CN115448594A - Glass and preparation method and application thereof - Google Patents
Glass and preparation method and application thereof Download PDFInfo
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- CN115448594A CN115448594A CN202211131877.5A CN202211131877A CN115448594A CN 115448594 A CN115448594 A CN 115448594A CN 202211131877 A CN202211131877 A CN 202211131877A CN 115448594 A CN115448594 A CN 115448594A
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- 239000011521 glass Substances 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000005728 strengthening Methods 0.000 claims abstract description 46
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 25
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims description 38
- 238000003426 chemical strengthening reaction Methods 0.000 claims description 32
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 24
- 239000006121 base glass Substances 0.000 claims description 18
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 150000003839 salts Chemical class 0.000 claims description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 12
- 235000010344 sodium nitrate Nutrition 0.000 claims description 12
- 239000004317 sodium nitrate Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 235000010333 potassium nitrate Nutrition 0.000 claims description 9
- 239000004323 potassium nitrate Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 16
- 238000005342 ion exchange Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 6
- 229910001415 sodium ion Inorganic materials 0.000 description 6
- 239000005341 toughened glass Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 229910001414 potassium ion Inorganic materials 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000006058 strengthened glass Substances 0.000 description 2
- 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 1
- 239000006018 Li-aluminosilicate Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006059 cover glass Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
-
- 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
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)
- Glass Compositions (AREA)
Abstract
The invention relates to the technical field of glass production, and discloses glass, a preparation method of the glass, the glass prepared by the preparation method and application of the glass. The glass of the present invention contains 50 to 62 mass% of SiO in terms of oxide 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a Maximum compressive stress CS of glass of the present invention>900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 mu m, and the strengthening depth DOL of the K layer>4.0 μm, vickers hardness>600HV. The glass of the present invention is excellent in falling resistance.
Description
Technical Field
The invention relates to the technical field of glass production, in particular to glass, a preparation method of the glass, the glass prepared by the preparation method and application of the glass.
Background
In recent years, with the continuous maturation of the 5G technology, the corresponding matched interconnection technology also comes, and the 5G provides a new technical support for various cross-border fusion. The most common products in modern intelligent terminals are novel smart phones and tablet computers, and the touch screen is particularly important in the aspect of use of the intelligent terminal. The outermost cover glass is one of the key materials for manufacturing the touch screen. Of course, glass can be used as both a functional material and a protective material. The conventional metal back cover plate interferes with the high-frequency transmission and reception of 5G signals, so that the number of antennas is increased to improve the transmission and reception of the signals. Glass materials can better solve the problems, but the fragile characteristic of the materials can prevent the glass materials from being applied to the rear cover plate on a large scale. Particularly, in the daily use process, the mobile phone inevitably falls and is damaged, and at the moment, the glass serving as the rear cover plate cannot protect the internal parts of the mobile phone.
Therefore, if the above problems are to be solved, it is required that the glass has both good permeability and better drop resistance, thereby improving the service life of the electronic product.
Disclosure of Invention
The invention aims to overcome the problem of poor anti-falling performance in the prior art, and provides glass which has the advantages of increased maximum compressive stress CS, strengthened depth DOL, vickers hardness and excellent anti-falling performance.
In order to achieve the above object, a first aspect of the present invention provides a glass containing 50% to 62% by mass of Si in terms of oxide based on the total mass of the glassO 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein a =0.5-0.7, b =2-4, c =8% -14%;
the maximum compressive stress CS of the glass is more than 900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 mu m, the strengthening depth DOL of the K layer is more than 4.0 mu m, and the Vickers hardness is more than 600HV.
Preferably, the glass contains 50-57% SiO in terms of mass percent of oxide 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
The second aspect of the present invention provides a method for producing a glass containing 50 to 62 mass% of SiO in terms of oxide, based on the total mass of the glass 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein a =0.5-0.7, b =2-4, c =8% -14%;
the preparation method comprises the following steps:
(1) Mixing raw materials for preparing glass to prepare base glass;
(2) Sequentially carrying out first chemical strengthening treatment and second chemical strengthening treatment on the base glass obtained in the step (1), wherein the first chemical strengthening process comprises the step of contacting the base glass with first strengthening liquid, and the first strengthening liquid is sodium nitrate molten salt; the second chemical strengthening process comprises the step of contacting the glass after the first chemical strengthening treatment with a second strengthening solution, wherein the second strengthening solution is a molten salt containing 20-30wt% of sodium nitrate and 70-80wt% of potassium nitrate based on the total weight of the second strengthening solution.
