CN109626816B - Mobile phone cover glass meeting requirements of 5G communication and 3D compression molding and process method - Google Patents
Mobile phone cover glass meeting requirements of 5G communication and 3D compression molding and process method Download PDFInfo
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- 238000007906 compression Methods 0.000 title description 2
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 15
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Images
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- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B11/00—Pressing molten glass or performed glass reheated to equivalent low viscosity without blowing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/012—Tempering or quenching glass products by heat treatment, e.g. for crystallisation; Heat treatment of glass products before tempering by cooling
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/02—Tempering or quenching glass products using liquid
- C03B27/03—Tempering or quenching glass products using liquid the liquid being a molten metal or a molten salt
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/04—Tempering or quenching glass products using gas
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses mobile phone cover glass meeting the requirements of 5G communication and 3D compression molding and a process method thereof, wherein the mobile phone cover glass is alkali aluminosilicate glass, and the chemical composition of the mobile phone cover glass comprises SiO2、B2O3、Al2O3Alkali metal oxide R2O, alkaline earth and divalent metal oxides RO, a clarifying agent and a surfactant; the process method comprises the following steps: melting the batch, carrying out one-step compression molding, and carrying out chemical strengthening treatment by a three-step method to finally obtain the mobile phone cover plate glass. The dielectric constant of the mobile phone cover plate glass is only 6.35-6.43, and is reduced by 10-20% compared with the existing mobile phone cover plate glass, so that the loss of 5G high-frequency transmission signals can be well reduced; the glass softening point temperature is less than 709 ℃, and the temperature is reduced by more than 175 ℃ compared with the existing mobile phone cover plate glass, so that the oxidation and the loss of the one-step compression molding of the cover plate protective glass to the surface of the mold can be reduced, the service life of the mold is prolonged, and the surface quality of the glass is improved.
Description
Technical Field
The invention belongs to the technical field of silicate glass, relates to mobile phone cover plate glass meeting 5G communication and 3D compression molding and a process method, and particularly relates to a glass material meeting the requirements of 5G communication on high wave transmission and low dielectric loss and a mobile phone 3D cover plate glass meeting the requirements of one-step 3D compression molding on low softening point and high strength.
Background
With the rapid development of communication technology, various advanced communication technologies are emerging continuously, various information forms are provided for human beings, and the production and living requirements of people are met. The experiments of Morse telegraph communication were successful in 1837, and Bell invented telephone in 1876, so that analog telephone was used for over a hundred years, and until the beginning of the 21 st century, optical fiber communication began to be used, and humans began to enter the digital communication era driven by Internet technology.
Modern communication technologies have gone through four generations: the first generation of mobile communication technology, 1g (first generation), is a cumbersome mobile phone for mobile phones in the 80 th 20 th century, which is an analog-based cellular radiotelephone system; the second generation mobile communication technology 2g (second generation) is mobile communication based on "global communication" to realize global network, international roaming and mobile information service with complete functions, and it is based on digital voice transmission technology of TDMA as core and mainly used to support and transmit voice information transmission and short message service; the third Generation mobile communication technology, i.e., the 3rd-Generation, perfectly combines wireless communication with internet data transmission, supports high-speed data transmission with a rate of several hundred Kbps, simultaneously transmits voice and data information, and with the rapid development of smart phones, a large number of smart phones gradually cover many fields of social contact, games, life, office and the like, so that the 3G technical industry chain is mature day by day, and simultaneously provides related services such as web browsing, music and the like on the basis of providing voice transmission services for people; the fourth generation mobile communication technology is 4G (the fourth generation), 4G has ultra-high data transmission speed, the download speed reaches 100Mbps, the upload speed can reach 20Mbps, and the requirements of most users on wireless networking services can be met. 4G finds wide application in mobile video, teleconferencing, online gaming, cloud computing-based applications, navigation of augmented reality technology, emergency response, and telemedicine.
The transmission rate of the 5G (the flight generation) communication technology reaches more than 1Gbps, people can access the era of the Internet of things from a simple mobile internet, low delay, high reliability and low power consumption of communication are realized, 5G communication is internationally and internationally developed for a long time, China starts to be commercially applied in 2019 first, the 5G communication technology can bring more humanized, convenient, safe and efficient services to people, and people and surrounding things are closely connected together.
In 12 months and 7 days in 2018, the 5G communication frequency range of development and application is declared to be 2.5-2.6GHz, 3.4-3.6GHz and 4.8-4.9GHz in China. The 5G communication technology has the characteristics of high speed (the speed is more than 100 times of 4G), low time delay (the time delay is only 1ms), low energy consumption, full network coverage and the like, and can enable people to be in a network all the time, so that the internet of everything state is achieved.
