CN117164231A - Chemically strengthened glass and preparation method and application thereof - Google Patents
Chemically strengthened glass and preparation method and application thereof Download PDFInfo
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- CN117164231A CN117164231A CN202311170628.1A CN202311170628A CN117164231A CN 117164231 A CN117164231 A CN 117164231A CN 202311170628 A CN202311170628 A CN 202311170628A CN 117164231 A CN117164231 A CN 117164231A
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- 239000005345 chemically strengthened glass Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 157
- 238000003426 chemical strengthening reaction Methods 0.000 claims abstract description 33
- 238000005342 ion exchange Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 11
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000013001 point bending Methods 0.000 claims abstract description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000011734 sodium Substances 0.000 claims description 30
- 238000005728 strengthening Methods 0.000 claims description 24
- 238000011282 treatment Methods 0.000 claims description 19
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 12
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000008395 clarifying agent Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 235000010333 potassium nitrate Nutrition 0.000 claims description 6
- 239000004323 potassium nitrate Substances 0.000 claims description 6
- 235000010344 sodium nitrate Nutrition 0.000 claims description 6
- 239000004317 sodium nitrate Substances 0.000 claims description 6
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 150000004820 halides Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010128 melt processing Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 3
- 229910001887 tin oxide Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 7
- 238000003754 machining Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 21
- 150000002500 ions Chemical class 0.000 description 12
- 230000009286 beneficial effect Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000006025 fining agent Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000005354 aluminosilicate glass Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000006058 strengthened glass Substances 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- -1 al2O3 Chemical compound 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000004031 devitrification Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 229910001631 strontium chloride Inorganic materials 0.000 description 2
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 2
- 229910001637 strontium fluoride Inorganic materials 0.000 description 2
- 238000004017 vitrification Methods 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 239000002310 Isopropyl citrate Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000006124 Pilkington process Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000006059 cover glass Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 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
- 238000001035 drying Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000004293 potassium hydrogen sulphite Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
The application provides chemically strengthened glass, a preparation method and application thereof, wherein the chemically strengthened glass adopts SiO 2 、Al 2 O 3 、B 2 O 3 、Na 2 O、K 2 O, mgO, caO, srO and BaO are used as main raw materials and are prepared by the processes of mixing, melting, forming, annealing, machining, chemical strengthening and the like. The Young's modulus of the obtained chemically strengthened glass is more than or equal to 75GPa; the stress value of the glass surface is more than or equal to 700MPa; the ion exchange layer has a depth of more than 20 mu m, a stress value of more than or equal to 200MPa at a depth of 3 mu m from the surface of the glass, and a Vickers hardness of more than or equal to 640kgf/mm 2 The softening point of the chemically strengthened glass is 670 ℃ to 960 ℃. StrengtheningThe parameter D is in the range of 5-30, the four-point bending strength is more than or equal to 700MPa, the high surface compressive stress and the deep ion exchange depth are realized, and the excellent impact resistance and anti-drop performance are realized.
Description
Technical Field
The application relates to the technical field of glass preparation, in particular to chemically strengthened glass and a preparation method and application thereof.
Background
With the advent of the 5G communications era, information transmission has been advanced toward higher speed and higher frequency, and smart phones, smart wearable devices and tablet computers have been advanced toward thinner and higher functionality while bringing convenience to life of people, and under such trend, higher requirements are put forward for cover plate protection glass of smart devices. In the field of display screen protective glass, high-alumina silicate electronic glass subjected to chemical strengthening is generally adopted, and the glass subjected to chemical strengthening treatment has excellent anti-drop and scratch resistance.
At present, domestic aluminosilicate cover glass is usually produced by adopting a float method and an overflow method, and high-aluminosilicate glass usually contains high Al content 2 O 3 ，Al 2 O 3 The addition of (3) can lead the glass to show excellent mechanical properties, especially the anti-drop and impact resistance after strengthening are improved, but the difficulties of melting, clarifying and forming become greater with the increase of the content of the glass. Glass containing high levels of alumina typically have melting temperatures greater than 1600 ℃ and very high liquidus temperatures, which are detrimental to glass melting, fining and forming, and also have a life for both the kiln and the refractory blockGreatly influencing.
Disclosure of Invention
The application aims to solve the technical problems that: how to form the aluminosilicate glass with medium aluminum content through the compounding of the components in a specific proportion, and the aluminosilicate glass has high surface compressive stress and deep ion exchange depth after strengthening, so that the aluminosilicate glass can show excellent impact resistance and anti-drop performance, and intelligent mobile equipment can be better protected.
In order to solve the technical problems, the embodiment of the application provides chemically strengthened glass;
the embodiment of the application also provides a preparation method of the chemically strengthened glass;
the embodiment of the application further provides an intelligent equipment protection cover plate.
