CN106830675A - A kind of glass composition, alkali silicate glass and its preparation method and application - Google Patents
A kind of glass composition, alkali silicate glass and its preparation method and application Download PDFInfo
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- CN106830675A CN106830675A CN201710059984.4A CN201710059984A CN106830675A CN 106830675 A CN106830675 A CN 106830675A CN 201710059984 A CN201710059984 A CN 201710059984A CN 106830675 A CN106830675 A CN 106830675A
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- chemical intensification
- oxide
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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
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
-
- 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
- C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
- C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
Abstract
The present invention relates to glass art, a kind of glass composition, alkali silicate glass and its preparation method and application are disclosed, on the basis of the weight of said composition, in terms of oxide, said composition contains the SiO of 40 80wt%2+B2O3+P2O5, 3 25wt% Al2O3, 10 25wt% Li2O+Na2O+K2The RE of O, the MgO+CaO+SrO+BaO of 0 15wt%, the ZnO of 0 5wt% and 0 5wt%2O3, wherein, said composition contains B2O3And P2O5In at least one, and contain ZnO and RE2O3In at least one.Alkali silicate glass of the invention has low fragility, good intensity and toughness concurrently.
Description
Technical field
The present invention relates to glass art, in particular it relates to a kind of glass composition, alkali silicate glass and its preparation side
Method and application.
Background technology
In field of liquid crystal display, backlight source module mainly has straight-down negative, side-light type etc..In the sidelight type backlight module of main flow
In, it is necessary to light guide plate is used as equal electro-optical device, its total reflection for utilizing light and scattering principle, in light guide plate top or bottom with optics
The many circular or square diffusion site (or very low power) of structure design, when light is mapped to diffusion point, using various densitys, greatly
The part total reflection light path of small different diffusion point destruction light and the interference of light, by CCFL line source or LED points
Light source is imported and is evenly distributed in light guide plate plane from light guide plate side, light is reflected to frontal planar, is formed
Towards the light source for projecting.As narrow frame and ultra-thin Display Technique develop, the main material-methyl methacrylate of original light guide plate
Ester (PMMA) due to that the problems such as the coefficient of expansion is excessive, heat-resistant stability is not high, cannot meet requirement.Glass material can be as
Another preferred material, but glass material exist fragility it is excessive, it is not flexible the shortcomings of, be unfavorable for curved-surface display device
Use.
In plane display field, screen products market development is touched recent years rapidly, current main product is condenser type
Touch-screen, its critical piece is the glass substrate that surface shields.With the development of Display Technique and touch technology, market
Requirement for glass substrate is increasingly improved.Because touch-screen applications are more and more extensive, the equipment of big-and-middle small size nearly all has
Have touch-screen, so the main performance of touch-screen is that to possess relatively low fragility and larger fracture toughness, and this performance be by
What the intensity of glass was embodied, so the intensity for improving glass itself is crucial.Strength of glass in addition to being influenceed by tempering,
The material side's composition of itself plays the decisive action of key.The cover sheet glass of main flow uses common sodium-calcium-silicate body on the market
System or high-alkali high alumina silicate systems carry out chemical tempering and reach enhanced purpose, and the cover-plate glass of newer type is using colourless blue precious
Stone is cut into slices as cover sheet.But there is larger defect in above-mentioned system.Therefore, either curved-surface display device or plane
Display device, in material side, aspect reduction fragility, raising toughness are one of important topics.
The content of the invention
The invention aims to overcome drawbacks described above of the prior art, there is provided a kind of glass composition, alkali silicon
Silicate glass and its preparation method and application, alkali silicate glass of the invention has low fragility, good intensity and toughness concurrently.
To achieve these goals, in a first aspect, the invention provides a kind of glass composition, with the weight of said composition
On the basis of amount, in terms of oxide, said composition contains the SiO of 40-80wt%2+B2O3+P2O5, 3-25wt% Al2O3、10-
The Li of 25wt%2O+Na2O+K2The RE of the ZnO and 0-5wt% of MgO+CaO+SrO+BaO, 0-5wt% of O, 0-15wt%2O3, its
In, said composition contains B2O3And P2O5In at least one, and contain ZnO and RE2O3In at least one.