The smart phone becomes an important mobile internet terminal for human, the glass material becomes an important component of the smart phone, and the glass material is applied to the smart phone and comprises front cover plate protective glass, touch control glass, display glass, light guide plate glass and rear cover plate protective glass, so that the glass is a functional material and a display material, is also a decorative material, and is formed by the front cover plate, the touch screen and the display screen to the rear cover plate, and the glass material is an ideal material. Taking the rear cover of the mobile phone as an example, the metal material can have an obvious absorption effect on the 5G high-frequency antenna, the glass material can enable electromagnetic signals to be transmitted smoothly, the metal rear cover plate needs 9 receiving/transmitting antennas, and the glass rear cover plate only needs 2 antennas, which shows that the glass material does not shield signals and has good wave-transmitting capacity. In addition, as wireless charging technology develops, a metal back cover has little application possibility, and a glass back cover may be well adequate. For 5G high-frequency signals, the glass material also needs to reduce the dielectric constant and minimize the dielectric loss, because the high permeability (light transmission and wave transmission), high hardness and wear resistance of the glass make the glass an optimal material for full-screen and full-screen curved mobile phone cover plates, but the brittleness and insufficient fall resistance of the glass are also important for the application of the glass, so that the glass is used as the cover plate of a smart phone, and the fall resistance of the glass is especially important for full-screen or full-screen curved mobile phones.
In 2013, in 10 months, samsung corporation in korea released a 3D curved screen mobile phone, which is different from the planar features of the screen of the traditional mobile phone, but has a certain radian, as shown in fig. 1. The 3D-shaped mobile phone has good holding feeling, conforms to the radian of the retina and has good video experience effect. The 3D curved surface screen is realized by the 3D structure of the glass outside the screen, commonly called 3D cover plate protection glass. The 3D curved surface screen mobile phone has larger screen area, the screen proportion is more than 93%, and the visual display effect is excellent.
The 3D cover plate protective glass is usually obtained by hot bending a sheet of flat glass with a thickness of 0.7-0.9mm, and the glass is alkali aluminosilicate glass capable of being chemically strengthened, for example, the chemical composition and chemical strengthening method of glass described in chinese patent ZL200810147442.3, the chemical composition (wt%) of the glass is as follows: SiO 22 55～65、B2O3 0.1～3、Al2O3 6～24、MgO+CaO+BaO+SrO 3～9、ZrO2 0～1、ZnO 0～2、Cl2 0.1～0.5、Sb2O3 0.1～1.0、SO3 0.1～0.5、F20.1 to 0.5; the chemical composition of the glass is prepared by a known flat glass production method, and then the glass is strengthened by a chemical toughening method, wherein the maximum ion exchange depth reaches 75 mu m, and the maximum surface compressive stress reaches 830 MPa. The chemical toughening method uses a potassium nitrate molten salt medium, the temperature is 430-490 ℃, the treatment time is 3-8 hours, and the patent shows that the treatment time is along with Al2O3The increase in content results in a softening point temperature (10)7.6Temperature corresponding to dpas viscosity) increases. The glass has high visible light transmittance, and has good impact resistance, high scratch resistance and high durability compared with common soda-lime glass, neutral medical glass and alkali-free high-alumina glass. The screen surface protection of plasma display products and liquid crystal display products, the protection of touch screens, the screen protection of cash dispensers and the screen protection of other electronic product screens (mobile phones, PDAs, media machines and the like) can be applied, and the impact and scratch damage of the glass surfaces of the display products can be effectively prevented.
At present, high-strength cover plate protective glass used for smart phones mainly takes Gorilla (Gorilla) series aluminosilicate glass of Corning corporation in America as an industrial standard pole, and has the characteristics of high strength, large elastic modulus, good wear resistance and scratch resistance and easy ion exchange enhancement of chemical strengthening.
To date in 2007, Gorilla glass Al2O3The content is continuously improved, 8 to 9 weight percent of Al is substituted from Gorilla 12O3Increasing the content to 23 to 24 weight percent of Al2O3，SiO257 to 58 weight percent of Na2O is maintained at 8-9 wt%, and 2-4 wt% of Li is added2O promotes ion exchange. In the paper "chemical enhancement ultra-thin alkali aluminosilicate glass development Profile and prospect", the Gorilla series glass softening point temperatures (10)7.6The temperature corresponding to the soft viscosity of the dPa glass) is 850-912 ℃, and the dielectric constant is more than 7.08. At present, the ion exchange surface compressive stress of the Gorilla cover plate protective glass is more than or equal to 850MPa, the surface compressive stress depth is more than or equal to 75mm, and the impact strength is up to 80 percent when the Gorilla cover plate protective glass falls from the height of 1.6m to a rough surface.