Preferably, the conditions of the first chemical strengthening treatment include: the temperature is 380-420 ℃, and the time is 1-3 hours; the conditions of the second chemical strengthening treatment include: the temperature is 370-380 deg.C, and the time is 0.15-3 hr.
Preferably, the second reinforcing fluid is a molten salt containing 25 to 30wt% of sodium nitrate and 70 to 75wt% of potassium nitrate, based on the total weight of the second reinforcing fluid.
Preferably, the glass contains 50-57% SiO in terms of mass percent of oxide 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
Preferably, step (1) comprises: mixing and melting raw materials for preparing the glass, and sequentially carrying out casting molding, annealing, cutting and polishing treatment to obtain the base glass.
The third aspect of the present invention provides a glass produced by the above production method.
Preferably, the maximum compressive stress CS of the glass is more than 900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 μm, the strengthening depth DOL of the K layer is more than 4.0 μm, and the Vickers hardness is more than 600HV.
The fourth aspect of the invention provides an application of the glass as a material of a front cover or a rear cover for a display screen of an intelligent terminal.
By controlling the components and content of the basic glass and the conditions of two times of chemical strengthening, the invention can produce better technical effects on the aspects of the surface compression stress value, the depth of a stress layer, the perfectness rate of the glass after falling, the anti-cracking performance and the like of a glass product. Specifically, the compressive stress value, the stress layer depth, the ball falling height and other properties of the glass obtained by the invention are obviously improved, the maximum compressive stress CS of the strengthened glass is more than 900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 mu m, the strengthening depth DOL of the K layer is more than 4.0 mu m, the Vickers hardness is more than 600HV, the falling-resistant height is up to 2m, the application of the glass on electronic products can be better met, and the service life of the electronic products can be effectively prolonged.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In a first aspect, the present invention provides a glass comprising 50 to 62% by mass of SiO in terms of oxide, based on the total mass of the glass 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein A =0.5-0.7, B =2-4, C =8% -14%.
In the present invention, the maximum compressive stress CS of the glass is >900MPa, the depth of reinforcement DOL (DOL (Na)) of the Na layer is > 130 μm, the depth of reinforcement DOL (DOL (K)) of the K layer is >4.0 μm, and the Vickers hardness is >600HV.
In the invention, a surface stress meter FSM-6000 is used for measuring the surface compressive stress; ion exchange layer depth was measured using a glass surface stress meter SLP-2000. The performance indicators involved are illustrated here: wherein CS is K + Surface compressive stress in Mpa; DOL (Na) is the depth of the CS (Na) layer in μm; DOL (K) is the depth of the CS (K) layer in μm.
According to a preferred embodiment of the invention, the glass contains 50% to 57% SiO in mass percent on the basis of the oxides 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
The second aspect of the present invention provides a method for producing a glass containing 50 to 62 mass% of SiO in terms of oxide, based on the total mass of the glass 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein a =0.5-0.7, b =2-4, c =8% -14%;
the preparation method comprises the following steps:
(1) Mixing raw materials for preparing glass to prepare base glass;
(2) Sequentially carrying out first chemical strengthening treatment and second chemical strengthening treatment on the base glass obtained in the step (1), wherein the first chemical strengthening process comprises the step of contacting the base glass with first strengthening liquid, and the first strengthening liquid is sodium nitrate molten salt; the second chemical strengthening process comprises the step of contacting the glass after the first chemical strengthening treatment with a second strengthening solution, wherein the second strengthening solution is a molten salt containing 20-30wt% of sodium nitrate and 70-80wt% of potassium nitrate based on the total weight of the second strengthening solution.
In the invention, sodium nitrate molten salt is used as a first strengthening liquid, and sodium ions (Na) + ) Can replace the lithium ions (Li) with the depth of 0-300 mu m on the surface of the lithium aluminosilicate glass + ) The original glass contains higher lithium ions, and the concentration difference of the lithium ions between the first strengthening liquid and the original glass provides stronger power for the exchange of lithium and sodium ions, thereby being beneficial to the formation of an ion exchange layer.