In some embodiments, the chemically strengthened glass comprises the following components in mole percent:
55-75% SiO 2 ；
1 to 12 percent of Al 2 O 3 ；
0 to 10 percent of B 2 O 3 ；
3 to 20 percent of Na 2 O；
0 to 10 percent of K 2 O and
2-15% MgO+CaO+SrO+BaO;
wherein, 1 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO)≥0.2；R 2 O is Na 2 O and K 2 The sum of the molar masses of O, RO is the sum of the molar masses of MgO, caO, srO and BaO.
In some embodiments, the chemically strengthened glass further comprises 0 to 7mol% ZnO; zrO 0-5 mol% 2 And 0 to 5mol% of P 2 O 5 。
In some embodiments, the chemically strengthened glass comprises the following components in mole percent:
60-72% of SiO 2 ；
3 to 10 percent of Al 2 O 3 ；
0～5% of B 2 O 3 ；
5 to 18 percent of Na 2 O；
1 to 8 percent of K 2 O；
4-13% MgO+CaO+SrO+BaO;
0-2% ZnO;
ZrO 0-2% 2 And
0 to 1% of P 2 O 5 ；
Wherein, 0.8 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO). Gtoreq.0.3, wherein R 2 O is Na 2 O and K 2 The sum of the molar masses of O and RO is the sum of the molar masses of MgO, caO, srO, baO.
In some embodiments, the chemically strengthened glass comprises the following components in mole percent:
60-72% of SiO 2 ；
3 to 10 percent of Al 2 O 3 ；
0 to 5 percent of B 2 O 3 ；
5 to 18 percent of Na 2 O；
1 to 8 percent of K 2 O；
4-13% MgO+CaO+SrO+BaO;
0.1-2% ZnO;
ZrO 0.85-2% 2 And
0.5 to 1 percent of P 2 O 5 ；
Wherein, 0.8 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO). Gtoreq.0.3, wherein R 2 O is Na 2 O and K 2 The sum of the molar masses of O and RO is the sum of the molar masses of MgO, caO, srO, baO.
In some embodiments, the mgo+cao+sro+bao comprises the following components in mole percent: mgO is more than or equal to 1mol% and less than or equal to 10mol%, caO is more than or equal to 0mol% and less than or equal to 10mol%, srO is more than or equal to 0mol% and less than or equal to 5mol% and BaO is more than or equal to 0mol% and less than or equal to 5mol%.
In the chemically strengthened glass of the present application, siO 2 As an essential component constituting a network structure, itThe addition of the glass can improve the heat resistance and chemical durability of the glass, so that the glass can obtain higher strain point and strength, but the SiO is too small 2 The main network structure of the glass is deteriorated, the dielectric constant of the glass is increased, the mechanical property and the heat resistance are deteriorated, and excessive SiO is produced 2 The melting temperature is increased, the brittleness is increased, and the production process is excessively high, and meanwhile, the ion exchange is not beneficial to the chemical strengthening, and the efficiency of the chemical strengthening is affected. Therefore, in order to further improve the comprehensive properties of the glass produced, 55mol% or less of SiO in terms of molar mass percent 2 Less than or equal to 72mol percent. Further preferably, 60mol% or less of SiO in terms of mole mass percent 2 ≤72mol％。
In the chemically strengthened glass of the present application, al 2 O 3 The glass has the advantages that the glass has high rigidity, the brittleness of the glass is increased, the glass has short material property, the forming becomes difficult, and meanwhile, the glass is easy to devitrify, the high-temperature surface tension and the high-temperature viscosity are overlarge, so that the difficulty of the glass production process is increased. Al (Al) 2 O 3 The volume of the aluminum oxide tetrahedron formed in the glass is larger than that of the silicon oxide tetrahedron in the glass, and the volume of the glass is expanded, so that the density of the glass is reduced, a strengthening channel is provided for the glass in the ion strengthening process, and the ion strengthening is promoted. When the content is too small, the space between glass networks becomes small, which is unfavorable for ion exchange and reduces the efficiency of chemical strengthening. In the chemically strengthened glass, al is calculated as oxide 2 O 3 The content of (2) is in the range of 1mol% to 12 mol%. Further preferably, 3mol% or less of Al in terms of mole percent 2 O 3 ≤10mol％。
In the chemically strengthened glass of the application, B 2 O 3 As the formed oxide of the glass, the glass can be independently formed, 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, B 2 O 3 Is also a good fluxing agent, can greatly reduce the glass melting temperature, and is beneficial to the vitrification process. But B is 2 O 3 When the content is too high, abnormal phenomena can occur, so that the heat resistance and the ion exchange capacity of the glass are obviously reduced. Comprehensively considering, based on the molar mass of the composition, B, calculated as oxide 2 O 3 The content of (2) is in the range of 0mol% to 10mol%. Further preferably, 0mol% or less of B in terms of mole percent 2 O 3 ≤5mol％。
P in chemically strengthened glass of the application 2 O 5 It is made of [ PO 4 ]The tetrahedrons are connected with each other to form a network, so that the glass network structure is in a loose state, and the network gaps become larger, thereby being beneficial to Na in the glass + K in ions and fused salts + Ion interdiffusion is carried out, and ion strengthening plays an important role in obtaining a layer with higher compressive stress in the glass strengthening process. Preferably, 0mol% in terms of mole mass percent<P 2 O 5 Less than or equal to 5mol percent. Further preferably, 1mol% or less of P in terms of mole percent 2 O 5 ≤3mol％。
