CN115028358A - Composition for preparing chemically strengthened glass with high liquidus viscosity, chemically strengthened glass and application thereof - Google Patents
Composition for preparing chemically strengthened glass with high liquidus viscosity, chemically strengthened glass and application thereof Download PDFInfo
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- CN115028358A CN115028358A CN202210575760.XA CN202210575760A CN115028358A CN 115028358 A CN115028358 A CN 115028358A CN 202210575760 A CN202210575760 A CN 202210575760A CN 115028358 A CN115028358 A CN 115028358A
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- 239000000203 mixture Substances 0.000 title claims abstract description 46
- 239000005345 chemically strengthened glass Substances 0.000 title claims abstract description 34
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 12
- 229910018068 Li 2 O Inorganic materials 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims description 26
- 238000003426 chemical strengthening reaction Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 16
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 238000000137 annealing Methods 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008395 clarifying agent Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 235000010333 potassium nitrate Nutrition 0.000 claims description 8
- 239000004323 potassium nitrate Substances 0.000 claims description 8
- 235000010344 sodium nitrate Nutrition 0.000 claims description 8
- 239000004317 sodium nitrate Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 7
- 238000005728 strengthening Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000003623 enhancer Substances 0.000 claims description 6
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 3
- 239000013067 intermediate product Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010128 melt processing Methods 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011521 glass Substances 0.000 abstract description 127
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000005342 ion exchange Methods 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 9
- 230000001965 increasing effect Effects 0.000 description 9
- 238000010998 test method Methods 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000005354 aluminosilicate glass Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000004031 devitrification Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000006025 fining agent Substances 0.000 description 2
- 238000007496 glass forming Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 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
- 239000001301 oxygen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002310 Isopropyl citrate Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910006404 SnO 2 Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003258 bubble free glass Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 210000001808 exosome Anatomy 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004293 potassium hydrogen sulphite Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000004017 vitrification 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- 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
- C03C3/089—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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
Abstract
The invention relates to the technical field of glass manufacturing, and discloses a composition for preparing chemically strengthened glass with high liquidus viscosity, chemically strengthened glass and application thereof. The composition contains the following components which are stored in a mixing way or are respectively and independently stored: SiO 2 2 、Al 2 O 3 、B 2 O 3 、Na 2 O、Li 2 O、K 2 O、RO n 、MgO、ZrO 2 、P 2 O 5 . The glass prepared by the glass composition provided by the invention has the advantages of high liquidus viscosity, high Young modulus, high mechanical strength and the like, and the crystallization risk of the glass in the production process can be reduced to a great extent. Meanwhile, the prepared glass has higher surface compressive stress and a very deep compressive stress exchange layer after being strengthened, so that the glass has good scratch resistance and impact resistance, and can well protect electronic equipment.
Description
Technical Field
The invention relates to the technical field of glass manufacturing, in particular to a composition for preparing chemically strengthened glass with high liquidus viscosity, chemically strengthened glass and application thereof.
Background
With the coming of the 5G communication era, smart phones, smart wearable devices and tablet computers are developing towards the trend of being thinner and more functional while bringing convenience to life of people, and under the trend, higher requirements are also put forward on the mechanical performance of cover plate protective glass of smart devices.
In the field of display screen protection glass, high aluminosilicate electronic glass subjected to chemical strengthening is generally adopted, and the glass subjected to chemical strengthening has excellent drop resistance and scratch resistance.
Currently, chemical strengthening is usually performed by one-step or two-step ion exchange, so that the glass has high surface Compressive Stress (CS) and high depth of layer (DOL) of the compressive stress. Generally, the greater the surface compressive stress and the depth of the compressive stress layer, the greater the strength of the glass. However, the improvement of the mechanical properties of the glass also requires the consideration of the compressive stress inside the glass, for example, the compressive stress at the depth of 30 μm, 50 μm and 100 μm from the surface of the glass, and these parameters determine the propagation of cracks inside the glass, which directly affects the mechanical properties of the glass.