The 3D cover plate protective glass processing technological process is shown in figure 2, and comprises the working procedures of glass sheet cutting and blanking, CNC (computer controlled precision engraving) processing, hot bending forming, surface grinding and polishing, chemical strengthening, screen printing/film coating and the like. The hot bending forming process is an important process link and is a key for realizing the 3D appearance of the mobile phone. The basic technical principle of hot bending molding is to heat a sheet glass original sheet to a temperature near the softening point, and apply a certain pressure by means of a mold to mold the softened sheet glass original sheet into an unrecoverable 3D shape, wherein the hot bending molding process principle and the temperature schedule of the 3D cover plate protective glass are shown in FIG. 3.
Although the 3D cover plate protection glass hot bending forming process promotes the development of 3D appearance mobile phones, the 3D cover plate protection glass hot bending forming process still has the following problems:
1. the finished product of the 3D cover plate protective glass after hot bending forming has thinned edges, and the thickness of the glass sheet is only 0.6 to 0.7 times that of the glass sheet, as shown in figures 1 and 3; the assembled mobile phone product has relatively poor anti-falling performance, and the side part of the mobile phone cover plate is often broken;
2. the 3D cover plate protective glass hot bending forming process belongs to a secondary hot processing forming process, and energy consumption can be greatly increased;
3. the hot-bending forming temperature is near the softening point, while the softening point temperature of the existing Gorilla series glass is higher than 850 ℃, the graphite mold can only be competent, and inert gas protection and heating furnace sealing are required to be carried out on the graphite mold, even if the surface oxidation and surface collapse of the graphite mold become keys for restricting the surface quality of the 3D cover plate protective glass;
4. the uniformity of the temperature field of the heating furnace and the pressure of the die are difficult to accurately control;
5. the manufacturing cost of the 3D cover plate protective glass is high, the price of the 3D curved surface glass is 70-120 yuan/piece larger than that of the 2.5D glass, and the price is 3-4 times that of the 3D curved surface glass;
6. the 3D cover plate protective glass hot bending forming manufacturing process is difficult, and the yield is generally only 40-60% or even lower;
7. the 3D cover plate protecting glass hot bending forming efficiency is not high generally, for example, the capacity of an 18-station glass hot bending forming machine is only 700 and 1000 sheets/24 h.
Disclosure of Invention
Aiming at the problems that the hot bending forming process of the 3D cover plate protective glass is insufficient and the softening point temperature and the dielectric constant of the existing high-strength aluminosilicate glass are higher, the invention provides a glass material which can meet the requirements of 5G communication on high wave-transmitting and low dielectric loss, can meet the requirements of one-step 3D compression molding on the chemical composition of the 3D mobile phone cover plate glass with low softening point and high strength, and is suitable for chemical strengthening and reinforcing treatment.
The invention discloses a mobile phone cover plate glass meeting the requirements of 5G communication and 3D compression molding, wherein the mobile phone cover plate glass is alkali aluminosilicate glass, and the chemical composition of the mobile phone cover plate glass comprises SiO2、B2O3、Al2O3Alkali metal oxide R2O and alkaline earth and divalent metal oxides RO.
As a further improvement of the invention, the molar ratio of O/(Si + B + P + Al) is 2.08-2.12, (R)2O+RO)/(B2O3+Al2O3) The molar ratio of (A) is 1.43-1.87.
As a further improvement of the invention, R2O is Li2O and Na2O, and the RO is MgO and ZnO.
As a further improvement of the invention, the chemical composition of the mobile phone cover plate glass comprises the following components in percentage by mass:
as a further improvement of the invention, Li2O：Na2The mass ratio of O is 1: 3, the sum of the mass percentages of ZnO and MgO is 4.3-7.4.
As a further improvement of the invention, the chemical composition of the mobile phone cover glass further comprises: clarifying agents and surfactants;
the clarifying agent comprises the following components in percentage by mass:
SO3 0.2
CeO2 0.1
the surfactant comprises the following components in percentage by mass:
MoO3 0.05
Nb2O5 0.05。
the invention also discloses a technological method of the mobile phone cover plate glass, which comprises the following steps:
step (1), melting batch;
step (2), carrying out one-time compression molding to obtain a mobile phone cover plate glass blank;
the glass for one-step compression molding has the melting temperature of T2, the feeding temperature of T4, the mold-entering temperature of T6, the glass softening point temperature of T7.6, the mold-exiting temperature of T12, the melt surface tension of Be and the dielectric constant (54MHz) of epsilon;
step (3), after trimming, punching and surface polishing, carrying out chemical strengthening treatment on the mobile phone cover plate glass blank to obtain mobile phone cover plate glass;
the chemical strengthening treatment adopts a three-step strengthening process, wherein the first step and the third step are molten salt media, and the second step is an air medium; the heat treatment temperature is as follows: the temperature of the third step is more than or equal to that of the second step, and the heat treatment time is as follows: the first step time is more than or equal to the third step time.