In the chemically strengthened glass of the present application, na 2 O is used as an external oxide of a glass network, and can provide free oxygen to break a silicon oxygen bond so as to reduce the viscosity and melting temperature of the glass, and excessive Na 2 O reduces the chemical stability and heat resistance of the glass. Na (Na) + As a component of ion exchange with K in molten salts + Chemical exchange is carried out to form a compressive stress layer on the surface of the glass, so that the surface compressive stress of the glass is increased, and more Na is added 2 O is not beneficial to the chemical exchange of the glass and affects the strength of the glass after strengthening. K (K) 2 O and Na 2 O has similar function in the glass structure and proper amount of K 2 O will be combined with Na 2 O generates mixed alkali effect, so that the glass performance is improved. Too much K 2 O may deteriorate the chemical resistance of the glass. Therefore, in order to further improve the comprehensive properties of the resultant glass, 3mol% or less of Na in terms of molar mass percent 2 O≤20mol％、0mol％≤K 2 O is less than or equal to 10mol percent. Further preferably in mole mass percentBased on the percentage, na is 5mol percent or less 2 O≤18mol％、1mol％≤K2O≤8mol％。
In the chemically strengthened glass, mgO and CaO belong to network external oxides, the MgO has the characteristics of improving the thermal stability of the glass and reducing the brittleness, is beneficial to reducing the melting point and the high-temperature viscosity of the glass, and the excessive content of MgO can increase the density, improve the occurrence rate of cracks, devitrification and phase separation and prevent ion exchange. CaO can relax and break the network structure of the glass and has fluxing effect to a certain extent, but too high content can deteriorate the chemical stability of the glass and seriously hinder ion exchange. MgO, caO, srO, baO are all alkaline earth oxides, and their addition is effective in reducing the high temperature viscosity of the glass to improve the meltability and formability of the glass and to increase the strain point of the glass. Therefore, in order to further improve the comprehensive properties of the obtained glass, it is preferable to contain MgO+CaO+SrO+BaO in an amount of 2mol% to 15mol%, and it is more preferable that MgO+CaO+SrO+BaO is 4mol% or less and 13mol% or less, in terms of mole percent. Still more preferably, mgO is 1 mol.ltoreq.10 mol.0 mol.ltoreq.CaO, srO is 0 mol.ltoreq.5 mol.ltoreq.0 mol.ltoreq.5 mol.0 mol.ltoreq.BaO.
ZnO has 18 outer-layer electronic structures, zn relative to alkaline earth metals 2+ Ions are more easily polarized, the viscosity of the glass (such as more than 1400 ℃) can be reduced at high temperature, the viscosity of the glass containing ZnO is smaller, the movement speed of atoms is higher, crystal nuclei are not easy to form, and therefore the crystallization upper limit temperature of the glass is reduced. In addition, zn 2+ The ionic radius is close to that of the Mg2+ charge, and the ionic radius and the Mg2+ charge are similar to each other, so that the mixed alkaline earth effect can be generated, and the optimal toughness, chemical resistance and dielectric property can be generated. However, when the ZnO content is too high, the damage and depolymerization of the glass network structure by ZnO are increased, which is unfavorable for reducing the dielectric constant and dielectric loss of the glass. In combination, the ZnO content is 0 to 7mol% in terms of mole percent, and more preferably 0.1mol% or less ZnO or less than 2mol% in terms of mole percent.
ZrO in chemically strengthened glass of the application 2 Can improve glassThe mechanical property and chemical stability of the glass are large in ionic radius, and the solubility in the glass is small, so that the viscosity of the glass can be obviously increased, and the crystallization tendency of the glass is increased. But proper amount of ZrO 2 The ion exchange performance and the thermal stability of the glass can be improved. Thus, in combination, zrO is preferably contained in an amount of 0mol% or less based on the molar mass percentage of each component 2 Less than or equal to 5mol percent. More preferably, 0.85mol% or less of ZrO 2 ≤2mol％。
In some embodiments, the composition of the chemically strengthened glass further comprises a fining agent, wherein the fining agent is at least one of sulfate, nitrate, halide, tin oxide, fluoride, and stannous oxide; the fining agent is present in the chemically strengthened glass in an amount of no greater than 1mol%. The specific selection of the clarifying agent is not particularly limited, and various kinds of agents commonly used in the art may be used, for example, sulfate may be sodium sulfate, nitrate may be sodium nitrate and/or potassium nitrate, halide may be sodium chloride and/or strontium chloride, and fluoride may be calcium fluoride.
In some embodiments, the fining agent is present in the chemically strengthened glass in an amount of 0.05 to 0.8mol%.