However, high Al content in high aluminosilicate glasses 2 O 3 Although the progress and depth of ion exchange can be accelerated, the scratch resistance of the glass is improved, but the melting difficulty of the glass is increased, and the temperature of 200 poise is usually over 1550 ℃, even 1650 ℃ and higher, so that the industrial manufacturing difficulty is high. Generally, such high aluminosilicate glasses have short frits, low liquidus viscosities, and a high risk of devitrification during production.
Therefore, the material property of the glass is prolonged, and the liquidus viscosity is increased, which is also an important direction for the research of the glass.
Disclosure of Invention
The invention aims to overcome the defect that the existing high-aluminosilicate glass cannot give consideration to excellent mechanical properties and processability.
In order to achieve the above object, a first aspect of the present invention provides a chemically strengthened glass composition for high liquidus viscosity production, which comprises two or more of the following components stored in admixture or separately:
SiO 2 、Al 2 O 3 、B 2 O 3 、Na 2 O、Li 2 O、K 2 O、RO n 、MgO、ZrO 2 、P 2 O 5 ；
based on the total weight of the composition, the SiO 2 Is 50-65 wt%, and the Al 2 O 3 In an amount of 20 to 40 wt%, said B 2 O 3 Is 0 to 5 wt%, the Na 2 The content of O is 3 to 10 wt%, and Li 2 The content of O is 2 to 10 weight percent, and the K is 2 The content of O is 0 to 5 weight percent, and the RO n Is 0-5 wt%, the MgO is 1-5 wt%, and the ZrO 2 In an amount of 0 to 3 wt%, said P 2 O 5 The content of (B) is 0-5 wt%;
wherein the RO n Selected from ZnO and TiO 2 At least one ofSeed;
definition K 1 ＝(SiO 2 Mass percentage of (b) + ZrO 2 Mass percentage of (B)/(Al) 2 O 3 Mass percentage of (B) + Na 2 Mass percent of O), and K 1 1.45-2.15;
definition K 2 ＝(Al 2 O 3 Mass percentage of (B) + 2 O 3 Mass percentage of (b) + ZrO 2 Mass percentage of (B) + P 2 O 5 Mass percent of (1)/(Na) 2 Mass percent of O + Li 2 Mass percentage of O + K 2 The mass percentage of O + the mass percentage of MgO), and K 2 2.55-6.00;
at the same time, B 2 O 3 Content of (A), K 2 Content of O, the RO n Of the ZrO 2 And the content of P 2 O 5 The content of (B) is not 0 at the same time.
Preferably, the SiO is present in an amount based on the total weight of the composition 2 Is 54-62 wt%, the Al 2 O 3 In an amount of 23 to 35 wt%, said B 2 O 3 Is 1-4 wt%, the Na 2 The content of O is 3.5 to 7 wt%, and Li 2 The content of O is 3-8 wt%, and K is 2 The content of O is 0.05 to 2 weight percent, and the RO n Is 0 to 3 wt%, the MgO content is 1 to 4 wt%, and the ZrO 2 In an amount of 0.5 to 1.2 wt%, said P 2 O 5 The content of (B) is 0.5-1.5 wt%;
and K is 1 Is 1.50-2.00, K 2 Is 2.65-4.00.
Preferably, a clarifying agent is included in the composition.
Preferably, the clarifying agent is at least one selected from sulfate, nitrate, halide, stannic oxide and stannous oxide.
A second aspect of the invention provides a method of making a high liquidus viscosity chemically strengthened glass, the method comprising:
(1) mixing the components of the composition for preparing the chemically strengthened glass with high liquidus viscosity, which is described in the first aspect, to obtain a mixture I;
(2) and sequentially carrying out melting treatment, molding treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment on the mixture I.
Preferably, in step (1), the mixing conditions at least satisfy: stirring is carried out under the stirring condition, the rotating speed of the stirring is 20-50rpm, and the time is 5-20 min.
Preferably, in the step (2), the conditions of the melt processing at least satisfy: the temperature is 1500-.
Preferably, in the step (2), the annealing treatment conditions at least satisfy: the temperature is 550-650 ℃ and the time is 1-3 h.