As a further improvement of the invention, the melting temperature of T2 is less than 1516 ℃, the feeding temperature of T4 is less than 1040 ℃, the mold-entering temperature of T6 is less than 817 ℃, the softening point temperature of T7.6 glass is less than 709 ℃, the mold-exiting temperature of T12 is less than 545 ℃, the melt surface tension Sigma is less than 321mN/m, and the dielectric constant (54MHz) epsilon is less than 6.43.
As a further improvement of the present invention, the chemical strengthening treatment includes:
the first step of molten salt treatment, medium is composite molten salt, and the composition of the composite molten salt is 0-40wt% of NaNO3And 60wt% to 100wt% KNO3Heat treatment temperatureThe temperature is 370 ℃ and 410 ℃, and the treatment time is 1-3 h;
the second step of heating treatment, wherein the medium is air, the heat treatment temperature is 410-420 ℃, and the treatment time is 0.3-1 h;
the third step is molten salt treatment, the medium is 100 percent potassium nitrate molten salt, the heat treatment temperature is 420-440 ℃, and the treatment time is 1-2 h.
As a further improvement of the invention, the mobile phone cover plate glass is in a 3D shape, the thickness is 0.6-1.1mm, and the specification is less than 7 inches.
Compared with the prior art, the invention has the beneficial effects that:
the most closely related dielectric constant of the invention is only 6.35-6.43, and the dielectric constant is reduced by more than 10% compared with the prior art, so that the loss of 5G high-frequency transmission signals can be well reduced. The glass melting temperature T2 of the invention is only 1481-1516 ℃, and is also obviously lower than the prior high-aluminum (Al)2O3Not less than 13 wt%) of cover plate glass, is generally greater than 1600 deg.C, creates technological conditions for obtaining high-quality clarified and homogenized glass, and is beneficial to production energy conservation, and the working point temperature T4 of the glass is only 1007-1040 deg.C, and is lower than that of the existing high-alumina (Al)2O3Not less than 13 wt%) of cover glass 1180-1280 ℃, the glass softening point temperature T7.6 of the invention is only 691-709 ℃, the reduction amplitude is more than 175 ℃, the mold-entering temperature T6 is only 793-817 ℃ and the mold-exiting temperature T12 is 537-545 ℃, which can reduce the oxidation and the loss of the cover glass to the mold surface by one-step mold pressing, prolong the service life of the mold and improve the surface quality of the glass, in addition, the surface tension of the glass in the mold pressing temperature range is only 310-321mN/m, and compared with the existing high aluminum (Al) glass2O3Not less than 13 wt%) is commonly 345 and 365mN/m, reduces more than 10%, and creates process conditions for rapid extension of glass melt during compression molding.
After the glass is treated by a three-step chemical strengthening process, the surface compressive stress CS of the glass is almost similar to that of the prior art, but the depth DOL of an ion exchange layer reaches 103-137 mu m, which is almost 100 percent higher than that of the prior 50 mu m and 75 mu m, and after the 3D mobile phone cover plate glass with the thickness of 0.7mm manufactured by the glass is assembled with the whole machine, the falling resistance height reaches more than 2 meters, 20 falling can be endured, and the falling resistance is also higher than that of the prior 1.6 meters.
Drawings
FIG. 1 is a diagram of a cover glass of a conventional mobile phone;
FIG. 2 is a flow chart of a conventional 3D cover plate cover glass processing process;
FIG. 3 is a diagram of the principle and temperature schedule of the existing 3D cover plate protective glass hot bending forming process;
fig. 4 is a flowchart of a processing method of a cover glass of a mobile phone according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention is described in further detail below with reference to the attached drawing figures:
the invention provides mobile phone cover plate glass meeting the requirements of 5G communication and 3D compression molding, which has the advantages of low glass softening point temperature, low dielectric constant and moderate glass structure elasticity; the mobile phone cover plate glass is alkali aluminosilicate glass, and the chemical composition of the mobile phone cover plate glass comprises SiO2、B2O3、Al2O3Alkali metal oxide R2O and alkaline earth and divalent metal oxides RO.
Further, the mobile phone cover plate glass also comprises other components which mainly comprise a clarifying agent and a surfactant.
The mobile phone cover plate glass provided by the invention comprises the following components:
SiO2is an essential component for forming the framework of the oxide glass, and the basic structural unit is siliconOxygen tetrahedron [ SiO4]The higher the content and the higher the melting point, the better the chemical durability and the higher the mechanical strength, the better the influence of Si-O bond, which is beneficial to reducing the dielectric constant of the glass, pure SiO2The dielectric constant of the glass is only 3.75, but the content of SiO is high2Glass can cause great difficulty in production and manufacturing.