In the invention, the second strengthening liquid with the specific proportion range is adopted, sodium in the glass obtained by the lithium-sodium ion exchange and potassium ions in the second strengthening liquid are subjected to second ion exchange, and the lithium-sodium ion exchange and the sodium-potassium ion exchange are sequentially carried out to limit the ion amount of the ion exchange, so that the phenomenon that the glass performance is reduced or spontaneous explosion is caused due to the excessive crowding effect generated by the ion exchange is avoided.
The second strengthening liquid is mainly used for exchanging sodium ions and potassium ions in the glass to form a deeper ion exchange layer. If the potassium nitrate content in the second strengthening liquid is less than 70wt%, sodium ions in the glass cannot be effectively exchanged; if the potassium nitrate content in the second strengthening liquid is higher than 80wt%, a jamming effect is easily formed, and the strengthening performance of the glass cannot be effectively improved.
In the present invention, the method for preparing the base glass from the raw materials in step (1) may be a method commonly used in the art, but the present invention provides a preferred embodiment in order to obtain a glass having better shatter resistance.
Preferably, the "mixing raw materials for glass production to produce base glass" described in the step (1) includes: mixing and melting raw materials for preparing glass, and sequentially carrying out casting molding, annealing, cutting and polishing treatment to obtain the base glass.
The specific manner of the casting, annealing, cutting and polishing processes is not particularly limited by the present invention, and those skilled in the art can perform the processes by using the conventional technical means in the field, and the present invention is not described herein again, and those skilled in the art should not be construed as limiting the present invention.
Preferably, in the present invention, the conditions of the first chemical strengthening treatment include: the temperature is 380-420 ℃ and the time is 1-3 hours.
Preferably, in the present invention, the conditions of the second chemical strengthening treatment include: the temperature is 370-380 deg.C, and the time is 0.15-3 hr.
According to a preferred embodiment of the invention, the second strengthening fluid contains 25-30wt% of sodium nitrate and 70-75wt% of potassium nitrate, based on the total weight of the second strengthening fluid.
According to a preferred embodiment of the invention, the glass contains 50% to 57% SiO in mass percent on the basis of the oxides 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
The preparation method of the glass further comprises the conventional technical means of cleaning, wiping, preheating and the like, and the skilled person can select the preparation method according to the actual needs, and the invention provides a specific embodiment in the following by way of example, and the skilled person cannot understand the limitation of the invention.
The third aspect of the present invention provides a glass produced by the above production method.
The maximum compressive stress CS of the glass prepared by the preparation method is more than 900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 mu m, the strengthening depth DOL of the K layer is more than 4.0 mu m, and the Vickers hardness is more than 600HV.
The fourth aspect of the invention provides an application of the glass as a material of a front cover or a rear cover for a display screen of an intelligent terminal.
The present invention will be described in detail below by way of examples. In the following examples, the materials used are all commercially available and the room temperature is 25. + -. 2 ℃.
Light transmittance: the sample was processed to a thickness of 0.7mm and polished in parallel with the opposite side, and the average light transmittance at 550nm was measured using a Hitachi U-41000 spectrophotometer.
Surface stress and stress layer depth: surface stress measurement is carried out by utilizing a surface stress meter FSM-6000; ion exchange layer depth was measured using a glass surface stress meter SLP-2000.
Falling ball is a falling resistance test: the process is carried out by using 25g of steel ball from the height of 30cm, the central point falls 3 times, each time the central point rises by 5cm, and the unit of the falling ball height is centimeter (cm).
Examples and comparative examples
(1) Preparation of base glass
The components and proportions of examples 1 to 7 and comparative examples 1 to 3 are shown in Table 1.
The compositions and proportions of examples 8 to 14 and comparative examples 4 to 6 were the same as in example 7.
The components in the examples and the comparative examples are weighed according to the glass compositions shown in Table 1, mixed uniformly in a sealed bag, poured into a platinum crucible to be melted at 1650 ℃, after being melted for 3 hours, the molten glass liquid is cast in a metal mold, the glass is transferred into a muffle furnace to be annealed at 630 ℃, the temperature is kept for 2 hours, precision annealing is carried out according to the cooling rate of 2 ℃/min, the breakage caused by the fact that the internal stress of the glass is not eliminated in later cutting is avoided, and the glass is made into small samples of 145 x 73 x 0.7mm glass plates through cutting and grinding, namely the base glass.
