depth DOL and the value of the compressive stress CS of the surface compressive stress layer are achieved, the thickness of a new stress layer can be formed again, and the depth DOL value of the stress layer can still reach 46-50 mu m and has a higher value of the CS. Of course, it is preferable to control the temperature at the time of the secondary strengthening treatment to 395 ℃ or less. Compared with primary strengthening or direct secondary strengthening, the invention can effectively break through the strengthening bottleneck of GG3 glass and achieve higher performance of GG3 glass.
In the method for strengthening the GG3 glass surface stress layer, the DOL value of GG3 glass is preferably reduced by 0.5-2.0 μm during the polishing treatment in the step B. During polishing treatment, the stress layer of the surface is damaged through polishing and grinding, a part of the surface is ground, the DOL value of the compressive stress layer is reduced in a small range, the relatively balanced and stable state of the surface after primary strengthening is damaged mainly after the DOL value is reduced through the damage of the surface stress layer, the activity of the surface is promoted again, and after a small part is reduced, the advantage of overlapping a new stress layer on the surface is facilitated, the DOL value requirement of the corresponding stress layer depth is also facilitated to be formed again, the requirement of the CS value is promoted to be higher, and therefore the strengthening performance of the GG3 glass is improved. Further preferably, the DOL value of the GG3 glass is decreased by 1.0 to 1.5 μm during the polishing treatment in the step B.
In the method for strengthening the GG3 glass surface stress layer, the CS value of the surface compressive stress is preferably reduced by 30-50 MPa during the polishing treatment in the step B. During polishing treatment, the small reduction of the CS value of the surface compressive stress is controlled, and similarly, the relatively balanced and stable state of the surface after primary strengthening can be destroyed, so that the activity of the surface is improved again, and after a small part of the surface is reduced, the advantage of forming a new stress layer on the surface in an overlapping manner is facilitated, so that the strengthening performance of the GG3 glass is improved. Compared with the compressive stress CS value of primary strengthening or direct secondary strengthening, the compressive stress CS value can be improved to more than 890MPa, the bottleneck that the strengthening compressive stress CS value of the existing GG3 glass can only be between 800 and 850MPa and cannot be improved is effectively broken through, and the strengthening performance of the GG3 glass is improved.
In the method for strengthening the GG3 glass stress layer, the concentration of sodium ions in the potassium nitrate molten salt in the step C is preferably less than 5000 ppm. Because the sodium ions in the strengthening liquid can be exchanged with the sodium ions in the glass to release the sodium ions to the strengthening liquid in the strengthening process, and the excessive sodium ions exist, the sodium ions in the strengthening liquid can be exchanged with the potassium ions exchanged to the surface of the glass instead, so that the process of sodium-potassium mixed exchange release is caused, the original exchange of the sodium-potassium ions can be damaged, the requirement of thicker surface compressive stress layer depth DOL and higher compressive stress CS value can not be effectively met, and the requirements of the compressive stress layer depth DOL and the compressive stress CS value in one-time strengthening can not be broken through. Therefore, the control of sodium ions in the potassium nitrate molten salt is also important in the secondary strengthening process, namely one of the reasons why the sodium salt is not added is adopted in the invention, and when the pure potassium nitrate molten salt is adopted in the secondary strengthening, the content requirement of the sodium ions in the strengthening liquid of the secondary strengthening must be considered when the strengthening liquid is repeatedly used. Of course, when repeated use is not considered, the novel salt potassium nitrate molten salt is basically pure potassium nitrate molten salt, sodium ions in the novel salt potassium nitrate molten salt can not be considered basically, and the concentration of the sodium ions in the novel salt potassium nitrate molten salt is below 200 ppm. As a further preference, the concentration of sodium ions in the potassium nitrate solution in step C is less than 1000 ppm.
In the method for strengthening the GG3 glass surface stress layer, the time of the secondary strengthening treatment in the step C is preferably 1.0-5.0 hours. Because the secondary strengthening needs to be carried out at a relatively low temperature, and the sodium-potassium ion exchange is better carried out in a slow state by combining with the control of the passing time, the requirements of better forming a new surface compressive stress layer depth and higher compressive stress CS value performance are facilitated.