According to a preferred embodiment, the operation of the chemical strengthening treatment comprises:
in the presence of a solvent, carrying out contact reaction on an intermediate product obtained after mechanical processing and a chemical enhancer;
wherein the conditions of the contact reaction at least satisfy: the temperature is 390-450 ℃, and the time is 1-6 h.
Preferably, the chemical enhancer is at least one selected from sodium nitrate and potassium nitrate.
A third aspect of the present invention provides a chemically strengthened glass with a high liquidus viscosity obtained by the method described in the second aspect.
Preferably, the chemically strengthened glass has a Young's modulus of 81-85GPa, a Vickers hardness of 640-680kgf/mm 2 。
Preferably, the CS _30, the CS _50 and the CS _100 of the chemically strengthened glass are not lower than 230MPa, not lower than 170MPa and higher than 70MPa respectively.
A fourth aspect of the invention provides a use of the high liquidus viscosity chemically strengthened glass of the third aspect in the manufacture of a smart device protective cover sheet.
According to the invention, the dosage of each component in the glass composition is accurately adjusted so that the mass half-component content of each component meets K 1 And K 2 Define and Range, and control Li 2 O、Na 2 O、K 2 O is in a reasonable range to provide appropriate free oxygen, to break the silicon-oxygen bond, to lower the melting temperature, to promote the [ BO ] of the network structure 4 ]While allowing a certain amount of [ BO ] to be present in the glass structure 3 ]The glass does not participate in the construction of a glass network structure, can block the expansion of microcracks when the glass cracks expand, and ensures that the mechanical property of the glass is improved to a certain extent, thereby obtaining the glass with excellent mechanical property and processing property.
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.
As described above, the first aspect of the present invention provides a composition for producing a chemically strengthened glass having a high liquidus viscosity, which comprises two or more of the following components stored in admixture or separately:
SiO 2 、Al 2 O 3 、B 2 O 3 、Na 2 O、Li 2 O、K 2 O、RO n 、MgO、ZrO 2 、P 2 O 5 ；
the SiO is present in an amount based on the total weight of the composition 2 Is 50-65 wt%, and the Al 2 O 3 In an amount of 20 to 40 wt%, said B 2 O 3 Is 0 to 5 wt%, the Na 2 The content of O is 3 to 10 wt%, and Li 2 The content of O is 2 to 10 weight percent, and the K is 2 The content of O is 0 to 5 weight percent, and the RO n Is 0-5 wt%, the MgO is 1-5 wt%, and the ZrO 2 In an amount of 0 to 3 wt%, said P 2 O 5 The content of (B) is 0-5 wt%;
wherein the RO n Selected from ZnO and TiO 2 At least one of (a);
definition K 1 ＝(SiO 2 Mass percentage of (b) + ZrO 2 Mass percent of (C)/(Al) 2 O 3 Mass percentage of (B) + Na 2 Mass percent of O), and K 1 1.45-2.15;
definition K 2 ＝(Al 2 O 3 Mass percentage of (B) + 2 O 3 Mass percentage of (b) + ZrO 2 Mass percentage of (B) + P 2 O 5 Mass percent of (1)/(Na) 2 Mass percent of O + Li 2 Mass percentage of O + K 2 The mass percentage of O + the mass percentage of MgO), and K 2 2.55-6.00;
at the same time, B 2 O 3 Content of (A), K 2 Content of O, the RO n Content of (b), the ZrO 2 And the content of P 2 O 5 The content of (b) is not 0 at the same time.