Preferably, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 0-30wt%；
It is further preferred that on the basis of the weight of said composition, in terms of oxide, B2O3Content be 1-10wt%；
It is further preferred that on the basis of the weight of said composition, in terms of oxide, B2O3Content be 15-25wt%.
Preferably, on the basis of the weight of said composition, in terms of oxide, P2O5Content be 0-20wt%, further it is excellent
Elect 4-16wt% as.
Preferably, on the basis of the weight of said composition, in terms of oxide, SiO2Content be 40-75wt%.
Preferably, on the basis of the weight of said composition, in terms of oxide, the content of ZnO is 0.2-5wt%, further
Preferably 0.5-4wt%.
Preferably, on the basis of the weight of said composition, in terms of oxide, RE2O3Content be 0.01-5wt%, enter one
Step is preferably 0.3-3wt%；
It is further preferred that RE2O3It is rare earth oxide Y2O3、La2O3、Gd2O3、Ce2O3、Yb2O3And Lu2O3In extremely
Few one kind, and by weight percentage, Y2O3+La2O3>0wt%.
Preferably, by weight percentage, 0.6<Na2O/(Li2O+Na2O+K2O)<1。
Preferably, on the basis of the weight of said composition, in terms of oxide, the content of MgO is 1-6wt%.
Preferably, the composition also contains fining agent, and the fining agent is more preferably sulfate, nitrate, oxygen
Change at least one in tin, stannous oxide, chloride and fluoride；On the basis of the weight of said composition, the content of fining agent
No more than 1wt%.
Second aspect, the invention provides a kind of method for preparing alkali silicate glass, the method is included institute of the present invention
The glass stated carries out melt process, forming processes, annealing and machining processes successively with composition.
Preferably, the method also includes that the product obtained to machining processes carries out chemical intensification treatment, further excellent
Selection of land, the chemical intensification treatment is a chemical intensification treatment or secondary chemical intensification treatment.
Preferably, the method also includes：Before chemical intensification treatment, the product obtained to machining processes carries out two
Thin treatment is drawn in secondary melting.
Preferably, the machining processes or second melting is controlled to draw the condition of thin treatment to be less than to prepare thickness
The glass of 0.1mm.
The product that machining processes preferably for thickness more than 0.1mm are obtained, carries out a chemical intensification treatment
Or secondary chemical intensification treatment.
The product that machining processes preferably for thickness more than 0.3mm are obtained, carries out secondary chemical enhanced place
Reason.
The product that machining processes preferably for thickness less than 0.1mm are obtained, carries out once chemical enhanced place
Reason.
The third aspect, the invention provides the alkali silicate glass that the above method is prepared.
Preferably, the elastic modelling quantity of the alkali silicate glass is higher than 60GPa, and density is less than 2.7g/cm3, 50-350 DEG C
In the range of thermal coefficient of expansion be less than 90 × 10-7/ DEG C, strain point temperature is higher than 550 DEG C, refractive index nDLess than 1.55,550nm ripples
The corresponding transmitance of length is more than 92%.
Preferably, the fracture toughness K of the glass for being obtained before the chemical intensification treatmentICMore than 1.0MPam1/2。
Preferably, the fracture toughness K of the glass that the chemical intensification treatment is obtainedICMore than 2MPam1/2, further preferably
More than 5MPam1/2, still more preferably more than 8MPam1/2。
Preferably, when thickness is more than 0.1mm, the compression stress that the glass surface obtained through chemical intensification treatment is formed
More than 600MPa, further preferably greater than 650MPa；Compression stress layer depth is more than 30 μm, further preferably greater than 35 μm.
Preferably, when thickness is more than 0.1mm, further preferably greater than 0.3mm, through the glass that secondary chemical intensification treatment is obtained
The compression stress that glass surface is formed is more than 600MPa, further preferably greater than 650MPa；Compression stress layer depth is more than 60 μm, enters
One step is preferably greater than 80 μm.
Preferably, when thickness is less than 0.1mm, the compression stress that the glass surface obtained through chemical intensification treatment is formed
More than 200MPa, further preferably greater than 300MPa；Compression stress layer depth is more than 5 μm, further preferably greater than 15 μm.
Preferably, when thickness is less than 0.1mm, the minimum bending radius of the glass obtained through chemical intensification treatment is less than
35mm, is further preferably no larger than 30mm.