In some embodiments, the strengthening parameter D of the chemically strengthened glass ranges from 5 to 30, where d= (4×na) 2 O+ZrO 2 +Al 2 O 3 ) and/RO, RO being the sum of the molar masses of MgO, caO, srO, baO.
In the above, na 2 O is an ion-exchange component, zrO 2 And Al 2 O 3 All provide channels for ion exchange, and play a beneficial role; mgO, caO, srO, baO is a component which is unfavorable for ion exchange, but is beneficial to other properties, and experiments prove that each property of the sample can be excellent under the proportion range of the formula.
In some embodiments, the chemically strengthened glass has a density of from 2.25 to 2.6g/cm 3 The chemically strengthened glass has a softening point of 670 ℃ to 960 ℃.
In some embodiments, the chemically strengthened glass has a density of from 2.35 to 2.55g/cm 3 The chemical strengtheningThe softening point of the glass is 700-910 ℃;
the depth of the ion exchange layer of the chemically strengthened glass is more than 20 mu m, the surface compressive stress of the glass is more than or equal to 600MPa, the four-point bending strength is more than or equal to 700MPa, and the Vickers hardness is more than or equal to 640kgf/mm 2 Young's modulus of 75GPa or more. When an object is deformed by an external factor (stress, humidity change, etc.), an internal force of interaction is generated between the parts in the object to resist the action of such external factor and to try to return the object from the deformed position to the position before deformation. The internal force per unit area at a certain point in the examined cross-section is called Stress. The chemical strengthening glass has a surface Compressive Stress (CS) and the greater the depth of the compressive stress layer, the higher the strength.
In some embodiments, the ion exchange layer depth is greater than 25 μm, the glass surface compressive stress is greater than or equal to 650MPa, the four-point flexural strength is greater than or equal to 700MPa, and the Vickers hardness is greater than or equal to 660kgf/mm 2 Young's modulus of 80GPa or more.
In some embodiments, the chemically strengthened glass has a strength factor ranging from 10 to 22, the strength factor calculated from the following equation:
DXS＝CS3×HV/(5ρ×R)
wherein DXS is an intensity factor; CS3 is a stress value of the chemically strengthened glass at a depth of 3 μm from the surface of the glass, E is a Young's modulus of the chemically strengthened glass, HV is a Vickers hardness of the chemically strengthened glass, ρ is a density of the chemically strengthened glass, and R is a four-point bending strength of the chemically strengthened glass.
In some embodiments, a method of making the chemically strengthened glass comprises: and mixing all the components of the chemically strengthened glass, and then sequentially carrying out melting treatment, forming treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment to form the chemically strengthened glass.
The present application is not particularly limited to the machining treatment, and may be performed by various machining methods commonly known in the art, for example, cutting, grinding, polishing, or the like, on the product obtained by the annealing treatment.
In some embodiments, the melt processing temperature is 1500 ℃ to 1650 ℃ for a period of 4 to 8 hours; the annealing treatment temperature is 550-650 ℃ and the time is 1-3h. The smaller the difference between the glass transition temperature and the softening point, the more easily and rapidly the glass solidifies when press molding and cooling are performed, and therefore, the glass does not easily melt and adhere to the press mold.
In some embodiments, the chemical strengthening treatment comprises one chemical strengthening treatment or a plurality of chemical strengthening treatments, wherein the chemical strengthening liquid adopted by the chemical strengthening treatment comprises sodium nitrate and/or potassium nitrate, the temperature of the chemical strengthening treatment is 380-480 ℃, and the time of the chemical strengthening treatment is 1-12 h. The specific strengthening temperature, molten salt ratio and strengthening time can be determined by those skilled in the art according to the actual situation, and are well known to those skilled in the art and will not be described herein.
In some embodiments, the smart device protective cover plate comprises the chemically strengthened glass, and the chemically strengthened glass is used for protecting components of the smart device. The intelligent equipment protection cover plate can be used as the protection glass of intelligent mobile equipment such as mobile phones and the like, and also can be used as the protection glass of controllers and displays.
Through the technical scheme, the chemically strengthened glass provided by the application is prepared by taking SiO2, al2O3, B2O3, na2O, K2O, mgO, caO, srO and BaO as main raw materials, firstly mixing all components, and then sequentially carrying out melting treatment, forming treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment, wherein the density is 2.25-2.6g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal expansion coefficient is (73-78) x 10 -7 The Young's modulus is greater than or equal to 75GPa at the temperature of/DEG C; the stress value (CS) of the glass surface is more than or equal to 700MPa; the depth of ion exchange layer (DOL) is more than 20 μm, the stress value (CS 3) at a depth of 3 μm from the glass surface is more than or equal to 200MPa, and the Vickers hardness is more than or equal to 640kgf/mm 2 The softening point of the chemically strengthened glass is 670 ℃ to 960 ℃. The strengthening parameter D is in the range of 5-30, the four-point bending strength (4 PB) is more than or equal to 700MPa, and the ion exchange membrane has high surface compressive stress and deep ion exchange depth andexhibits excellent impact resistance and anti-drop properties.