In the method for strengthening the GG3 glass stress layer, the temperature of the secondary strengthening treatment in the step C is preferably 381-390 ℃. The exchange of sodium and potassium ions under a slow posture is facilitated, the stress layer can be adsorbed and formed in a more sufficient time in the process of forming the stress layer, and the requirement of a deeper DOL value is met.
In the method for strengthening the GG3 glass surface stress layer, the concentration of sodium ions in the potassium nitrate molten salt in the step A is preferably less than 5000 ppm. In order to meet the requirement of forming a better stress layer in primary strengthening, when the strengthening liquid in the primary strengthening is considered to be reused, the concentration requirement of sodium ions in the strengthening liquid should be preferably controlled, so that the surface compressive stress layer depth formed in the primary strengthening can be maximized and the requirement of a higher compressive stress CS value can be effectively ensured. As a further preference, the concentration of sodium ions in the potassium nitrate molten salt in step C is less than 1000 ppm.
In the method for strengthening the GG3 glass stress layer, the polishing solution used in the polishing treatment in the step B preferably comprises the following components in percentage by mass:
cerium oxide: 20% -30%, wherein the particle size of the cerium oxide is 300-350 nm;
silicon carbide: 5.0% -10%, wherein the grain diameter of the silicon carbide is 300-350 nm;
inorganic base: 10% -20%;
sodium fluoride: 1.0% -5.0%; the balance being water.
Through the cerium oxide and the carborundum crocus of adopting above-mentioned small particle size mix, can effectual grinding destroy surperficial stress layer system, reduce the degree of depth in surface stress layer, and the crocus purpose that adopts small particle size also is the microcrack that forms in the sodium potassium ion exchange process for better detaching surface, realize high-efficient polishing, thereby make follow-up secondary strengthening in-process can form better stress layer again, make better assurance form the effect of compressive stress degree of depth DOL value and compressive stress CS value. The pH value of the polishing solution is preferably controlled to be 8-9, and as a further preference, the polishing treatment further comprises fine polishing treatment by adopting a brush. Adopt the polishing solution to polish the processing back and adopt the brush to carry out the fine polishing again, be equivalent to further carry out the fine polishing, can carry out the fine polishing to the edge of glass, eliminate the stress extrusion's at glass edge problem, and also can overcome the negative effect of the ion of not exchanging completely to glass performance, further promotion glass's strength properties. The fine polishing adopts hairbrush processing to compare with the polishing solution processing of the previous step, the polishing solution processing mainly comprises grinding and removing the depth of a partial surface stress layer, damaging the surface stress layer, and better forming the effect of a deeper DOL value during secondary strengthening, and the fine polishing further eliminates the influence of the edge of the glass, thereby being beneficial to improving the effect of the CS value. The brush can be made of pig hair or rubber silk.
In summary, compared with the prior art, the invention has the following advantages:
1. polishing the surface of GG3 glass after primary strengthening to destroy the stress layer on the surface of the glass, putting the glass into pure potassium nitrate molten salt for secondary strengthening after the stress layer is destroyed by polishing, and enabling the temperature of the secondary strengthening to be lower than that of the primary strengthening, so that the double effects of reforming better surface compressive stress layer depth DOL and compressive stress CS values can be realized, a new stress layer can be superposed again even after the stress layer is removed by polishing, and the DOL value of the stress layer depth can be at least kept to be within the range of 46-50 mu m; more importantly, the high-strength high-toughness high-strength high-toughness high-strength high-.
2. During polishing treatment, the stress layer on the surface is damaged through polishing and grinding, the DOL value of the depth of the compressive stress layer is reduced slightly, the relatively balanced and stable state of the surface after primary strengthening can be damaged, the activity of the surface is improved again, the advantage of forming a new stress layer by superposition on the surface is facilitated, the requirement of forming the depth of the thicker stress layer is also facilitated, and the strengthening performance of the GG3 glass is improved.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples, but the present invention is not limited to these examples.