B2O3Also an auxiliary component constituting the skeleton of the oxide glass, B2O3The melting temperature is only 450 ℃, the melting characteristic of the glass can be promoted, the high-temperature viscosity of the glass can be reduced, and the softening point of the glass is reduced. B is2O3Boron-oxygen trigonal [ BO ] is mainly used in glass melt structure3]And boron-oxygen tetrahedron [ BO4]In two forms, especially boron oxygen trigones [ BO3]The positive and negative charges have coincident gravity centers and no polarity, so that the dielectric constant of the glass is obviously reduced, and the dielectric loss of the glass is favorably reduced. The dielectric constant of glass is mainly influenced by polarization, which includes 1) electron displacement polarization, and the electron cloud in the ion or atom is deformed under the action of an external electric field, so that the dipole moment is changed; 2) ion displacement polarization, under the action of an external electric field, positive and negative ions deviate from the original positions and change dipole moment generated when relative displacement is carried out; 3) orientation polarization is caused by the directional arrangement of polar molecules in the glass under the action of an external electric field. The dielectric constant of glass is closely related to the chemical composition, in terms of ionic polarizability and mobility. The B-O bond energy is also greater than the Si-O bond energy, which results in B2O3The glass dielectric constant is only 3.20, so B2O3It has a great contribution to lowering the dielectric constant of the glass, and is a chemical composition preferable for mass applications.
A12O3Is an intermediate oxide, can be a network former or a network exosome, and is mainly determined by a network exosome R2Number of O and RO, (R)2O+RO)/A12O3At most 1, A12O3Enter the glass network to form alundum tetrahedron (AlO)4]The remainder of the oxygen imparts boron oxygen trigonometry [ BO ]3]Partially converted into boron-oxygen tetrahedron [ BO4]If there is no A12O3In the presence of SiO2And B2O3The glass is not easy to melt mutually, and the phase separation of the glass is easy to occur, so that the stability of the glass state is reduced. A12O3Not only can adjust the network structure of the glass, but also can greatly improve the chemical stability of the glass, simultaneously can reduce the phase separation and crystallization tendency of the glass, and is also an essential component for improving the hardness and the mechanical strength of the glass, which is an important component for improving the elastic modulus, but also has obvious improvement on the viscosity of the glass, so the A12O3Too much content shortens the glass frit property and decreases the value of Δ T (T4-T7.6, T4 and T7.6 are glass viscosity 104dPa·s、107.6The corresponding temperature value for dpas, hereinafter similar symbols are to be understood).
R2O is an alkali metal oxide, which means an oxide of an element of main group IA of the periodic Table of the elements, e.g. Li2O、Na2O、K2O、Rb2O、Cs2O, etc., but the present invention uses only Li2O、Na2And O is used together, so that the alkali-mixed glass not only can play a role in the mixed alkali effect, but also can reduce the dielectric loss, improve the chemical stability, improve the melting property, reduce the glass melting temperature, reduce the low-temperature viscosity of the glass, and increase the delta T value, the glass material property and the precision forming of the glass.
RO is alkaline earth metal oxide and divalent metal oxide, the invention is characterized in that only MgO and ZnO are used in the glass composition, CaO is not contained, and Ca is used2+Radius (0.099nm) and Na+Very similar radii (0.095nm), and Ca2+Charge ratio Na+Twice as large as sodium ion, and its field strength is much larger than that of sodium ion, and can block Na during ion exchange+Na migration from the inside of the glass to the molten salt to cause chemical strengthening+The diffusion rate is significantly reduced and results in K+A reduction in ion exchange depth (DOL value); and Mg of MgO2+Zn of ZnO with ionic radius of only (0.068nm)2+The ionic radius is only (0.074nm), and the ionic radii of the two are all in proportion to Na+Has an ionic radius (0.095nm) much smallerCan not cause the obstruction of ion exchange during chemical strengthening, and can also participate in ion exchange, so that the ion exchange efficiency can be greatly improved, for example, the common ion exchange is K in high-temperature potassium nitrate dissolved salt+(r is 0.133nm) exchange of Na in the glass surface+(r-0.095 nm), large diameter K+Into the glass, while Na inside the glass+And the effluent enters potassium nitrate molten salt, and the ion exchange ratio is 1: 1. and in Mg2+And Zn2+Each Mg when participating in ion exchange and satisfying the charge balance condition2+Or Zn2+Coming out of the glass interior, there will be 2 Ks+Entering the glass, the ion exchange ratio is large 1: 2, so that MgO and ZnO in the glass composition are more advantageous for chemical strengthening. MgO is beneficial to improving the elastic modulus of the glass, and MgO and ZnO are beneficial to melting the glass, promoting the melting of the glass, reducing the high-temperature viscosity of the glass and enabling the glass to be T2 (10)2The corresponding temperature value of dPa.s, which is generally defined as the glass melting and refining temperature, and the temperature of T4 (which is the glass working point temperature and also serves as a feeding temperature reference point) are obviously reduced, so that the glass melting and preparing difficulty is reduced. In addition, ZnO is favorable for reducing the surface tension of glass, has a promoting effect on spreading and extending the glass melt, and is favorable for both ultrathin molding and ultrathin compression molding; ZnO has larger refractive index, and can endow the glass surface with better glossiness.