Detailed Description
Embodiments of the present application are described in further detail below with reference to examples. The following detailed description of embodiments is provided to illustrate the principles of the application and not to limit the scope of the application, which may be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein, but rather should be construed to include all technical solutions falling within the scope of the appended claims.
These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the application to those skilled in the art. It should be noted that: the relative arrangement of parts and steps, the composition of materials, numerical expressions and numerical values set forth in these embodiments should be construed as exemplary only and not limiting unless otherwise specifically stated.
As used herein, the word "comprising" or "comprises" and the like means that elements preceding the word encompass the elements recited after the word, and that no other elements are excluded from the possible coverage as well.
All terms used herein have the same meaning as understood by one of ordinary skill in the art to which the present application pertains, unless specifically defined otherwise. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but where appropriate, the techniques, methods, and apparatus should be considered part of the specification.
In the following examples, each material used was commercially available as not specifically described, and the method used was conventional in the art.
In some embodiments, the melt processing temperature is 1500 ℃ to 1650 ℃ for a period of 4 to 8 hours; the annealing treatment temperature is 550-650 ℃ and the time is 1-3h. The smaller the difference between the glass transition temperature and the softening point, the more easily and rapidly the glass solidifies when press molding and cooling are performed, and therefore, the glass does not easily melt and adhere to the press mold.
In some specific embodiments, the chemical strengthening treatment comprises one chemical strengthening treatment or multiple chemical strengthening treatments, wherein the chemical strengthening liquid adopted by the chemical strengthening treatment comprises sodium nitrate and/or potassium nitrate, the temperature of the chemical strengthening treatment is 380-480 ℃, and the time of the chemical strengthening treatment is 1-12 h.
In the following examples and comparative examples, glass density in g/cm was measured with reference to ASTM C-693 3 。
The coefficient of thermal expansion of glass at 50-350℃was measured with a horizontal dilatometer in units of 10 with reference to ASTM E-228 -7 /℃。
Young's modulus of glass in GPa was measured by reference to ASTM C-623 using a materials mechanics tester.
The Vickers hardness of glass was measured in kgf/mm using a Vickers hardness tester with reference to ASTM E-384 2 。
4PB was measured in MPa using a universal tester with reference to ASTM E-1820.
The glass height Wen Nianwen curve is determined with reference to ASTM C-965 using a rotary high temperature viscometer, wherein 40000P corresponds to a molding temperature T4 in degrees Celsius.
The glass liquidus temperature TL was measured in degrees Celsius using a step furnace method with reference to ASTM C-829.
The glass surface compressive stress and ion exchange depth (in MPa) were measured using an FSM-6000LE surface stress meter.
Examples 1 to 6
The chemically strengthened glass provided in this example comprises the following components:
55 to 75mol percent of SiO 2 ；
1 to 12mol% of Al 2 O 3 ；
0 to 10mol% of B 2 O 3 ；
3 to 20mol% of Na 2 O；
0 to 10mol% of K 2 O；
2 to 15mol% of MgO+CaO+SrO+BaO;
0 to 7mol% of ZnO;
ZrO 0-5 mol% 2 And
0 to 5mol% of P 2 O 5 ；
Wherein, 1 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO)≥0.2；R 2 O is Na 2 O and K 2 The sum of the molar masses of O, RO is the sum of the molar masses of MgO, caO, srO and BaO.
The specific contents of the above components are shown in Table 1, the components are weighed according to Table 1, mixed well, and the mixture is poured into a platinum crucible, then heated in a 1700℃resistance furnace for 5 hours, and stirred using a platinum rod to discharge bubbles. Pouring the melted glass liquid into a stainless steel cast iron grinding tool to form a specified blocky glass product, annealing the glass product in an annealing furnace for 2 hours, and turning off a power supply and cooling to 25 ℃ along with the furnace. Cutting, grinding and polishing the glass product, and then cleaning with deionized water and drying to obtain glass with the thickness of 0.7 mm. And then carrying out ion exchange to obtain the chemically strengthened glass, wherein the strengthening salt is mixed salt of potassium nitrate and sodium nitrate in a ratio of 20:80, the strengthening temperature is 390 ℃, and the strengthening time is 2 hours.
The respective properties of each glass product were measured, and the results are shown in Table 1.
TABLE 1 chemical strengthened glass of examples 1-6 each component and Properties
Examples 7 to 12
The chemically strengthened glass of examples 7 to 12 were substantially the same as that of examples 1 to 6 in terms of the content, and were prepared by the same preparation method as that of examples 1 to 6, with the specific reference to Table 2, to obtain glass products having a thickness of 0.7 mm.
The respective properties of each glass product were measured, and the results are shown in Table 2.