Example 1
After a product GG3 glass surface cover to be strengthened is arranged in a corresponding jig, the glass surface cover is placed in a pre-execution furnace for preheating treatment, the preheating temperature is increased slowly from 0 ℃ to 380 ℃, the temperature is kept constant for 15 minutes, the phenomena that the GG3 glass surface cover is cracked and the like caused by overlarge temperature difference when the product GG3 glass surface cover is directly placed in a high-temperature strengthening furnace are avoided through preheating treatment, after preheating, the preheated GG3 glass surface cover is transferred into pure potassium nitrate molten salt with the temperature of 410 ℃ to 420 ℃ in the strengthening furnace for primary strengthening treatment for 8 hours, after the primary strengthening treatment is finished, the temperature is reduced to normal temperature, the GG3 glass surface cover after primary strengthening can be sampled for detection performance, the GG3 glass surface cover is placed in a polishing machine for polishing treatment of a formed stress layer, the surface stress layer and micro-cracks on the surface are damaged through polishing treatment, and during polishing treatment, the depth DOL value of the GG3 glass is reduced by, the polishing solution comprises the following components in percentage by mass:
cerium oxide: 20 percent, and the particle size of the cerium oxide is 300-350 nm; silicon carbide: 10 percent, and the grain diameter of the silicon carbide is 300-350 nm; inorganic base: 20 percent; sodium fluoride: 5.0 percent; the balance of deionized water; preferably, after the polishing treatment by using the polishing solution is finished, the edge of the glass is finely polished by using a brush, so that the stress extrusion effect of the edge is removed;
and then, preheating the polished GG3 glass surface cover again, wherein the preheating temperature is slowly increased to 370 ℃ from 0-370 ℃, keeping the temperature for 15 minutes, transferring the preheated GG3 glass surface cover into pure potassium nitrate molten salt with the temperature of about 380 ℃ in a strengthening furnace to carry out secondary strengthening treatment for 1 hour, and obtaining the corresponding GG3 glass surface cover after the secondary strengthening treatment.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 840MPa and a compressive stress depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has the compressive stress CS value of 950MPa and the depth of layer DOL value of 50 μm.
The method can form a new depth DOL value and a new compression stress CS value of the superimposed compression stress layer, and can meet the requirement of a better CS value.
Example 2
After a product GG3 glass surface cover to be strengthened is installed on a corresponding jig, the glass surface cover is placed into a pre-execution furnace for preheating treatment, the preheating temperature is slowly increased to 390 ℃ from 0-390 ℃, the temperature is kept constant for 15 minutes, the preheated GG3 glass surface cover is transferred into pure potassium nitrate molten salt with the temperature of 410 ℃ in the strengthening furnace for primary strengthening treatment for 10 hours, after the primary strengthening treatment is finished and the temperature is reduced to normal temperature, the once strengthened GG3 glass surface cover can be sampled for detection performance for comparison; putting the GG3 glass surface cover subjected to primary strengthening into a polishing machine to polish the formed stress layer, damaging the stress layer on the surface and fine micro cracks on the surface through polishing, and reducing the depth DOL value of the compressive stress of GG3 glass by 1.5 μm during polishing, wherein the polishing solution comprises the following components in percentage by mass:
cerium oxide: 30 percent, and the grain diameter of the cerium oxide is 300 nm; silicon carbide: 5.0 percent, and the grain diameter of the silicon carbide is 350 nm; inorganic base: 10 percent; sodium fluoride: 3.0 percent; the balance of deionized water; preferably, after the polishing treatment by using the polishing solution is finished, the edge of the glass is finely polished by using a pig hair brush, so that the stress extrusion effect of the edge is removed;
and then, preheating the polished GG3 glass surface cover again, wherein the preheating temperature is slowly increased to 375 ℃ from 0-375 ℃, keeping the temperature for 15 minutes, transferring the preheated GG3 glass surface cover into pure potassium nitrate molten salt with the temperature of about 385 ℃ in a strengthening furnace to carry out secondary strengthening treatment for 2.0 hours, and obtaining the corresponding GG3 glass surface cover after the secondary strengthening treatment.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 820MPa and a depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 930MPa and a compressive stress depth of layer DOL value of 48 μm.