The clarifying agent of the invention is a composite clarifying agent and consists of SO3(supplied by anhydrous sodium sulphate) and CeO2The components are combined together; the surfactant is a bi-component composite surfactant composed of MoO3And Nb2O5And (4) forming. The clarifying agent and the surfactant promote the clarification of the glass and the reduction of the surface tension of the glass, improve the melting quality of the glass body, eliminate bubbles and stripes, facilitate the rapid extension of the press-formed glass and reduce the retraction of the glass melt.
Based on the effects of the components, the chemical composition of the mobile phone cover plate glass comprises the following components in percentage by mass:
wherein:
Li2O：Na2the mass ratio of O is 1: 3;
the sum of the mass percentages of ZnO and MgO is 4.3-7.4;
the molar ratio of O/(Si + B + P + Al) is 2.08-2.12, (R)2O+RO)/(B2O3+Al2O3) The molar ratio of (A) is 1.43-1.87.
The principle of the specific mixture ratio is as follows:
the molar ratio of O/(Si + B + P + Al) reflects the degree of compactness of the glass structure network, when the ratio is 2.0, the glass structure is the most compact and basically has three-dimensional network connection, and the ratio of the Bridge Oxygen (BO) reaches 100 percent and is completely based on the basic structural unit body [ FO ] of the glass4]The (F represents elements such as Si, Al, B, P and the like) tetrahedrons are connected with each other at the vertex, the glass with the mixture ratio is extremely infusible, and the forming difficulty is extremely high. When the above ratio is 2.5, the glass structure is changed from a three-dimensional network structure to a two-dimensional layered structure, the glass structure becomes very loose, all properties of the glass are deteriorated, the ratio of the Bridge Oxygen (BO) is only 75%, and the ratio of the non-bridge oxygen (NBO) is 25%, and the basic structural unit body of the glass [ FO ] is4](F represents Si, Al, B, P, etc.) tetrahedra are connected in a substantially planar manner, resulting in a glass which becomes well-melted, but has extremely poor molding characteristics and extremely poor physical and chemical properties.
The invention combines the glass network pores with proper size specification required in the chemical strengthening of the glass, and finds that when the ratio of O/(Si + B + P + Al) reaches 2.08-2.12, the glass structure can ensure proper tightness, maintain the three-dimensional connection of the glass network structure, maintain various physical and chemical properties of the glass, form four-membered rings, five-membered rings and six-membered rings in the glass network structure, create larger structural holes for Li+、Na+、K+、Mg2+、Zn2+And a space structure is created for glass to enter and exit.
(R2O+RO)/(B2O3+Al2O3) Molar ratio reflects network exosome (R)2O+RO，R2O is Li2O and Na2O; RO is MgO and ZnO) provides oxygen atoms for glass network formers and intermediatesAbility, if the ratio is greater than 1, will result in receptor (B)2O3、Al2O3) All transformed into tetrahedra of structural units of the glass network ([ BO)4]、[AlO4]) Excess oxygen atoms for the decomposition of SiO2The formed compact network reduces the viscosity of the glass, promotes the melting of the glass and reduces the forming viscosity of the glass. When the ratio is more than 1.4, the melting temperature, the feeding temperature and the softening temperature of the glass can be obviously reduced, and the delta T value is increased, so that the glass frit property is prolonged, and the one-step compression molding of the glass melt is facilitated, namely (R) of the invention2O+RO)/(B2O3+Al2O3) The molar ratio is 1.43-1.87.
As shown in fig. 4, the present invention provides a process method for a cover glass of a mobile phone, comprising:
step (1), melting the batch;
step (2), carrying out one-time compression molding to obtain a mobile phone cover plate glass blank; wherein:
the feeding temperature of the glass subjected to one-step compression molding is T4 temperature, the mold-entering temperature is T6 temperature, the softening point temperature of the glass is T7.6 temperature, and the mold-discharging temperature is T11 temperature;
in the process of one-time compression molding, the glass melt is contacted with the mold, and supercooling is formed on the surface of the glass melt, so that the surface structure of the glass is frozen, the surface structure is relatively loose, and favorable conditions are created for ion exchange.