The inventor of the invention defines the content range of each component in the glass fiber composition provided by the invention based on the following thought:
SiO 2 the addition of the component necessary for forming a network structure can improve the heat resistance and chemical durability of the glass, and enable the glass to obtain a higher strain point. However, too little SiO 2 The main network structure of the glass is poor, and the mechanical property and the heat resistance are poor; excess SiO 2 The melting temperature of the glass is increased, the brittleness of the glass is increased, the production process is over-required, and ion exchange in chemical strengthening is not facilitated, so that the chemical strengthening efficiency is influenced. The inventors of the present invention found, after extensive studies, that when SiO is used 2 When the content of (A) is more than or equal to 50 wt%, the mechanical property, thermal stability and chemical resistance of the prepared glass can be improved, but when the content is too high, the flexibility of the glass is reduced. Therefore, in order to further improve the comprehensive performance of the prepared glass, the SiO in the glass composition provided by the invention is limited 2 In an amount of 50-65wt％。
Al 2 O 3 The addition of the composite material can promote the integrity of network connection, greatly improve the heat resistance, ion exchange depth, surface compressive stress and mechanical stability of the glass, and simultaneously lead the structure of the glass to tend to be rigid and increase the brittleness of the glass; the glass is easy to devitrify, the high-temperature surface tension and the high-temperature viscosity are too high, and the difficulty of the glass production process is increased; however, if the content is too large, the glass has a short glass gob property and is difficult to mold. In addition, due to Al 2 O 3 The aluminum tetrahedra formed in the glass has a larger volume than the silicon tetrahedra, so that the glass expands in volume, thereby reducing the density of the glass, providing strengthening channels for ions in the glass during chemical strengthening and promoting the ion strengthening. The inventors of the present invention comprehensively consider that Al in the glass composition provided by the present invention is limited 2 O 3 The content of (B) is 20-40 wt%.
B 2 O 3 The oxide serving as a glass forming body can independently generate glass, and the addition of the oxide can enhance the chemical stability and mechanical property of the glass, reduce the thermal expansion coefficient of the glass and accelerate the ion exchange process during chemical strengthening; in addition, B 2 O 3 Is also a good fluxing agent, can greatly reduce the melting temperature of the glass, and is also beneficial to the vitrification process. But B 2 O 3 When the content is too high, an abnormal phenomenon occurs, so that the heat resistance of the glass and the ion exchange capacity during chemical strengthening are remarkably reduced. The inventors of the present invention considered comprehensively that B in the glass composition provided by the present invention is limited 2 O 3 The content of (B) is 1-5 wt%.
Li 2 O is one of essential components of the basic glass, belongs to network external components, can obviously reduce the viscosity and the melting difficulty of the glass by adding the O, and is taken as a main component of ion exchange during chemical strengthening, and proper Li 2 O can significantly improve the mechanical strength and surface hardness of the glass and increase the rate of ion exchange. In the chemical strengthening process, the NaNO is reacted with NaNO in the molten salt 3 Na in (1) + Ion exchange to provideThe depth of the compressive stress layer of the glass is increased, and the impact resistance of the glass is further improved. Therefore, Li in the glass composition provided by the present invention is limited 2 The content of O is 2-10 wt%.
Na 2 O is used as a network exosome oxide of the glass, and the addition of the oxide can provide free oxygen to break silicon-oxygen bonds so as to reduce the viscosity and melting temperature of the glass; but excessive Na 2 O reduces the chemical stability and heat resistance of the glass. Na contained therein + As a component of ion exchange during chemical strengthening, with K in the molten salt + Carrying out chemical exchange to form a compressive stress layer on the surface of the glass, and increasing the surface compressive stress of the glass; and too little Na 2 O is detrimental to the chemical exchange of the glass and thus affects the strength of the glass after strengthening. Therefore, Na is limited in the glass composition provided by the present invention 2 The content of O is 3-10 wt%.
K 2 O is also a glass exo-network oxide, with Na 2 O has a similar effect in the glass structure, and a proper amount of K 2 O will react with Na 2 O generates mixed alkali effect, so that the glass performance is improved. Therefore, the inventors of the present invention have studied to define K in the glass composition provided by the present invention 2 The content of O is 0 to 3 wt%.