Fourth aspect, display is being prepared the invention provides glass composition of the present invention or alkali silicate glass
Application in device and/or solar cell, it is guide-lighting preferably in plane or flexible liquid crystal display part backlight module is prepared
The screen surface protection glass material of plate material, flat board or Flexible Displays product, the substrate glass substrate of Flexible Displays product
The cover-plate glass of the substrate glass material, plane and/or flexible solar battery of material, plane and/or flexible solar battery
Answering in material, safety glass, bulletproof glass, intelligent automobile glass, intelligent transportation display screen, intelligent show window and smart card ticket
With.
Glass composition of the invention, is a kind of frit side for strengthening effect with good chemical, belongs to alkali silicic acid
Salt glass system, it is adaptable to which the various Conventional glassmaking methods such as float glass process, press over system, rolling process, glass tube down-drawing are used to produce thickness>
The plate glass or thickness of 0.1mm<(i.e. once moulding method obtains thickness to the flexible glass of 0.1mm<The flexible glass of 0.1mm),
Or thin method is drawn for producing thickness suitable for second melting<The flexible glass of 0.1mm.The glass that the present invention is prepared
Glass, has good intensity and toughness concurrently, is appropriate for large-scale industrial production.
A preferred embodiment of the invention, the SiO containing certain content in glass composition2、B2O3、
P2O5、Al2O3、Li2O、Na2O、K2O, MgO, CaO, SrO, BaO, ZnO and RE2O3, prepared using this glass composition
Glass, elastic modelling quantity is higher than 60GPa, and density is less than 2.7g/cm3, the thermal coefficient of expansion in the range of 50-350 DEG C is less than 90 × 10-7/ DEG C, strain point temperature is higher than 550 DEG C, refractive index nDTransmitance corresponding less than 1.55,550nm wavelength is more than 92%；Wherein,
(correspond to machining processes or second melting draws the thin glass for processing and obtaining) before chemical intensification treatment, the fracture of glass is tough
Property KICMore than 1.0MPam1/2, the fracture toughness K of the glass that chemical intensification treatment is obtainedICMore than 2MPam1/2(preferably greater than
5MPa·m1/2, further preferably greater than 8MPam1/2)。
In preceding preferred embodiment, it is preferable that when thickness is more than 0.1mm, the glass obtained through chemical intensification treatment
The compression stress that glass surface is formed is more than 600MPa, further preferably greater than 650MPa；Compression stress layer depth is more than 30 μm, enters
One step is preferably greater than 35 μm.
In preceding preferred embodiment, it is preferable that when thickness is more than 0.1mm, further preferably greater than 0.3mm, through secondary
The compression stress that the glass surface that chemical intensification treatment is obtained is formed is more than 600MPa, further preferably greater than 650MPa；Compression
Stress layer depth is more than 60 μm, further preferably greater than 80 μm.
In preceding preferred embodiment, it is preferable that when thickness is less than 0.1mm, the glass obtained through chemical intensification treatment
The compression stress that glass surface is formed is more than 200MPa, further preferably greater than 300MPa；Compression stress layer depth is more than 5 μm, enters
One step is preferably greater than 15 μm.Preferably, when thickness is less than 0.1mm, the glass obtained through chemical intensification treatment it is minimum curved
Bilge radius are less than 35mm, are further preferably no larger than 30mm.
Glass composition of the invention or alkali silicate glass can be used to prepare display device and/or solar cell,
Screen particularly for preparing light guide panel material, flat board or Flexible Displays product in plane or flexible liquid crystal display part backlight module
Curtain surface protection glass material, the substrate glass substrate material of Flexible Displays product, plane and/or flexible solar battery
The cover-plate glass material of substrate glass material, plane and/or flexible solar battery, safety glass, bulletproof glass, intelligent automobile
Glass, intelligent transportation display screen, intelligent show window, smart card ticket and the neck of low fragility high tenacity glass material is needed for other
Domain.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific embodiment
Specific embodiment of the invention is described in detail below.It should be appreciated that described herein specific
Implementation method is merely to illustrate and explain the present invention, and is not intended to limit the invention.