Step (3), after trimming, punching and surface polishing, carrying out chemical strengthening treatment on the mobile phone cover plate glass blank to finally obtain the mobile phone cover plate glass; wherein:
the chemical strengthening treatment adopts a three-step strengthening process, wherein the first step and the third step are molten salt media, and the second step is an air medium; the heat treatment temperature is as follows: the temperature of the third step is more than or equal to that of the second step, and the heat treatment time is as follows: the first step time is more than or equal to the third step time.
The specific chemical strengthening treatment process comprises the following steps:
in the first step of molten salt treatment, the medium is composite molten salt, and the composition of the composite molten salt is 0-40wt% of NaNO3And 60wt% to 100wt% KNO3The heat treatment temperature is 370-410 ℃, and the treatment time is 1-3 h;
the second step of heating treatment, wherein the medium is air, the heat treatment temperature is 410-;
and step three, molten salt treatment is carried out, wherein the medium is 100 percent potassium nitrate molten salt, the heat treatment temperature is 420-.
The viscosity characteristic of the glass melted by the batch meets the requirement of a one-time compression molding process, the feeding temperature T4 is less than 1040 ℃, T7.6 is less than 709 ℃, and the mobile phone cover plate protective glass with the thickness of 0.6-1.1mm and the specification of less than 7 inches can be molded, and the form of the mobile phone cover plate protective glass is a 3D shape.
The embodiment is as follows:
the invention relates to a method and an instrument for testing physical and chemical process performance and chemical strength performance, which comprises the following steps:
the elastic modulus is measured by GB/T7962.6-2010 colorless optical glass test method part 6: young's modulus, shear modulus and Poisson's ratio;
the density measurement adopts GB/T7962.20-2010 colorless optical glass test method part 20: density (Density);
the average linear thermal expansion coefficient is measured by GB _ T16901-2015 determination of the average linear thermal expansion coefficient of glass;
the surface tension measurement refers to the foreign language published by tianying and the like, namely research on the surface tension of the glass melt under high temperature conditions, the collection of discourse of the Chinese society for measuring and testing, 2013, 9 months;
the dielectric constant is measured by adopting SJ/T11043 and 1996 'test method for high-frequency dielectric loss and dielectric constant of electronic glass';
t2 and T4 temperature measurement adopts SJ/T11040-;
the T7.6 temperature measurement adopts GB/T28195-2011 glass softening point test method;
the mold-in temperature T6 and the mold-out temperature T12 were calculated by fitting the Fulcher formula "New glass technology" P94.
The surface Compressive Stress (CS) measurement adopts a surface stress measuring instrument manufactured by Nippon discount original company, and the instrument model is FSM-6000 LE;
measuring depth of ion exchange layer (DOL) by using Electronic Probe (EPMA), grinding and polishing end face of ion exchanged glass, performing line scanning along cross section to obtain depth and concentration of related ions, and detecting K+。
The results of the measurement of the glass of the present invention by the above test method are shown in table 1, and GG3 of comparative example 1 is a third generation product of corning Gorilla glass, and GG5 of comparative example 2 is a fifth generation product of corning Gorilla glass.
TABLE 1
Note: "-" indicates that no relevant value is indicated in the product sample.
Compared with comparative examples 1 and 2, the elastic modulus of the invention is superior to that of the third generation and is similar to that of the fifth generation.
The dielectric constant closely related to the object of the present invention is only 6.35 to 6.43, which is 10 to 20% lower than that of 7.08 and 7.59 of comparative examples 1 and 2, and thus the 5G high frequency transmission signal loss can be well reduced. The glass melting temperature T2 of the invention is only 1481-1516 ℃, which is also obviously lower than the prior high-aluminum (Al)2O3Not less than 13 wt%) of cover glass, is more than 1600 deg.C, and is favorable for obtaining high-quality clarified homogenized glass, at the same time it is favourable for saving energy, and its working point temperature T4 is only 1007-1040 deg.C, and is lower than existent high-aluminium (Al) glass2O3Not less than 13 wt%) of cover plate glass 1180-1280 ℃, the glass softening point T7.6 temperature of the invention is only 691-709 ℃, the temperature is greatly reduced compared with 900 ℃ and 884 ℃ of comparative examples 1 and 2, the reduction range is more than 175 ℃, the mold-in temperature T6 is only 793-817 ℃ and the mold-out temperature T12 is 537-545 ℃, and the situation that the surface of the mold is subjected to one-step mold pressing of the cover plate protective glass can be reducedOxidation and loss, prolongs the service life of the die and improves the surface quality of the glass, and in addition, the surface tension of the glass in the compression molding temperature range is only 310 and 321mN/m, compared with the prior high-aluminum (Al)2O3Not less than 13 wt.%) and only 345-365mN/m, reducing by more than 10%, creating technological conditions for rapid extension of the compression-molded glass melt. After the glass is treated by the three-step strengthening process, the surface compressive stress CS of the glass is almost similar to that of comparative example 1 and comparative example 2, but the depth DOL of an ion exchange layer reaches 103-137 mu m, which is almost 100% higher than that of 50 mu m and 75 mu m of comparative example 1 and comparative example 2, and after the 3D mobile phone cover plate protective glass with the thickness of 0.7mm is assembled with a whole machine, the anti-falling height reaches 2 m, the glass can endure 20 falls, and the anti-falling damage of the glass is 1.6m higher than that of the comparative example.