MgO、ZnO、TiO 2 As chemically strengthened ion exchange modified oxides for glass, the addition of the chemically strengthened ion exchange modified oxides can effectively reduce the high-temperature viscosity of the glass, thereby improving the melting property and the forming property of the glass and accelerating the ion exchange process of the glass. Wherein, MgO also has the functions of improving the thermal stability of the glass and reducing the brittleness; the excessive MgO content increases the density of the glass and increases the incidence of cracks, devitrification and phase separation. Wherein, ZnO can also effectively improve ion exchange performance, and has the functions of improving the thermal stability of glass, and increasing the chemical resistance, mechanical strength and flexibility of the glass below the softening point of the ZnO. However, the content of ZnO is too large to improve the glass forming stability. In alumino-silicate glasses, Ti 4+ Mainly by [ TiO ] 6 ]The octahedron is filled in the gaps of the glass network, thereby being beneficial to promoting the ion exchange process during chemical strengthening and improving the chemical strengthening performance. At the same time because of ZnO and TiO 2 Has larger ionic radius and field intensity, and simultaneously has the function of enhancing the heat treatment stability and/or the thermochemical treatment stability, and can reduce the warping deformation. However, too much content of both results in an increase in glass density and a decrease in glass formation stability. The inventors of the present invention have comprehensively considered to limit ZnO and TiO in the glass composition provided by the present invention 2 The content of (B) is limited to 0-5 wt%, and the content of MgO is limited to 0-5 wt%.
ZrO 2 The addition of the (B) can improve the mechanical property and chemical resistance stability of the glass, the ionic radius of the glass is larger, the solubility of the glass in the glass is small, and the viscosity and the crystallization tendency of the glass can be obviously increased. But an appropriate amount of ZrO 2 The ion exchange performance and thermal stability of the glass can be improved. Thus, the ZrO content of the glass composition provided by the present invention is limited 2 The content of (B) is 0-3 wt%.
P 2 O 5 In glass with [ PO ] 4 ]The tetrahedrons are connected into a network, so that the glass network structure is in a loose state, and the network gaps are enlarged, thereby being beneficial to Na in the glass + K in ions and molten salts + Ions are diffused mutually, and the ion strengthening plays a promoting role in the chemical strengthening process of the glass, and plays an important role in obtaining a higher compressive stress layer. Thus, P in the glass composition provided by the present invention is limited 2 O 5 The content of (B) is 0-5 wt%.
In addition, the inventor of the invention also finds that when the mass percentage of each component meets K through creative research 1 And K 2 The definition and the range are beneficial to the improvement of the mechanical property and the processability of the glass.
Preferably, the SiO is present in an amount based on the total weight of the composition 2 Is 54-62 wt%, the Al 2 O 3 In an amount of 23 to 35 wt%, said B 2 O 3 Is 1-4 wt%, the Na 2 The content of O is 3.5 to 7 wt%, and Li 2 The content of O is 3 to 8 weight percent, and the K is 2 The content of O is 0.05 to 2 weight percent, and the RO n Is 0 to 3 wt%, the MgO content is 1 to 4 wt%, and the ZrO 2 Of (1) containsIn an amount of 0.5 to 1.2 wt%, said P 2 O 5 The content of (B) is 0.5-1.5 wt%;
and K is 1 Is 1.50-2.00, K 2 Is 2.65-4.00.
Preferably, a clarifying agent is optionally included in the composition.
Preferably, the clarifying agent is present in an amount of 0 to 1 wt%, based on the total weight of the composition. More preferably, the clarifying agent is present in an amount of 0.05 to 0.80 wt%, based on the total weight of the composition.
In the present invention, the kind of the fining agent is not particularly limited, and may be selected by those skilled in the art according to the technical means known in the art, but in order to obtain a uniform bubble-free glass, the fining agent is preferably at least one selected from the group consisting of sulfate, nitrate, halide, tin oxide, and stannous oxide. Illustratively, the sulfate may be sodium sulfate, the nitrate may be at least one of sodium nitrate and potassium nitrate, the chloride may be at least one of sodium chloride and strontium chloride, and the fluoride may be calcium fluoride, etc.
As previously mentioned, a second aspect of the invention provides a method of making a high liquidus viscosity chemically strengthened glass, the method comprising:
(1) mixing the components of the high liquidus viscosity chemically strengthened glass composition of the first aspect to obtain a mixture I;
(2) and sequentially carrying out melting treatment, molding treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment on the mixture I.