In a first aspect, the invention provides a kind of glass composition, on the basis of the weight of said composition, with oxide
Meter, said composition contains the SiO of 40-80wt%2+B2O3+P2O5, 3-25wt% Al2O3, 10-25wt% Li2O+Na2O+
K2The RE of the ZnO and 0-5wt% of MgO+CaO+SrO+BaO, 0-5wt% of O, 0-15wt%2O3, wherein, said composition contains
B2O3And P2O5In at least one, and contain ZnO and RE2O3In at least one.
It will be understood by those skilled in the art that in glass composition of the invention, " said composition contains B2O3With
P2O5In at least one, and contain ZnO and RE2O3In at least one " refer to said composition except containing foregoing certain content
Component outside, also contain B2O3And/or P2O5And contain ZnO and/or RE2O3, i.e. B2O3And P2O5Content it is different when be 0,
And ZnO and RE2O3Content it is different when be 0.
In glass composition of the invention, SiO2Used as the matrix for constituting network structure, its addition can improve glass
Heat resistance and chemical durability, and glass is difficult devitrification, it is also helpful for During Vitrification in vitro.But excessive SiO2Can make
Obtain melt temperature to raise, fragility increases, excessive demand is proposed to production technology.The present inventor further sends out under study for action
It is existing, by percentage to the quality, SiO2Content >=40wt% when, can further improve the mechanicalness of the glass for preparing
Energy, resistance to chemical corrosion.Therefore, in order to further improve the combination property of the glass for preparing and reduce fragility, preferably
In the case of, on the basis of the weight of said composition, in terms of oxide, SiO2Content be 40-75wt%.
In glass composition of the invention, B2O3、P2O5As the matrix for constituting alkali silicate glass, can be individually created
Glass, its addition can reduce the fragility of glass, while B2O3、P2O5It is also good cosolvent, glass melting temperature can be greatly reduced
Degree, it is also helpful for During Vitrification in vitro.But excessive B2O3、P2O5The reduction of glass low-temperature viscosity can be caused.Therefore, it is comprehensive
Consider, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 0-30wt%.The present inventor is grinding
It has furthermore been found that by percentage to the quality in studying carefully, B2O3Content be 1-10wt% when, can further improve what is prepared
The chemical enhanced effect of glass, raising compression.Therefore, in order to further improve the glass for preparing combination property and
Chemical enhanced effect, under preferable case, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 1-
10wt%；Wherein, the present inventor has further been found that by percentage to the quality under study for action, B2O3Content be 15-
During 25wt%, the toughness of the glass for preparing can be further improved.Therefore, in order to further improve the glass for preparing
Combination property and toughness, under preferable case, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 15-
25wt%.
Under preferable case, on the basis of the weight of said composition, in terms of oxide, P2O5Content be 0-20wt%, enter one
Step is preferably 4-16wt%.Wherein, SiO need to be met2+B2O3+P2O5Content be 40-80wt%.
In glass composition of the invention, Al2O3Addition can accelerate the process and depth of ion exchange, but it is striven
Take the very capable of free oxygen by force, largely introduce Al2O3The degree of opening of glass structure can be reduced, glass is tended to rigidity, increase glass
The fragility of glass, at the same the easy devitrification of glass, thermal coefficient of expansion can be caused to reduce and be difficult to be matched with periphery material, high temperature surface tension
And high temperature viscosity is excessive, process of glass difficulty etc. is increased.Consider, on the basis of the weight of said composition, to aoxidize
Thing meter, Al2O3Content be 3-25wt%, preferably 5-24wt%.
In glass composition of the invention, Li2O、Na2O and K2O be all make high temperature viscometrics reduction, improve meltbility into
Point, appropriate its content of increase can be effectively reduced the high temperature viscosity of glass, so as to improve meltbility and formability, and can improve
Devitrification.However, its too high levels can increase the thermal expansion of glass and reduce the chemical durability of glass, and too high levels have on the contrary
The tendency that increased devitrification resistance deteriorates, therefore, consider, on the basis of the weight of said composition, in terms of oxide, 10wt%≤Li2O
+Na2O+K2O≤25wt% (Li2O+Na2O+K2O refers to contain Li2O、Na2O and K2At least one in O).Preferably, 0.6<
Na2O/(Li2O+Na2O+K2O)<1。
In glass composition of the invention, MgO, CaO, SrO, BaO belong to alkaline earth oxide, their addition
The high temperature viscosity of glass can effectively be reduced so as to improve the meltbility and formability of glass, and strain point and the poplar of glass can be improved
Family name's modulus；But its content excessively can increase density, crackle, devitrification, the incidence of split-phase are improved.Therefore, consider, with
On the basis of the weight of said composition, in terms of oxide, the alkaline earth oxide RO containing 0-15wt%, wherein RO=MgO,
Any one or more in CaO, SrO and BaO.Preferably, on the basis of the weight of said composition, in terms of oxide, MgO's
Content is 1-6wt%.