TABLE 2 chemical strengthened glass of examples 7-12 Components and Properties
Comparative examples 1 to 3
The chemically strengthened glass of this comparative example was substantially the same as that of examples 1 to 6 in terms of the content, and was prepared by the same preparation method as that of examples 1 to 6, with the specific reference to Table 3, to obtain a glass product having a thickness of 0.7 mm.
The respective properties of each glass product were measured, and the results are shown in Table 3.
TABLE 3 chemical strengthened glass of comparative examples each component and property
The experimental results of examples 1-12 above show that the density of the chemically strengthened glass of the present application is 2.25-2.6g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The thermal expansion coefficient is (73-78) x 10 -7 The Young's modulus is greater than or equal to 75GPa at the temperature of/DEG C; the stress value (CS) of the glass surface is more than or equal to 700MPa; the depth of ion exchange layer (DOL) is more than 20 μm, the stress value (CS 3) at a depth of 3 μm from the glass surface is more than or equal to 200MPa, and the Vickers hardness is more than or equal to 640kgf/mm 2 The softening point of the chemically strengthened glass is 670 ℃ to 960 ℃.
(Al of comparative examples 1 and 3 2 O 3 +B 2 O 3 )/(R 2 O+RO) ratioValues greater than 0.8 lead to an increase in the liquidus temperature and the T4 temperature of the glass, which is disadvantageous for production.
The chemical strengthening glass of the application has a strengthening parameter D in the range of 5-30, a D value of 42.18 in comparative example 2, and poor strengthening effect; the D value of comparative example 3 was 3.76, and the ion exchange depth of the glass was small.
The four-point bending strength (4 PB) of the chemically strengthened glass of the application is more than or equal to 700MPa, and the four-point bending strength (4 PB) of comparative example 2 is 652MPa.
Experiments show that when the strength factor (DXS) of the chemically strengthened glass is in the range of 9-22, the chemically strengthened glass has high surface compressive stress and deep ion exchange depth, and has excellent impact resistance and anti-falling performance.
Single factor test
In the chemically strengthened glass of the present application, al 2 O 3 The glass has the advantages that the glass has high rigidity, the brittleness of the glass is increased, the glass has short material property, the forming becomes difficult, and meanwhile, the glass is easy to devitrify, the high-temperature surface tension and the high-temperature viscosity are overlarge, so that the difficulty of the glass production process is increased. Al (Al) 2 O 3 The volume of the aluminum oxide tetrahedron formed in the glass is larger than that of the silicon oxide tetrahedron in the glass, and the volume of the glass is expanded, so that the density of the glass is reduced, a strengthening channel is provided for the glass in the ion strengthening process, and the ion strengthening is promoted. When the content is too small, the space between glass networks becomes small, which is unfavorable for ion exchange and reduces the efficiency of chemical strengthening. In the chemically strengthened glass, al is calculated as oxide 2 O 3 The content of (2) is 1-12 mol%, and the prepared glass has better performance. Further preferably, 3mol% or less of Al in terms of mole percent 2 O 3 Less than or equal to 10mol percent, and the prepared glass has optimal performance.
In the chemically strengthened glass of the application, B 2 O 3 As a glass forming oxide, glass alone can be produced, which is added withCan enhance the chemical stability and mechanical property of the glass, reduce the thermal expansion coefficient of the glass, and accelerate the ion exchange process, B 2 O 3 Is also a good fluxing agent, can greatly reduce the glass melting temperature, and is beneficial to the vitrification process. But B is 2 O 3 When the content is too high, abnormal phenomena can occur, so that the heat resistance and the ion exchange capacity of the glass are obviously reduced. Comprehensively considering, based on the molar mass of the composition, B, calculated as oxide 2 O 3 The content of (2) is in the range of 0mol% to 10mol%. Further preferably, 0mol% or less of B in terms of mole percent 2 O 3 ≤5mol％。
P in chemically strengthened glass of the application 2 O 5 It is made of [ PO 4 ]The tetrahedrons are connected with each other to form a network, so that the glass network structure is in a loose state, and the network gaps become larger, thereby being beneficial to Na in the glass + K in ions and fused salts + Ion interdiffusion is carried out, and ion strengthening plays an important role in obtaining a layer with higher compressive stress in the glass strengthening process. Preferably, 0mol% in terms of mole mass percent<P 2 O 5 Less than or equal to 5mol percent. Further preferably, 1mol% or less of P in terms of mole percent 2 O 5 ≤3mol％。