Preferably, in step (1), the mixing conditions at least satisfy: stirring is carried out under the stirring condition, the rotating speed of the stirring is 20-50rpm, and the time is 5-20 min.
It should be noted that, in the present invention, there is no particular limitation on the temperature and time of the melting treatment and the annealing treatment, and those skilled in the art can select them according to the technical means known in the art, but in order to obtain chemically strengthened glass with better mechanical properties, the present invention provides a preferred embodiment, and in the step (2), the conditions of the melting treatment at least satisfy: the temperature is 1500 ℃ and 1650 ℃, and the time is 4-8 h.
Preferably, in the step (2), the annealing treatment is performed under conditions at least satisfying: the temperature is 550-650 ℃ and the time is 1-3 h.
In the present invention, the machining method is not particularly limited, and various machining methods known in the art may be used, and the machining method may be exemplified by cutting, grinding, polishing, and the like of the product obtained by the annealing treatment.
According to a preferred embodiment, the operation of the chemical strengthening treatment comprises:
in the presence of a solvent, carrying out contact reaction on the intermediate product after mechanical processing and a chemical enhancer;
wherein the conditions of the contact reaction at least satisfy: the temperature is 390-450 ℃, and the time is 1-6 h.
Preferably, the chemical enhancer is at least one selected from sodium nitrate and potassium nitrate.
It is noted that when a combination of both sodium nitrate and potassium nitrate is used, the ratio of the two amounts can be determined by one skilled in the art by combining techniques known in the art with practical considerations. Illustratively, the ratio of the sodium nitrate to the potassium nitrate is (1: 99) - (99: 1).
As previously mentioned, a third aspect of the present invention provides a chemically strengthened glass with a high liquidus viscosity prepared by the method of the second aspect.
Preferably, the chemically strengthened glass has a Young's modulus of 81-85GPa, a Vickers hardness of 640-680kgf/mm 2 。
Preferably, the CS _30, the CS _50 and the CS _100 of the chemically strengthened glass are not lower than 230Mpa, not lower than 170Mpa and higher than 70Mpa respectively.
As previously mentioned, a fourth aspect of the present invention provides a use of the high liquidus viscosity chemically strengthened glass of the third aspect in the manufacture of a smart device protective cover sheet.
The present invention will be described in detail below by way of examples.
In the following examples, the raw materials used are all commercially available unless otherwise specified.
In the following examples, the total amount of the composition used is 100g unless otherwise specified.
In the present invention, the room temperature means 25 ± 2 ℃ unless otherwise specified.
Example 1
(1) 56.89g of SiO were mixed at room temperature 2 26.00g of Al 2 O 3 3.00g of B 2 O 3 5.00g of Na 2 O, 5.00g of Li 2 O, 0.01g of K 2 O, 2.10g of MgO, 1.00g of ZrO 2 1.00g of P 2 O 5 And 0.20g of SnO 2 (clarifying agent) stirring at the rotating speed of 25rpm for 10min to obtain a mixture I;
(2) adding the mixture I into a platinum crucible, heating and treating at 1650 ℃ for 4 hours in a lifting furnace, stirring, exhausting, adding into a mold, forming into block glass, then placing the block glass into an annealing furnace, annealing at 580 ℃ for 2 hours at constant temperature, cooling to room temperature along with the furnace, cutting, grinding and polishing the obtained block glass, and soaking the obtained block glass and the obtained glass primary product in a weight ratio of sodium nitrate to potassium nitrate of 85: 15 in the molten salt, strengthening for 2h at 390 ℃ to obtain chemically strengthened glass I; and then soaking the chemically strengthened glass I in a solution of sodium nitrate and potassium nitrate in a weight ratio of 5: strengthening in the molten salt of 95 ℃ for 1h at 400 ℃ to obtain the chemically strengthened glass S1.