The method can form a new depth DOL value and a new compression stress CS value of the superimposed compression stress layer, and can meet the requirement of a better CS value.
Example 3
After a product GG3 glass surface cover to be strengthened is installed on a corresponding jig, the glass surface cover is placed into a pre-execution furnace for preheating treatment, the preheating temperature is slowly increased to 400 ℃ from 0-400 ℃, the temperature is kept constant for 15 minutes, the preheated GG3 glass surface cover is transferred into pure potassium nitrate molten salt with the temperature of 420 ℃ in the strengthening furnace for primary strengthening treatment for 9 hours, after the primary strengthening treatment is finished and the temperature is reduced to normal temperature, the once strengthened GG3 glass surface cover can be sampled for detection performance for comparison; putting the GG3 glass surface cover after primary strengthening into a polishing machine to polish the formed stress layer, destroying the stress layer on the surface and fine micro cracks on the surface by polishing, and reducing the depth DOL value of the compressive stress of GG3 glass by 1.0 μm and the CS value of the compressive stress by about 42MPa during polishing, wherein the polishing solution comprises the following components in percentage by mass:
cerium oxide: 25 percent, and the particle size of the cerium oxide is 350 nm; silicon carbide: 8.0 percent and the grain diameter of the silicon carbide is 300 nm; inorganic base: 15 percent; sodium fluoride: 1.0 percent; the balance of deionized water; preferably, after the polishing treatment by using the polishing solution is finished, the edge of the glass is finely polished by using a pig hair brush, so that the stress extrusion effect of the edge is removed;
and then, preheating the polished GG3 glass surface cover again, wherein the preheating temperature is slowly increased to 380 ℃ from 0-380 ℃, keeping the temperature for 15 minutes, transferring the preheated GG3 glass surface cover into pure potassium nitrate molten salt with the temperature of about 390 ℃ in a strengthening furnace to carry out secondary strengthening treatment for 3.0 hours, and obtaining the corresponding GG3 glass surface cover after the secondary strengthening treatment is finished.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass surface cover after the primary strengthening has a compressive stress CS value of 815MPa and a compressive stress depth of layer DOL value of 47 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 920MPa and a compressive stress depth of layer DOL value of 48 μm.
Example 4
After a product GG3 glass surface cover to be strengthened is installed on a corresponding jig, the glass surface cover is placed into a pre-execution furnace for preheating treatment, the preheating temperature is from 0 ℃ to 400 ℃, the temperature is slowly increased to 400 ℃, the temperature is kept for 15 minutes, the preheated GG3 glass surface cover is transferred into pure potassium nitrate molten salt with the temperature of 415 ℃ in the strengthening furnace for primary strengthening treatment for 10 hours, after the primary strengthening treatment is finished and the temperature is reduced to normal temperature, the once strengthened GG3 glass surface cover can be sampled for detection performance for comparison; putting the GG3 glass surface cover after primary strengthening into a polishing machine to polish the formed stress layer, destroying the stress layer on the surface and fine micro cracks on the surface by polishing, and reducing the depth DOL value of the compressive stress of GG3 glass by 0.5 μm and the CS value of the compressive stress by about 30MPa during polishing, wherein the polishing solution comprises the following components in percentage by mass:
cerium oxide: 27%, and the particle size of the cerium oxide is 330 nm; silicon carbide: 9.0 percent, and the grain diameter of the silicon carbide is 330 nm; inorganic base: 12 percent; sodium fluoride: 3.0 percent; the balance of deionized water; controlling the pH value of the polishing solution to be 8.0-9.0, and preferably, after the polishing treatment by the polishing solution is finished, finely polishing the edge of the glass by using a pig hair brush to remove the stress extrusion effect of the edge;
and then, preheating the polished GG3 glass surface cover again, wherein the preheating temperature is slowly increased to 370 ℃ from 0-370 ℃, keeping the temperature for 15 minutes, transferring the preheated GG3 glass surface cover into pure potassium nitrate molten salt with the temperature of 381 ℃ in a strengthening furnace for secondary strengthening treatment for 3.0 hours, and obtaining the corresponding GG3 glass surface cover after the secondary strengthening treatment.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 812MPa and a depth of layer DOL value of 47 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 915MPa and a compressive stress depth of layer DOL value of 48 μm.