In glass composition of the invention, bivalent metal oxide according to it in the periodic table of elements status with to property
Influence is different, can be divided into two classes：One class is the alkaline earth oxide for being located at main group, its ion R2+With 8 exoelectron knots
Structure；Equations of The Second Kind is located at periodic table subgroup (such as ZnO, CdO), its ion R2+With 18 outer electronic structures, in glass two
The configuration state of person from glass property influence be different.Relative to alkaline-earth metal, the Zn with 18 electronics layer structures2+From
Son is easier to be polarized, and glass viscosity (such as 1450 DEG C) can be reduced under high temperature, is conducive to eliminating bubble；When total alkali content and network
When intermediate oxide molecular proportion is more than 1, after introducing glass as network outer body, Zn2+Tend to form tetrahedron with four-coordination
[ZnO4] exist, compared with [ZnO6] glass structure is more loose, is under the identical condition of high temperature with the glass without ZnO and compared, contain
The glass viscosity of ZnO is smaller, and atomic motion speed is bigger, it is impossible to forms nucleus, it is necessary to further reduce temperature, is just conducive to crystalline substance
The formation of core, thus, reduce the crystallization ceiling temperature of glass；There are lifting intensity, hardness below softening point, increase glass
Chemical resistance, reduces fragility value, reduces the effect of thermal expansion coefficient of glass.ZnO content can excessively make the strain point of glass significantly
Degree is reduced.Therefore, consider, under preferable case, on the basis of the weight of said composition, in terms of oxide, the content of ZnO is
0.2-5wt%, more preferably 0.5-4wt%.
In glass composition of the invention, rare earth oxide RE2O3Often have in some aspect of performances for improving glass
The performances such as unique ability, bending strength, elastic modelling quantity, the strain point of such as glass significantly go up with the addition of rare earth oxide
Rise, promote the reduction of glass fragility, fracture toughness is significantly increased.After the network outer bodies such as alkaline-earth metal, ZnO introduce glass composition, mistake
Surplus oxygen atom causes that the bridge oxygen bond rupture in glass structure generates non-bridging oxygen, and the presence of these non-bridging oxygens significantly reduces glass
Bending strength.RE2O3Addition promote the internal structure of glass to change, the Si-O-RE chemical bonds for being generated are by glass
Isolated island NE is reconnected, and improves the network structure of glass, such that it is able to greatly improve glass bending strength,
The performances such as elastic modelling quantity, strain point, RE is increased when further2O3When, because the non-bridging oxygen quantity for being available for adjustment is reduced, therefore glass
The above-mentioned performance change of glass is little.Therefore, consider, under preferable case, on the basis of the weight of said composition, with oxide
Meter, RE2O3Content be 0.01-5wt%, more preferably 0.3-3wt%.From absorption spectrum etc., other performance synthesises consider,
Present invention introduces RE2O3It is rare earth oxide Y2O3、La2O3、Gd2O3、Ce2O3、Yb2O3And Lu2O3In at least one, and with
Percentage by weight meter, Y2O3+La2O3>0wt%.
In glass composition of the invention, according to the difference of glass preparation technique, composition can also contain as glass
Fining agent when glass is melted, the fining agent is preferably sulfate, nitrate, tin oxide, stannous oxide, chloride and fluoride
In at least one；On the basis of the weight of said composition, the content of fining agent is not more than 1wt%.It is specific for fining agent
There is no particular limitation for selection, can be various selections commonly used in the art, and such as sulfate can be sodium sulphate, and nitrate can
Think sodium nitrate and/or potassium nitrate, chloride can be sodium chloride and/or strontium chloride, and fluoride can be calcirm-fluoride.