Examples 2 to 12
Examples 2 to 12 were carried out in a similar manner to example 1, except that the amounts of the raw materials were varied to obtain glasses S2, S3, S4, S5, S6, S7, S8, S9, S10, S11 and S12, respectively, as shown in table 1.
Comparative example 1
This comparative example was conducted in a similar manner to example 1, except that the starting materials were used in different amounts and the remaining conditions were the same as in example 1, to give glass DS1, see Table 1 for details.
Comparative example 2
This comparative example was conducted in a similar manner to example 1 except that the starting materials were used in different amounts and the remaining conditions were the same as in example 1 to obtain glass DS2, as shown in Table 1.
Comparative example 3
This comparative example was conducted in a similar manner to example 1 except that the starting materials were used in different amounts and the remaining conditions were the same as in example 1 to obtain glass DS3, as shown in Table 1.
Comparative example 4
This comparative example was carried out in a similar manner to example 1, except that: without using B 2 O 3 、K 2 O、ZrO 2 And P 2 O 5 Otherwise, the conditions were the same as in example 1, giving glass DS4, see Table 1 for details.
TABLE 1
TABLE 1
Test example
The glasses prepared in the examples and comparative examples were subjected to the following tests, the specific test methods are as follows, and the specific results are shown in table 2:
(1) the density of the glass is determined in g/cm according to the test method in ASTM C-693 3 。
(2) The coefficient of thermal expansion of the glass at 50-350 ℃ is determined in units of 10 using a horizontal dilatometer according to the test method in ASTM E-228 -7 /℃。
(3) Young's modulus of glass was measured in GPa using a Material mechanical testing machine according to the test method in ASTM C-623.
(4) Vickers hardness of glass was measured using a Vickers hardness tester in kgf/mm according to the test method in ASTM E-384 2 。
(5) The strain point of the glass was measured in degrees centigrade using an annealing point strain point tester according to the test method in ASTM C-336.
(6) The high temperature visco-temperature curve of the glass was determined using a rotary high temperature viscometer with reference to the test method in ASTM C-965, where the 40000P viscosity corresponds to a forming temperature T4 in units of ℃.
(7) The upper devitrification temperature limit of the glass is determined using the temperature gradient furnace method with reference to the test method in ASTM C-829, wherein the liquidus temperature TL is measured in degrees Celsius.
(8) The compressive stress (in MPa) at the glass surface, the depth (in μm) of the compressive stress layer, the partial compressive stress (in MPa) at a depth of 30 μm from the glass surface, and the partial compressive stress (in MPa) at a depth of 50 μm from the glass surface were measured by a FSM-6000LE surface stress meter.
TABLE 2
TABLE 2
As can be seen from the results in Table 2, the glass prepared by the composition provided by the invention has the advantages of high liquidus viscosity, high Young's modulus, high mechanical strength and the like, and the crystallization risk of the glass in the production process can be reduced to a great extent. The glass prepared at the same time has higher surface compressive stress after being strengthened and a very deep compressive stress exchange layer, wherein the partial compressive stress (CS _30) with the depth of 30 mu m from the surface of the glass is more than or equal to 230MPa, the partial compressive stress (CS _50) with the depth of 50 mu m from the surface of the glass is more than 170MPa, and the partial compressive stress (CS _100) with the depth of 100 mu m from the surface of the glass is more than 70MPa, so that the glass has good scratch resistance and impact resistance, and can well protect electronic equipment.
