CN103722816B - High-intensity ultra-thin glass and preparation method thereof - Google Patents
High-intensity ultra-thin glass and preparation method thereof Download PDFInfo
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- CN103722816B CN103722816B CN201310746974.XA CN201310746974A CN103722816B CN 103722816 B CN103722816 B CN 103722816B CN 201310746974 A CN201310746974 A CN 201310746974A CN 103722816 B CN103722816 B CN 103722816B
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- 239000011521 glass Substances 0.000 title claims abstract description 146
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 27
- 238000005728 strengthening Methods 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 238000007747 plating Methods 0.000 claims description 48
- 230000035882 stress Effects 0.000 claims description 19
- 230000035939 shock Effects 0.000 claims description 9
- 238000013007 heat curing Methods 0.000 claims description 6
- 230000008646 thermal stress Effects 0.000 claims description 6
- 238000009527 percussion Methods 0.000 claims description 4
- 238000001723 curing Methods 0.000 claims description 3
- 238000001771 vacuum deposition Methods 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000011247 coating layer Substances 0.000 abstract 4
- 238000012360 testing method Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- 239000005354 aluminosilicate glass Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a high-intensity ultra-thin glass and a preparation method thereof. The high-intensity ultra-thin glass comprises a glass matrix, wherein at least one coating layer with stress is adhered to the surface of the glass matrix, and an expansion coefficient of the coating layer is different from that of the glass matrix. With the adoption of the preparation method, by adopting a coating mode and utilizing the difference of the expansion coefficients of the coating layer and the glass matrix, the coating layer has a deformation relative to the glass matrix when forming a film on the surface of the glass matrix so as to form another uniformly distributed stress on the surface of the glass matrix, the stress can be used for strengthening the intensity of the glass again, also lowering the deformation quantity of the glass when the glass is impacted and carrying out effective supplementary for secondarily strengthening the intensity of the glass after strengthening.
Description
Technical field
The present invention relates to a kind of high strength slim glass, every field can be widely used in, refer in particular to be suitable for
Touch screen glass and protection glass in display surface.
Background technology
Glass material is increasingly being applied to electronic applications, and its superior case hardness and structural strength are glass materials
The typical characteristic of material, the design of electric terminal increasingly trends towards large scale and slimming, for the thin glass of this high intensity by a large number
Application.The feature of this glass maximum is exactly that initial strength is inadequate, it is necessary to use ion to exchange chemical enhanced method at salt bath ring
Border carries out ion exchange and toughness reinforcing increases intensity.But for the thickness ultra-thin glass less than 0.7mm, especially it is less than when thickness
During 0.5mm, exchanged by ion merely increase strength of glass can not make completely the intensity of glass reach design and make
With requiring.Such as: 1) when the thickness of glass is less than 0.7mm, even if glass is toughness reinforcing through ion exchange, its bending strength is with anti-
Impact strength still can not reach requirement；2) thickness is less than touch screen or the display screen protection glass of 0.7mm, exchanges through ion
After toughness reinforcing, even if the bending strength of glass and impact strength can reach enough intensity, but after being impacted, owing to depositing
At bigger deformation quantity, impulsive force can be transferred directly on display screen, causes display screen to rupture.Therefore, it is necessary to existing
Ultra-thin glass reinforcement technique makes innovation.
Summary of the invention
It is an object of the invention to provide a kind of high strength slim glass and preparation method thereof, ultra-thin to improve in prior art
The problem that strength of glass is the highest.
The technical solution adopted in the present invention is to provide a kind of high strength slim glass, and described glass includes glass basis,
The surface of described glass basis has the film plating layer of stress, the coefficient of expansion of described film plating layer and described glass with at least one of which
The coefficient of expansion of matrix is different.
The present invention also provides for the preparation method of a kind of high strength slim glass, comprises the following steps: under atmospheric environment,
Glass basis external coating has coating, by heat cure or ultra-violet curing coating, reduces temperature and has plating to room temperature, acquirement surface
The coated glass of film layer；Described coating has thermal stress；The coefficient of expansion of described film plating layer and the expansion system of described glass basis
Number difference.
The present invention also provides for the preparation method of another high strength slim glass, comprises the following steps: pass through Vacuum Deposition
The mode of film, in glass basis surface attachment coating, reduction temperature to room temperature, is opened vacuum and is obtained the surface plating with film plating layer
Film glass；Described coating has thermal stress；The coefficient of expansion of described film plating layer is different from the coefficient of expansion of described glass basis.