In the chemically strengthened glass of the present application, na 2 O is used as an external oxide of a glass network, and can provide free oxygen to break a silicon oxygen bond so as to reduce the viscosity and melting temperature of the glass, and excessive Na 2 O reduces the chemical stability and heat resistance of the glass. Na (Na) + As a component of ion exchange with K in molten salts + Chemical exchange is carried out to form a compressive stress layer on the surface of the glass, so that the surface compressive stress of the glass is increased, and more Na is added 2 O is not beneficial to the chemical exchange of the glass and affects the strength of the glass after strengthening. K (K) 2 O and Na 2 O has similar function in the glass structure and proper amount of K 2 O will be combined with Na 2 O generates mixed alkali effect, so that the glass performance is improved. Too much K 2 O may deteriorate the chemical resistance of the glass. Thus, in order to further improve the overall properties of the resulting glassMolar mass percent is 3mol% or less Na 2 O≤20mol％、0mol％≤K 2 O is less than or equal to 10mol percent. Further preferably, 5mol% or less of Na in terms of molar mass percent 2 O≤18mol％、1mol％≤K2O≤8mol％。
In the chemically strengthened glass, mgO and CaO belong to network external oxides, the MgO has the characteristics of improving the thermal stability of the glass and reducing the brittleness, is beneficial to reducing the melting point and the high-temperature viscosity of the glass, and the excessive content of MgO can increase the density, improve the occurrence rate of cracks, devitrification and phase separation and prevent ion exchange. CaO can relax and break the network structure of the glass and has fluxing effect to a certain extent, but too high content can deteriorate the chemical stability of the glass and seriously hinder ion exchange. MgO, caO, srO, baO are all alkaline earth oxides, and their addition is effective in reducing the high temperature viscosity of the glass to improve the meltability and formability of the glass and to increase the strain point of the glass. Therefore, in order to further improve the comprehensive properties of the obtained glass, it is preferable to contain MgO+CaO+SrO+BaO in an amount of 2mol% to 15mol%, and it is more preferable that MgO+CaO+SrO+BaO is 4mol% or less and 13mol% or less, in terms of mole percent. Still more preferably, mgO is 1 mol.ltoreq.10 mol.0 mol.ltoreq.CaO, srO is 0 mol.ltoreq.5 mol.ltoreq.0 mol.ltoreq.5 mol.0 mol.ltoreq.BaO.
ZnO has 18 outer-layer electronic structures, zn relative to alkaline earth metals 2+ Ions are more easily polarized, the viscosity of the glass (such as more than 1400 ℃) can be reduced at high temperature, the viscosity of the glass containing ZnO is smaller, the movement speed of atoms is higher, crystal nuclei are not easy to form, and therefore the crystallization upper limit temperature of the glass is reduced. In addition, zn 2+ The ionic radius is close to that of the Mg2+ charge, and the ionic radius and the Mg2+ charge are similar to each other, so that the mixed alkaline earth effect can be generated, and the optimal toughness, chemical resistance and dielectric property can be generated. However, when the ZnO content is too high, the damage and depolymerization of the glass network structure by ZnO are increased, which is unfavorable for reducing the dielectric constant and dielectric loss of the glass. In combination, the ZnO content is 0 to 7mol% in terms of mole mass%, and further preferably in terms of mole massThe ZnO is more than or equal to 0mol percent and less than or equal to 2mol percent.
ZrO in chemically strengthened glass of the application 2 Can improve the mechanical property and chemical stability of the glass, has larger ionic radius and small solubility in the glass, can obviously increase the viscosity of the glass and increase the crystallization tendency of the glass. But proper amount of ZrO 2 The ion exchange performance and the thermal stability of the glass can be improved. Thus, in combination, zrO is preferably contained in an amount of 0mol% or less based on the molar mass percentage of each component 2 Less than or equal to 5mol percent. More preferably, 0mol% or less of ZrO 2 ≤2mol％。
In some embodiments, the composition of the chemically strengthened glass further comprises a fining agent, the fining agent being at least one of a sulfate, nitrate, halide, tin oxide, fluoride, and stannous oxide; the fining agent is present in the chemically strengthened glass in an amount of no greater than 1 mole percent. The specific selection of the clarifying agent is not particularly limited, and various kinds of agents commonly used in the art may be used, for example, sulfate may be sodium sulfate, nitrate may be sodium nitrate and/or potassium nitrate, halide may be sodium chloride and/or strontium chloride, and fluoride may be calcium fluoride.
In some embodiments, the chemically strengthened glass of embodiments 1-12 is formed into a smart device protective cover sheet for protecting components of a smart device. The intelligent equipment protection cover plate can be used as the protection glass of intelligent mobile equipment such as mobile phones and the like, and also can be used as the protection glass of controllers and displays.
Thus, various embodiments of the present application have been described in detail. In order to avoid obscuring the concepts of the application, some details known in the art have not been described. How to implement the solutions applied herein will be fully apparent to those skilled in the art from the above description.
While certain specific embodiments of the application have been described in detail by way of example, it will be appreciated by those skilled in the art that the above examples are for illustration only and are not intended to limit the scope of the application. It will be understood by those skilled in the art that the foregoing embodiments may be modified and equivalents substituted for elements thereof without departing from the scope and spirit of the application. In particular, the technical features mentioned in the respective embodiments may be combined in any manner as long as there is no structural conflict.