Example 5
In the embodiment, the nitrate molten salt used in the secondary strengthening is potassium nitrate molten salt which is repeatedly used for many times, and the concentration of sodium ions in the potassium nitrate molten salt is less than 1000 ppm.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 820MPa and a depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 923MPa and a compressive stress depth of layer DOL value of 47 μm.
It is shown that the presence of sodium ions in the secondary strengthening liquid has a certain influence on the performance after strengthening.
Example 6
In this example, the nitrate molten salt used for the secondary strengthening was potassium nitrate molten salt used repeatedly, and the concentration of sodium ions in the potassium nitrate molten salt was 4800 ppm.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 821MPa and a depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 905MPa and a compressive stress depth of layer DOL value of 47 μm.
It is shown that the increase of sodium ions in the secondary strengthening liquid has a certain influence on the performance of the CS value after strengthening.
Example 7
In the present example, both the nitrate molten salt used for the primary strengthening and the nitrate molten salt used for the secondary strengthening were potassium nitrate molten salts that were repeatedly used, and the concentration of sodium ions in the potassium nitrate molten salt used for the primary strengthening was 1000ppm or less, and the concentration of sodium ions in the potassium nitrate molten salt used for the secondary strengthening was 1000ppm or less.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass surface cover after the primary strengthening has a compressive stress CS value of 810MPa and a compressive stress depth of layer DOL value of 44 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 917MPa and a compressive stress depth of layer DOL value of 47 μm.
It is shown that the increase of sodium ions in the primary and secondary strengthening liquids has a certain influence on the performance of the CS value after strengthening.
Example 8
In the present example, both the nitrate molten salt used for the primary strengthening and the nitrate molten salt used for the secondary strengthening were potassium nitrate molten salts that were repeatedly used, and the concentration of sodium ions in the potassium nitrate molten salt used for the primary strengthening was 5000ppm or less, and the concentration of sodium ions in the potassium nitrate molten salt used for the secondary strengthening was 5000ppm or less.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 800MPa and a compressive stress depth of layer DOL value of 43 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 900MPa and a compressive stress depth of layer DOL value of 47 μm.
It is shown that the increase of sodium ions in the primary and secondary strengthening liquids has a certain influence on the performance of the CS value after strengthening.
Comparative example 1
In order to better show the significance of the polishing treatment adopted by the invention on the performance of the stress layer, the comparative example is compared and illustrated by directly carrying out secondary strengthening treatment.
After a product GG3 glass surface cover to be strengthened is arranged in a corresponding jig, the glass surface cover is placed in a pre-execution furnace for preheating treatment, the preheating temperature is increased slowly from 0 ℃ to 380 ℃, the temperature is kept constant for 15 minutes, the phenomena that the GG3 glass surface cover is cracked and the like caused by overlarge temperature difference when the glass surface cover is directly placed in a high-temperature strengthening furnace are avoided through preheating treatment, after preheating, the preheated GG3 glass surface cover is transferred into pure potassium nitrate molten salt with the temperature of 410 ℃ to 420 ℃ in the strengthening furnace for carrying out primary strengthening treatment for 8 hours, after the primary strengthening treatment is finished, the temperature is reduced to normal temperature, the GG3 glass surface cover after primary strengthening can be sampled for carrying out detection performance, then the GG3 glass surface cover after primary strengthening is preheated again, the preheating temperature is increased slowly from 0 ℃ to 370 ℃, the temperature is kept constant for 15 minutes, then the preheated GG3 glass surface cover is transferred into the pure potassium nitrate molten salt with the temperature of about 380 ℃ in the strengthening furnace for carrying out secondary strengthening, and after the secondary strengthening treatment is finished, obtaining the corresponding GG3 glass surface cover after secondary strengthening.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 840MPa and a compressive stress depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 840MPa and a compressive stress depth of layer DOL value of 48 μm.