It will be understood by those skilled in the art that in glass composition of the invention, composition contains SiO2、B2O3、
P2O5、Al2O3、Li2O、Na2O、K2O, MgO, CaO, SrO, BaO, ZnO and RE2O3Refer to that said composition contains compound containing Si, contains
B compounds, containing P-compound, compound containing Al, compound containing Li, compound containing Na, compound containing K, compound containing Mg, containing Ca
Compound, compound containing Sr, compound containing Ba, compound containing Zn and compound containing RE, such as carbonate, nitre containing foregoing each element
Hydrochlorate, sulfate, phosphate, subcarbonate, oxide etc., and the foregoing each component for referring to content with the oxygen of each element
Compound meter, the carbonate of specific each element, nitrate, sulfate, phosphate, subcarbonate, the selection of oxide are this
Known to art personnel, will not be repeated here.
In glass composition of the invention, when preparing alkali silicate glass using it, glass why is enabled to have
There is excellent combination property, be mainly attributed to the mutual cooperation between each component, especially SiO in composition2、B2O3、P2O5、
Al2O3、Li2O、Na2O、K2O, MgO, CaO, SrO, BaO, ZnO and RE2O3Between mating reaction, it is more particularly foregoing specific to contain
Mutual cooperation between each component of amount, particularly limits the B of content and ratio2O3And/or P2O5And ZnO and/or RE2O3's
Introduce, the effective toughness for improving glass.
Second aspect, the invention provides a kind of alkali silicate glass, on the basis of the weight of the glass, the glass contains
There is the SiO of 40-80wt%2+B2O3+P2O5, 3-25wt% Al2O3, 10-25wt% Li2O+Na2O+K2O, 0-15wt%'s
The RE of the ZnO and 0-5wt% of MgO+CaO+SrO+BaO, 0-5wt%2O3, wherein, the glass contains B2O3And P2O5In at least
One kind, and contain ZnO and RE2O3In at least one.
Preferably, in alkali silicate glass, on the basis of the weight of glass, B2O3Content be 0-30wt%；
It is further preferred that on the basis of the weight of glass, B2O3Content be 1-10wt%；
It is further preferred that on the basis of the weight of glass, B2O3Content be 15-25wt%.
Preferably, in alkali silicate glass, on the basis of the weight of glass, P2O5Content be 0-20wt%, further it is excellent
Elect 4-16wt% as.
Preferably, in alkali silicate glass, on the basis of the weight of glass, SiO2Content be 40-75wt%.
Preferably, in alkali silicate glass, on the basis of the weight of glass, the content of ZnO is 0.2-5wt%, further
Preferably 0.5-4wt%.
Preferably, in alkali silicate glass, on the basis of the weight of glass, RE2O3Content be 0.01-5wt%, enter one
Step is preferably 0.3-3wt%；It is further preferred that RE2O3It is rare earth oxide Y2O3、La2O3、Gd2O3、Ce2O3、Yb2O3With
Lu2O3In at least one, and by weight percentage, Y2O3+La2O3>0wt%.
Preferably, in alkali silicate glass, on the basis of the weight of glass, 0.6<Na2O/(Li2O+Na2O+K2O)<1。
Preferably, in alkali silicate glass, on the basis of the weight of glass, the content of MgO is 1-6wt%.
Preferably, in alkali silicate glass, on the basis of the weight of glass, clarification agent content is not more than 1wt%, preferably
Ground, fining agent is preferably at least one in sulfate, nitrate, tin oxide, stannous oxide, chloride and fluoride.
The third aspect, the invention provides a kind of method for preparing alkali silicate glass, the method is included institute of the present invention
The glass stated carries out melt process, forming processes, annealing and machining processes successively with composition.
In the method for the present invention, foregoing corresponding contents description is referred to for the specific restriction of glass composition, herein
Repeat no more.
Process of the present invention it is preferred in the case of, the condition of melt process includes：Temperature is less than 1600 DEG C, and the time is more than
1h.Those skilled in the art can determine specific melt temperature and melting time according to actual conditions, and this is art technology
Known to personnel, will not be repeated here.