(2) Chemical strengthening treatment
Procedure of chemical strengthening treatment of examples 1 to 7 and comparative examples 1 to 3:
preheating the base glass at 360 ℃ for 1 hour, immersing the preheated base glass into a first strengthening solution (sodium nitrate molten salt) and treating at 380 ℃ for 2 hours to obtain strengthened glass I; and after the temperature of the tempered glass I is reduced and the tempered glass I is cooled to room temperature, cleaning, wiping and secondary preheating (the temperature is 360 ℃ and the time is 1 hour) by using pure water to obtain the tempered glass I after secondary preheating, and then soaking the tempered glass I after secondary preheating into a second strengthening solution (30 wt% of sodium nitrate molten salt and 70wt% of potassium nitrate molten salt) and processing for 2 hours at 370 ℃ to obtain the tempered glass II. The performance parameters of the tempered glass II were measured, and the specific results are shown in Table 1.
The conditions of the chemical strengthening treatment of examples 8 to 14 and comparative examples 4 to 6 are shown in Table 2.
TABLE 1
As can be seen from table 1: in examples 1 to 7, when the glass components meet the ranges and the A, B, C value meets the requirements of the technical scheme of the invention, the high-strength cover plate glass is obtained through a chemical strengthening process, the visible light transmittance of the obtained glass at 550mm is 90%, the surface compressive stress CS is greater than 900MPa after chemical strengthening, the depth of a CS (Na) layer is greater than or equal to 130 μm, the depth of a CS (K) layer is greater than 4.0 μm, and the obtained glass has excellent chemical strengthening performance; the falling ball height is more than 180cm.
The above properties are significantly reduced with respect to the present invention for comparative example 1 (D1), comparative example 2 (D2) and comparative example 3 (D3) in which the glass composition and/or A, B, C value do not satisfy the requirements of the technical solution of the present invention, and particularly for comparative example 2 and comparative example 3 in which A, B, C value is different from the solution of the present invention, CS is less than 850MPa, the depth of CS (Na) layer is <130 μm, the depth of CS (K) layer is <3.5 μm, and the ball drop height is not more than 170cm.
It can be seen that the content of each component in the glass composition and the values of A, B and C both satisfy the range of the present invention, and that the glass composition has a superior technical effect on the surface compression stress value, the depth of the stress layer, the fraction of glass after falling, the fracture resistance, and the like, relative to the case where the content of the component is not within the range of the present invention and only the content of each component satisfies the range of the present invention but A, B, C does not satisfy the requirements.
TABLE 2
Table 2 is mainly used to illustrate the effects of the material formulation of given components and contents, the compressive stress values, the stress layer depths and the ball drop heights obtained by different chemical strengthening methods; examples 8 to 14 and comparative example 4 (D4), comparative example 5 (D5), and comparative example 6 (D6) were chemically strengthened twice.
As can be seen from table 2: when the strengthening conditions of the embodiment 13 are met, the surface compressive stress CS of the strengthened product is up to 950Mpa, the falling ball height is up to 200cm, and the product has very excellent chemical strengthening performance; comparative examples 5 and 6 are inferior to examples in performance, in that the molten salt ratio of the reinforcing liquid used for the second chemical strengthening is different, and comparative example 4 is the worst in performance because the second chemical strengthening time is shorter, so that the CS stress layer depth and the ball drop height of the product after the strengthening are lower. From the above results, it can be seen that the above-mentioned related properties are significantly improved by adopting the technical scheme of the strengthening process of the present invention to strengthen the product.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including various technical features being combined in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. Glass, characterized in that it contains 50-62% SiO in mass percent on the basis of the total mass of the glass, calculated as the mass percent of the oxides 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 ；
And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein a =0.5-0.7, b =2-4, c =8% -14%;
the maximum compressive stress CS of the glass is more than 900MPa, the strengthening depth DOL of the Na layer is more than or equal to 130 mu m, the strengthening depth DOL of the K layer is more than 4.0 mu m, and the Vickers hardness is more than 600HV.