The invention not only has remarkable advantages in the aspects of glass chemical composition, forming method and strengthening method, but also can solve the problem of thin edge of glass caused by hot bending forming through the mould, and effectively reduces the damage of the glass cover plate caused by falling of a mobile phone.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The mobile phone cover plate glass meeting the requirements of 5G communication and 3D compression molding is characterized in that the mobile phone cover plate glass is alkali aluminosilicate glass, and the chemical composition of the mobile phone cover plate glass comprises SiO2、B2O3、Al2O3Alkali metal oxide R2O and alkaline earth and divalent metal oxides RO;
the molar ratio of O/(Si + B + P + Al) is 2.08-2.12, (R)2O+RO)/（B2O3+Al2O3) The molar ratio of (A) is 1.43-1.87;
said R is2O is Li2O and Na2O, wherein the RO is MgO and ZnO;
the mobile phone cover plate glass comprises the following chemical components in percentage by mass:
SiO2 58-62
B2O35.2-6.4
Al2O3 13-17
Li2O 3.0-3.4
Na2O 9.0-10.2
MgO 2.8-3.2
ZnO 1.4-4.2；
the technological method of the mobile phone cover plate glass comprises the following steps:
step (1), melting batch;
step (2), carrying out one-time compression molding to obtain a mobile phone cover plate glass blank;
the glass obtained by one-step compression molding has the melting temperature of T2, the feeding temperature of T4, the mold-entering temperature of T6, the glass softening point temperature of T7.6, the mold-exiting temperature of T12, the melt surface tension of Be and the dielectric constant of Ɛ under the frequency condition of 54 MHz;
step (3), after trimming, punching and surface polishing are carried out on the mobile phone cover plate glass blank, chemical strengthening treatment is carried out to obtain mobile phone cover plate glass;
the melting temperature of T2 is less than 1516 ℃, the feeding temperature T4 is less than 1040 ℃, the mold entering temperature of T6 is less than 817 ℃, the glass softening point temperature of T7.6 is less than 709 ℃, the mold exit temperature of T12 is less than 545 ℃, the melt surface tension Be is less than 321mN/m, and the dielectric constant Ɛ is less than 6.43;
the chemical strengthening treatment adopts a three-step strengthening process, wherein the first step and the third step are molten salt media, and the second step is an air medium; the heat treatment temperature is as follows: the third step temperature is more than or equal to the second step temperature and more than or equal to the first step temperature, and the heat treatment time is as follows: the first step time is more than or equal to the third step time;
the chemical strengthening treatment comprises the following steps:
the first step of molten salt treatment, medium is composite molten salt, and the composition of the composite molten salt is 0-40wt% of NaNO3And 60wt% to 100wt% KNO3The heat treatment temperature is 370-;
the second step of heating treatment, wherein the medium is air, the heat treatment temperature is 410-;
and step three, molten salt treatment is carried out, wherein the medium is 100 percent potassium nitrate molten salt, the heat treatment temperature is 420-.
2. The cover glass for cellular phones according to claim 1, wherein Li is2O：Na2The mass ratio of O is 1: 3, the sum of the mass percentages of ZnO and MgO is 4.3-7.4.
3. The cover glass of claim 2, wherein the chemical composition of the cover glass further comprises: clarifying agents and surfactants;
the clarifying agent comprises the following components in percentage by mass:
SO3 0.2
CeO2 0.1
the surfactant comprises the following components in percentage by mass:
MoO3 0.05
Nb2O5 0.05。
4. the cover glass of claim 1, wherein the cover glass is in a 3D configuration having a thickness of 0.6-1.1mm and a gauge of less than 7 inches.
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| 印刷电路板用低介电铝硼硅酸盐玻璃结构与性能的研究;杜钊;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140815(第8期);B015-202 * |
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Effective date of registration: 20220708 Address after: 437099 No.1, henger Road, high tech Zone, Xianning City, Hubei Province Applicant after: XIANNING CSG PHOTOVOLTAIC GLASS CO.,LTD. Address before: Room 201, 213 building, Wangjing Garden East, Chaoyang District, Beijing 100102 Applicant before: Tian Yingliang |