The beneficial effects of the present invention is: use plated film mode, utilize glass basis with film plating layer the coefficient of expansion not
With so that film plating layer is when glass basis surface filming, and film plating layer deformation occurs relative to glass basis, thus at glass basis table
Face forms other equally distributed stress, and this stress can promote strength of glass again, and reduces glass and rushed
Deformation quantity when hitting, again promotes for the intensity of glass after strengthening and is made that effective supplementing.
Detailed description of the invention
In order to make the technical problem to be solved, technical scheme and beneficial effect clearer, below tie
Close embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein is only in order to solve
Release the present invention, be not intended to limit the present invention.
The present invention provides a kind of high strength slim glass, and described glass includes glass basis, the surface of described glass basis
There is the coefficient of expansion of the film plating layer of stress, the coefficient of expansion of described film plating layer and described glass basis with at least one of which not
With.
Wherein, glass basis can be the glass arbitrarily needing to improve intensity, has the most carried out chemical ion exchange strengthening
After glass, strengthening glass with having the film plating layer of stress, promoting strength of glass further.Glass basis preferred thickness
Less than or equal to the glass of 0.7mm, the more preferably thickness glass less than or equal to 0.5mm.Can be with one layer or many on glass basis
Layer film plating layer, the comprehensive coefficient of expansion of one or more layers film plating layer is different from the coefficient of expansion of glass basis.Film plating layer is at glass
During matrix surface film forming, there is deformation in relative glass basis, forms other equally distributed stress on surface, improves glass
Intensity.
Further, film plating layer invests the shock surface (i.e. outer surface) of glass basis, has compressive stress.There is compressive stress
Film plating layer is under the conditions of 20 DEG C, and the comprehensive coefficient of linear thermal expansion of one or more layers film plating layer is less than 9 × 10-6/℃。
Further, film plating layer invests the non-percussion face (i.e. inner surface) of glass basis, has tensile stress.There is tensile stress
Film plating layer under the conditions of 20 DEG C, the comprehensive coefficient of linear thermal expansion of one or more layers film plating layer be more than 6 × 10-6/℃。
Described strength of glass height thickness ultrathin, is adapted to the trend of hyundai electronics end product designs, especially suitable
In needing bending strength and the higher touch screen of impact strength or display screen protection glass, have a wide range of applications.
The present invention also provides for the preparation method of a kind of high strength slim glass, comprises the following steps: under atmospheric environment,
Glass basis external coating has coating, by heat cure or ultra-violet curing coating, reduces temperature and has plating to room temperature, acquirement surface
The coated glass of film layer；Described coating has thermal stress；The coefficient of expansion of described film plating layer and the expansion system of described glass basis
Number difference.
Wherein, the mode of application is spraying, showering, roller coat, blade coating, spin coating or lifting.
The present invention also provides for the preparation method of another high strength slim glass, comprises the following steps: pass through Vacuum Deposition
The mode of film, in glass basis surface attachment coating, reduction temperature to room temperature, is opened vacuum and is obtained the surface plating with film plating layer
Film glass；Described coating has thermal stress；The coefficient of expansion of described film plating layer is different from the coefficient of expansion of described glass basis.
Further illustrate below in conjunction with design parameter.