Claims (10)
1. The chemically strengthened glass is characterized by comprising the following components in percentage by mole:
55-75% SiO 2 ；
1 to 12 percent of Al 2 O 3 ；
0 to 10 percent of B 2 O 3 ；
3 to 20 percent of Na 2 O；
0 to 10 percent of K 2 O and
2-15% MgO+CaO+SrO+BaO;
wherein, 1 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO)≥0.2；R 2 O is Na 2 O and K 2 The sum of the molar masses of O, RO is the sum of the molar masses of MgO, caO, srO and BaO.
2. The chemically strengthened glass according to claim 1, further comprising 0 to 7mol% ZnO; zrO 0-5 mol% 2 And 0 to 5mol% of P 2 O 5 。
3. The chemically strengthened glass of claim 2, wherein the chemically strengthened glass comprises the following components in mole percent:
60-72% of SiO 2 ；
3 to 10 percent of Al 2 O 3 ；
0 to 5 percent of B 2 O 3 ；
5 to 18 percent of Na 2 O；
1 to 8 percent of K 2 O；
4-13% MgO+CaO+SrO+BaO;
0-2% ZnO;
ZrO 0-2% 2 And
0 to 1% of P 2 O 5 ；
Wherein, 0.8 is more than or equal to (Al) 2 O 3 +B 2 O 3 )/(R 2 O+RO). Gtoreq.0.3, wherein R 2 O is Na 2 O and K 2 The sum of the molar masses of O and RO is the sum of the molar masses of MgO, caO, srO, baO.
4. A chemically strengthened glass according to claim 2 or claim 3 wherein the mgo+cao+sro+bao comprises the following components in mole percent: mgO is more than or equal to 1mol% and less than or equal to 10mol%, caO is more than or equal to 0mol% and less than or equal to 10mol%, srO is more than or equal to 0mol% and less than or equal to 5mol% and BaO is more than or equal to 0mol% and less than or equal to 5mol%; the chemically strengthened glass also comprises a clarifying agent, wherein the clarifying agent is at least one of sulfate, nitrate, halide, tin oxide, fluoride and stannous oxide; the content of the clarifying agent in the chemically strengthened glass is not more than 1mol%; preferably, the content of the clarifying agent in the chemically strengthened glass is 0.05-0.8mol%; the strengthening parameter D of the chemically strengthened glass ranges from 5 to 30, wherein D= (4×Na) 2 O+ZrO 2 +Al 2 O 3 ) and/RO, RO being the sum of the molar masses of MgO, caO, srO, baO.
5. The chemically strengthened glass of any one of claims 1-4 wherein the chemically strengthened glass has a density of from 2.25 to 2.6g/cm 3 The softening point of the chemically strengthened glass is 670-960 ℃; preferably, the chemically strengthened glass has a density of from 2.35 to 2.55g/cm 3 The chemically strengthened glass has a softening point of 700 ℃ to 910 ℃;
the depth of the ion exchange layer of the chemically strengthened glass is more than 20 mu m, the surface compressive stress of the glass is more than or equal to 600MPa, the four-point bending strength is more than or equal to 700MPa, and the Vickers hardness is more than or equal to 640kgf/mm 2 Young's modulus of 75GPa or more; preferably, the depth of the ion exchange layer is greater than 25 μm, the compressive stress on the surface of the glass is greater than or equal to 650MPa, the four-point bending strength is greater than or equal to 700MPa, and the Vickers hardness is greater than or equal to 660kgf/mm 2 Young's diseaseModulus of 80GPa or more.
6. The chemically strengthened glass of any one of claims 2-4 wherein the chemically strengthened glass has a strength factor in the range of 10-22, the strength factor calculated from the equation:
DXS＝CS10×HV/(5ρ×R)
wherein DXS is an intensity factor; CS10 is a stress value of the chemically strengthened glass at a depth of 10 μm from the glass surface, E is a Young's modulus of the chemically strengthened glass, HV is a Vickers hardness of the chemically strengthened glass, ρ is a density of the chemically strengthened glass, and R is a four-point bending strength of the chemically strengthened glass.
7. A method of making the chemically strengthened glass of any one of claims 1-6, comprising: and mixing all the components of the chemically strengthened glass, and then sequentially carrying out melting treatment, forming treatment, annealing treatment, mechanical processing treatment and chemical strengthening treatment to form the chemically strengthened glass.
8. The method of claim 7, wherein the melt processing temperature is 1500 ℃ to 1650 ℃ for a period of 4 to 8 hours; the annealing treatment temperature is 550-650 ℃ and the time is 1-3h.
9. The method according to claim 7, wherein the chemical strengthening treatment comprises one chemical strengthening treatment or a plurality of chemical strengthening treatments, the chemical strengthening liquid adopted by the chemical strengthening treatment comprises sodium nitrate and/or potassium nitrate, the temperature of the chemical strengthening treatment is 380-480 ℃, and the time of the chemical strengthening treatment is 1-12 h.
10. The intelligent equipment protection cover plate is characterized by comprising the chemically strengthened glass according to any one of claims 1-6, wherein the chemically strengthened glass is used for protecting components of intelligent equipment.
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