The method shows that the upper limit of the CS value of the compressive stress of the surface cannot be improved and cannot be broken through when the secondary strengthening is directly carried out.
Comparative example 2
This comparative example is to illustrate the effect of sodium ion concentration on the performance of the surface stress layer when a molten potassium nitrate salt that is repeatedly used for secondary strengthening is used. In this comparative example, the concentration of sodium ions exceeding 5000ppm was used, specifically, the concentration of sodium ions in the molten potassium nitrate salt used for the secondary strengthening was 6000 ppm.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 820MPa and a depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 792MPa and a compressive stress depth of layer DOL value of 44 μm.
The method shows that the requirement for improving the performance of the surface stress layer cannot be met if the concentration of sodium ions in the repeatedly used potassium nitrate molten salt is too high in the secondary strengthening, and the requirement for the performance of the surface stress layer of the glass after the primary strengthening is not met.
Comparative example 3
In this comparative example, the temperature of the second strengthening needs to be lower than that of the first strengthening, and the second strengthening is performed under the same temperature conditions as those of the first strengthening in comparative example 1. I.e. both the primary and secondary strengthening temperatures are 410 ℃.
The other processing procedures are the same as those in embodiment 2, and are not repeated here, and finally the corresponding secondarily-strengthened GG3 glass cover is obtained.
The performance of the obtained intermediate GG3 glass watch cover after primary strengthening and the performance of the obtained final GG3 glass watch cover after secondary strengthening are tested, and the results show that:
the GG3 glass watch cover after the primary strengthening has a compressive stress CS value of 820MPa and a depth of layer DOL value of 46 μm.
The final GG3 glass surface cover after secondary strengthening has a compressive stress CS value of 852MPa and a compressive stress depth of layer DOL value of 47 μm.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (9)
1. A method of enhancing a GG3 glass surface stress layer, the method comprising the steps of:
A. putting GG3 glass to be strengthened into potassium nitrate molten salt, and strengthening under the condition of controlling the temperature to be between 410 and 420 ℃ to form a stress layer on the surface to obtain primary strengthened GG3 glass;
B. polishing the primary strengthened GG3 glass to damage a surface stress layer;
C. and then putting the polished toughened GG3 glass into potassium nitrate molten salt, and performing secondary strengthening treatment under the condition of controlling the temperature to be 380-400 ℃ to obtain corresponding secondarily strengthened GG3 glass.
2. The method for strengthening the GG3 glass stress layer according to claim 1, wherein the depth of compressive stress DOL of the GG3 glass is reduced by 0.5-2.0 μm during the polishing treatment in step B.
3. The method for strengthening GG3 glass stress layer according to claim 1, wherein the CS value of the surface compressive stress is reduced by 30-50 MPa when polishing in step B.
4. The method for strengthening the GG3 glass stress layer according to claim 1, wherein the concentration of sodium ions in the potassium nitrate molten salt in the step C is less than 5000 ppm.
5. The method for strengthening the GG3 glass stress layer according to claim 4, wherein the concentration of sodium ions in the potassium nitrate molten salt in the step C is less than 1000 ppm.
6. The method for strengthening the GG3 glass stress layer according to any one of claims 1-5, wherein the time of the secondary strengthening treatment in step C is 1.0-5.0 hours.
7. The method for strengthening the GG3 glass stress layer according to claim 6, wherein the secondary strengthening treatment in step C is performed at a temperature of 381-390 ℃.
8. The method for strengthening the GG3 glass stress layer according to any one of claims 1-5, wherein the concentration of sodium ions in the potassium nitrate molten salt in the step A is less than 5000 ppm.
9. The method for strengthening the GG3 glass stress layer according to any one of claims 1-5, wherein the polishing solution used in the polishing treatment in the step B comprises the following components by mass percent:
cerium oxide: 20% -30%, wherein the particle size of the cerium oxide is 300-350 nm;
silicon carbide: 5.0% -10%, wherein the grain diameter of the silicon carbide is 300-350 nm;
inorganic base: 10% -20%;
sodium fluoride: 1.0% -5.0%; the balance being water.
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