Embodiment 1
Taking aluminum isopropylate. 50%, zirconium oxychloride 30%, ethanol 17%, nitric acid 3% through 48h, 25 DEG C of constant temperature 85-95 DEG C, 10h is ripe
Change, the mode of the slow lifting of use, first dipping 3-6s in coating liquid, after then lifting plated film with 8-9cm/min speed, the coolest
After dry 15min, in drying baker 80-100 DEG C of dry 30min, uniformly adhere to coating at glass basis shock surface, be passed through ammonia and urge
Change 20-120min, through 350-550 DEG C, 30-60min heat cure, slowly reduce the temperature (speed with 0.5 DEG C of average minute clock
Degree) to room temperature, obtain coated glass.Through measuring, the thickness of this film plating layer is 75nm, and comprehensive coefficient of linear thermal expansion is 5.4 × 10-6/℃。
Embodiment 2
Take butyl titanate 60%, ethanol 35%, hydrochloric acid 5% through 48h, 25 DEG C of constant temperature 85-95 DEG C, 10h ripening, use and carry slowly
The mode drawn, first impregnates 3-6s in coating liquid, after then lifting plated film with 8-9cm/min speed, after natural airing 15min,
In drying baker 80-100 DEG C of dry 30min, uniformly adhere to coating at glass basis shock surface, be passed through ammonia catalysis 20-
120min, through 350-550 DEG C, 30-60min heat cure, slowly reduces temperature (with the speed of 0.5 DEG C of average minute clock) to often
Temperature, obtains titanium oxide filming glass.Through measuring, the thickness of this silicon oxide film plating layer is 80nm, and comprehensive coefficient of linear thermal expansion is 2.8
×10-6/℃。
Embodiment 3
Take tetraethyl orthosilicate 50%, ethanol 49%, hydrochloric acid 1% through 48h, 25 DEG C of constant temperature 85-95 DEG C, 10h ripening, use slow
The mode of lifting, first impregnates 3-6s, after then lifting plated film with 8-9cm/min speed, natural airing 15min in coating liquid
After, in drying baker 80-100 DEG C of dry 30min, uniformly adhere to coating at glass basis shock surface, be passed through ammonia catalysis 20-
120min.Repeat above operation, plural layers can be adhered on matrix.Again through 350-550 DEG C, 30-60min heat cure, slow
Slowly temperature (with the speed of 0.5 DEG C of average minute clock) is reduced to room temperature, acquirement multilayer oxygen SiClx coated glass.Through measuring, this oxygen
The thickness of SiClx film plating layer is 150nm, and comprehensive coefficient of linear thermal expansion is 6.3 × 10-6/℃。
Embodiment 4 quantitative measurement
Test method: contrast common ultra-thin strengthening glass and high-strength with plated film by doing crooked test and shock-testing
Spend ultra-thin strengthening glass (sample glass in embodiment 3)；
Glass substrate: NEG CX-01TW overflow down draw aluminosilicate glass；
Glass size: 100*60*0.7mm；
Glass ion give-and-take conditions: 440 DEG C, 7 hours；
Coated glass specification: using the method in embodiment 3, glass surface carries out plated film after strengthening.
Glass surface stress and stress depth calibrator: FSM6000 surface stress instrument；
Strength of glass measuring instrument: Instron four-point bending measuring instrument (upper span: 30mm, lower span: 60mm)；
Shock-testing: falling ball impact test frame, 130g stainless steel ball starts freely falling body from 20cm, if glass is the most broken, raises
5cm impacts, until glass breaking；
The common ultra-thin strengthening glass strain of table 1 and break height test
Table 2 high strength slim strengthening glass strain and break height test
It is curved test and impact after taking high strength slim glass numbering obtained by common strengthening glass and the present invention, surveys
Test result, as above shown in Tables 1 and 2, compares and understands high strength slim glass mean break height provided by the present invention from 47.2cm
Bringing up to 79.4cm, reach as high as 90cm, impact resistance is obviously enhanced, and used coating film thickness is 150nm, and comprehensive line heat is swollen
Swollen coefficient is 6.3 × 10-6/ DEG C, owing to there is coefficient of expansion difference extra compressive stress of superposition on the shock surface of glass, for from
The intensity of the glass after son exchange again promotes and is made that effective supplementing, and its bending strength and impact strength are enough satisfied to be set
Meter and use requirement, after being impacted, deformation quantity is less, beneficially product protection.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (6)
1. a high strength slim glass, it is characterised in that described glass includes glass basis, and the surface of described glass basis is attached
Having at least one of which to have the film plating layer of stress, the coefficient of expansion of described film plating layer is different from the coefficient of expansion of described glass basis；
Film plating layer on the shock surface of described glass basis comprehensive coefficient of linear thermal expansion in the case of 20 degrees Celsius is less than 9 × 10-6/
℃；Film plating layer on the non-percussion face of described glass basis in the case of 20 degrees Celsius comprehensive coefficient of linear thermal expansion more than 6 ×
10-6/℃；
Described glass basis is the glass after strengthening；The thickness of described glass basis is less than or equal to 0.5 millimeter；Described film plating layer exists
Relative to glass basis, deformation occurs during glass body surface film forming.
High strength slim glass the most according to claim 1, it is characterised in that described film plating layer invests rushing of glass basis
Hit face, and the stress that described film plating layer is had is compressive stress.