2. The glass according to claim 1, wherein the glass contains 50-57% SiO in terms of mass percent of oxides 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
3. A method for producing glass, characterized in that the glass contains 50-62% SiO in terms of mass percentage of oxides based on the total mass of the glass 2 17% -35% of Al 2 O 3 1% -8% of Na 2 O, 0-2% of K 2 O, 2-11% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 (ii) a And the mass percentage of each component in the glass satisfies the value of A, B, C in the formulas (1) to (3):
formula (1) A = SiO 2 /(SiO 2 +Al 2 O 3 )，
Formula (2) B = Al 2 O 3 /(Na 2 O+K 2 O+Li 2 O)，
Formula (3) C = Na 2 O+K 2 O+Li 2 O，
Wherein a =0.5-0.7, b =2-4, c =8% -14%;
the preparation method comprises the following steps:
(1) Mixing raw materials for preparing the glass to prepare base glass;
(2) Sequentially carrying out first chemical strengthening treatment and second chemical strengthening treatment on the base glass obtained in the step (1), wherein the first chemical strengthening process comprises the step of contacting the base glass with first strengthening liquid, and the first strengthening liquid is sodium nitrate molten salt; the second chemical strengthening process comprises the step of contacting the glass after the first chemical strengthening treatment with a second strengthening solution, wherein the second strengthening solution is a molten salt containing 20-30wt% of sodium nitrate and 70-80wt% of potassium nitrate based on the total weight of the second strengthening solution.
4. The production method according to claim 3, wherein the conditions of the first chemical strengthening treatment include: the temperature is 380-420 ℃, and the time is 1-3 hours; the conditions of the second chemical strengthening treatment include: the temperature is 370-380 deg.C, and the time is 0.15-3 hr.
5. A method according to claim 3, wherein the second strengthening fluid is a molten salt comprising 25-30wt% sodium nitrate and 70-75wt% potassium nitrate, based on the total weight of the second strengthening fluid.
6. The production method according to claim 3, wherein the SiO is contained in the glass in an amount of 50 to 57% by mass as an oxide 2 27% -34% of Al 2 O 3 2% -4% of Na 2 O, 1% -2% of K 2 O, 6-10% of Li 2 O, 0-2% of B 2 O 3 And 3% -5% of ZrO 2 。
7. The production method according to claim 3, wherein the step (1) includes: mixing and melting raw materials for preparing the glass, and sequentially carrying out casting molding, annealing, cutting and polishing treatment to obtain the base glass.
8. Glass produced by the production method according to any one of claims 4 to 7.
9. The glass according to claim 8, wherein the glass has a maximum compressive stress CS >900MPa, a strengthening depth DOL of the Na layer of not less than 130 μm, a strengthening depth DOL of the K layer of not less than 4.0 μm, and a Vickers hardness of not less than 600HV.
10. Use of the glass according to claim 1-2, 8 or 9 as a material for a front cover or a back cover of a display screen of a smart terminal.
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| CN110803872A (en) * | 2019-12-05 | 2020-02-18 | 四川旭虹光电科技有限公司 | Inorganic strengthened glass and preparation method and application thereof |
| CN110937824A (en) * | 2019-12-05 | 2020-03-31 | 四川旭虹光电科技有限公司 | Chemically strengthened glass and preparation method and application thereof |
| CN110981188A (en) * | 2019-12-05 | 2020-04-10 | 四川旭虹光电科技有限公司 | Inorganic chemically strengthened glass and preparation method and application thereof |
| CN114671618A (en) * | 2022-04-24 | 2022-06-28 | 清远南玻节能新材料有限公司 | Microcrystalline glass, tempered glass, and preparation method and application thereof |
| US20220281769A1 (en) * | 2021-02-26 | 2022-09-08 | AGC Inc. | Chemically strengthened glass and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110803872A (en) * | 2019-12-05 | 2020-02-18 | 四川旭虹光电科技有限公司 | Inorganic strengthened glass and preparation method and application thereof |
| CN110937824A (en) * | 2019-12-05 | 2020-03-31 | 四川旭虹光电科技有限公司 | Chemically strengthened glass and preparation method and application thereof |
| CN110981188A (en) * | 2019-12-05 | 2020-04-10 | 四川旭虹光电科技有限公司 | Inorganic chemically strengthened glass and preparation method and application thereof |
| US20220281769A1 (en) * | 2021-02-26 | 2022-09-08 | AGC Inc. | Chemically strengthened glass and manufacturing method thereof |
| CN114671618A (en) * | 2022-04-24 | 2022-06-28 | 清远南玻节能新材料有限公司 | Microcrystalline glass, tempered glass, and preparation method and application thereof |
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