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 (11)
1. A composition for preparing chemically strengthened glass with high liquidus viscosity, which is characterized by comprising the following components stored in a mixed manner or independently:
SiO 2 、Al 2 O 3 、B 2 O 3 、Na 2 O、Li 2 O、K 2 O、RO n 、MgO、ZrO 2 、P 2 O 5 ；
based on the total weight of the composition, the SiO 2 Is 50-65 wt%, and the Al 2 O 3 In an amount of 20 to 40 wt%, said B 2 O 3 Is 0 to 5 wt%, the Na 2 The content of O is 3 to 10 wt%, and Li 2 The content of O is 2-10 wt%, and K is 2 The content of O is 0 to 5 weight percent, and the RO n Is 0-5 wt%, the MgO is 1-5 wt%, and the ZrO 2 In an amount of 0 to 3 wt%, said P 2 O 5 The content of (B) is 0-5 wt%;
wherein the RO n Selected from ZnO and TiO 2 At least one of;
definition K 1 ＝(SiO 2 Mass percentage of (b) + ZrO 2 Mass percent of (C)/(Al) 2 O 3 Mass percentage of (B) + Na 2 Mass percent of O), and K 1 1.45-2.15;
definition K 2 ＝(Al 2 O 3 Mass percentage of (B) + 2 O 3 Mass percentage of (b) + ZrO 2 Mass percentage of (B) + P 2 O 5 Mass percent of (1)/(Na) 2 Mass percent of O + Li 2 Mass percentage of O + K 2 The mass percentage of O + the mass percentage of MgO), and K 2 Is 2.55-6.00;
at the same time, B 2 O 3 Content of (b), said K 2 Content of O, the RO n Of the ZrO 2 And the content of P 2 O 5 The content of (B) is not 0 at the same time.
2. The composition of claim 1, wherein the SiO is present in an amount based on the total weight of the composition 2 Is 54-62 wt%, the Al 2 O 3 In an amount of 23 to 35 wt%, said B 2 O 3 Is 1-4 wt%, the Na 2 The content of O is 3.5 to 7 wt%, and Li 2 The content of O is 3 to 8 weight percent, and the K is 2 The content of O is 0.05 to 2 weight percent, and the RO n Is 0 to 3 wt%, the MgO content is 1 to 4 wt%, and the ZrO 2 In an amount of 0.5 to 1.2 wt%, said P 2 O 5 The content of (B) is 0.5-1.5 wt%;
and K is 1 Is 1.50-2.00, K 2 Is 2.65-4.00.
3. The composition of claim 1 or 2, wherein the composition comprises a clarifying agent; and/or the presence of a gas in the atmosphere,
the clarifying agent is at least one selected from sulfate, nitrate, halide, stannic oxide and stannous oxide.
4. A method of making a high liquidus viscosity chemically strengthened glass, comprising:
(1) mixing the components of the composition for preparing a chemically strengthened glass with high liquidus viscosity according to any one of claims 1 to 3 to obtain a mixture I;
(2) and sequentially carrying out melting treatment, molding treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment on the mixture I.
5. The method according to claim 4, wherein in step (1), the mixing condition at least satisfies: the stirring is carried out under the stirring condition, the rotating speed of the stirring is 20-50rpm, and the time is 5-20 min.
6. The method according to claim 4 or 5, wherein in step (2), the conditions of the melt processing are at least satisfied: the temperature is 1500-; and/or the presence of a gas in the gas,
in the step (2), the conditions of the annealing treatment at least satisfy: the temperature is 550-650 ℃ and the time is 1-3 h.
7. The method according to any one of claims 4 to 6, wherein the operation of chemically strengthening treatment comprises:
in the presence of a solvent, carrying out contact reaction on an intermediate product obtained after mechanical processing and a chemical enhancer;
wherein the conditions of the contact reaction at least satisfy: the temperature is 390-450 ℃, and the time is 1-6 h.
8. The method according to claim 7, wherein the chemical enhancer is at least one selected from the group consisting of sodium nitrate and potassium nitrate.
9. A high liquidus viscosity chemically strengthened glass prepared by the method of any one of claims 4 to 8.
10. The high liquidus viscosity chemically strengthened glass as defined in claim 9, wherein the chemically strengthened glass has a Young's modulus of 81-85GPa, a Vickers hardness of 640-680kgf/mm 2 (ii) a And/or the presence of a gas in the gas,
the CS _30 of the chemically strengthened glass is not lower than 230MPa, the CS _50 is not lower than 170MPa, and the CS _100 is higher than 70 MPa.
11. Use of the high liquidus viscosity chemically strengthened glass of claim 9 or 10 in the manufacture of a smart device protective cover sheet.
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