High strength slim glass the most according to claim 1, it is characterised in that described film plating layer invests the non-of glass basis
Shock surface, and the stress that described film plating layer is had is tensile stress.
4. the preparation method of a high strength slim glass, it is characterised in that comprise the following steps: under atmospheric environment, at glass
Glass matrix surface is coated with coating, by heat cure or ultra-violet curing coating, reduces temperature and has plated film to room temperature, acquirement surface
The coated glass of layer；Described coating has thermal stress；The coefficient of expansion of described film plating layer and the coefficient of expansion of described glass basis
Different；Described glass basis is the glass after strengthening；The thickness of described glass basis is less than or equal to 0.5 millimeter；Described film plating layer
Relative to glass basis, deformation occurs when glass body surface film forming；Film plating layer on the shock surface of described glass basis is taken the photograph 20
In the case of family name's degree, comprehensive coefficient of linear thermal expansion is less than 9 × 10-6/℃；Film plating layer on the non-percussion face of described glass basis exists
In the case of 20 degrees Celsius, comprehensive coefficient of linear thermal expansion is more than 6 × 10-6/℃。
Preparation method the most according to claim 4, it is characterised in that the mode of described application be spraying, showering, roller coat,
Blade coating, spin coating or lifting.
6. the preparation method of a high strength slim glass, it is characterised in that comprise the following steps: by the way of vacuum coating
In glass basis surface attachment coating, reduction temperature to room temperature, open vacuum and obtain the surface coated glass with film plating layer；Institute
State coating and there is thermal stress；The coefficient of expansion of described film plating layer is different from the coefficient of expansion of described glass basis；Described glass base
Body is the glass after strengthening；The thickness of described glass basis is less than or equal to 0.5 millimeter；Described film plating layer becomes at glass body surface
Relative to glass basis, deformation occurs during film；Film plating layer on the shock surface of described glass basis is comprehensive in the case of 20 degrees Celsius
Coefficient of linear thermal expansion is less than 9 × 10-6/℃；Film plating layer on the non-percussion face of described glass basis is in the case of 20 degrees Celsius
Comprehensive coefficient of linear thermal expansion is more than 6 × 10-6/℃。
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| CN201310746974.XA CN103722816B (en) | 2013-12-30 | 2013-12-30 | High-intensity ultra-thin glass and preparation method thereof |
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| CN201310746974.XA CN103722816B (en) | 2013-12-30 | 2013-12-30 | High-intensity ultra-thin glass and preparation method thereof |
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| CN103722816A CN103722816A (en) | 2014-04-16 |
| CN103722816B true CN103722816B (en) | 2017-01-11 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948536B (en) * | 2016-06-16 | 2019-02-26 | 深圳市东丽华科技有限公司 | Single strengthening layer glass and preparation method thereof |
| CN107117809A (en) * | 2017-06-29 | 2017-09-01 | 合肥达户电线电缆科技有限公司 | A kind of monitoring device cover plate |
| CN110372216B (en) * | 2018-04-12 | 2022-05-03 | 重庆鑫景特种玻璃有限公司 | Plane glass, toughened glass, 3D curved surface microcrystalline glass and preparation process thereof |
| CN108751733B (en) * | 2018-05-31 | 2020-02-21 | 厦门大学 | Silica sol reinforced hollow safety glass and preparation method thereof |
| CN115477478A (en) * | 2022-09-23 | 2022-12-16 | 新福兴玻璃工业集团有限公司 | Solar control coated glass and online preparation method thereof |
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| CN101209904A (en) * | 2006-12-26 | 2008-07-02 | 比亚迪股份有限公司 | Plated film glass |
| CN102584027A (en) * | 2012-01-09 | 2012-07-18 | 宁波永新光学股份有限公司 | Method for plating antireflection film on surface of optical glass tempered by chemical method |
| CN103232171A (en) * | 2013-03-29 | 2013-08-07 | 中国建筑材料科学研究总院 | Glass cover plate for touch screens and preparation method thereof |
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| CN101209904A (en) * | 2006-12-26 | 2008-07-02 | 比亚迪股份有限公司 | Plated film glass |
| CN102584027A (en) * | 2012-01-09 | 2012-07-18 | 宁波永新光学股份有限公司 | Method for plating antireflection film on surface of optical glass tempered by chemical method |
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