Process of the present invention it is preferred in the case of, the condition of annealing includes：Temperature is higher than 550 DEG C, further preferably
Higher than 580 DEG C, the time is more than 0.1h.Those skilled in the art can determine specific annealing temperature and annealing according to actual conditions
Time, this is well known to those skilled in the art, and will not be repeated here.
In the method for the present invention, for machining processes, there is no particular limitation, can be common various in this area
Machining mode, for example, can be that will make annealing treatment the product for obtaining to be cut, ground, polished.
In order to further improve the combination property of glass, under preferable case, the method also includes obtaining machining processes
To product carry out chemical intensification treatment.It is further preferred that the chemical intensification treatment is a chemical intensification treatment or two
Secondary chemical intensification treatment is (wherein, it will be understood by those skilled in the art that secondary chemical intensification treatment refers to be changed twice
Learn intensive treatment).
In the method for the present invention, can produce thick by the various Conventional glassmaking methods such as float glass process, press over system, glass tube down-drawing
Plate glass or thickness of the degree more than 0.1mm<The flexible glass (corresponding to once moulding method) of 0.1mm, it is also possible to by secondary
Thin method flexible glass of the production thickness less than 0.1mm is drawn in melting.Wherein it is possible to directly be more than the flat board of 0.1mm to thickness
Glass carries out chemical intensification treatment, it is also possible to thickness<The flexible glass of 0.1mm carries out chemical intensification treatment.Specifically, for
Thickness<The chemical intensification treatment of the flexible glass of 0.1mm, if being that can obtain thickness by one-shot forming<The flexible glass of 0.1mm
When, can directly carry out chemical intensification treatment.If being not less than 0.1mm by the thickness of glass that one-shot forming is obtained, the method is also
Before chemical intensification treatment being included in, the product obtained to machining processes carries out second melting and draws thin treatment, by glass
Glass thickness draws and is as thin as, less than 0.1mm, then carrying out chemical intensification treatment.Under preferable case, control the machining processes or
Person's second melting draws the condition of thin treatment to prepare glass of the thickness less than 0.1mm, i.e. machining processes or second melting
The thickness of the glass that thin treatment (i.e. before chemical intensification treatment) obtains is drawn to be less than 0.1mm.For the tool that second melting draws thin treatment
There is no particular limitation for body method, can be various methods commonly used in the art, for example, the condition of the thin treatment of second melting drawing can
To include：Plate glass of the thickness less than 1mm is produced by glass-making processes such as float glass process, press over system, glass tube down-drawings, by flat board glass
Glass is transported to succeeding stretch shaped device inlet, with appropriate speed V0Mm/min is inwardly sent into drawing and forming stove, control
Drawing and forming region viscosity is about 105.5-107With appropriate speed V in the range of pool, by stretching-machine and roller1Mm/min is carried out
Volume to volume winds, so as to obtain ultrathin flexible glass board material of the thickness less than 0.1mm, the pull speed V1More than V0。
Wherein, the object of chemical intensification treatment can be that machining processes or second melting draw the thin product for processing and obtaining
Thing.The mode of chemical intensification treatment can be selected as the case may be, it is preferable that the machinery for thickness more than 0.1mm
The product that working process is obtained, carries out a chemical intensification treatment or secondary chemical intensification treatment；It is more than 0.3mm's for thickness
The product that machining processes are obtained, carries out secondary chemical intensification treatment；Machining processes for thickness less than 0.1mm are obtained
The product for arriving, carries out a chemical intensification treatment.
Preferably, the method for chemical intensification treatment includes：The product that machining processes are obtained is placed in 350-480 DEG C
Forced fluid (LiNO3、NaNO3And KNO3In at least one) in melt process at least 0.1h, for example process 0.5-15h.Wherein,
As it was previously stated, alkali metal can be any one in Li, Na, K in glass of the invention, in a chemical intensification treatment,
If the alkali metal in glass is mainly Li, forced fluid is melting NaNO3；If under optimum condition, alkali metal is mainly
Na, then forced fluid is melting KNO3If alkali metal is mainly K, be not suitable for doing chemical intensification treatment.Secondary chemical enhanced
During the first time chemical intensification treatment for the treatment of, if the alkali metal in glass is mainly Li, forced fluid is melting LiNO3With
NaNO3(LiNO3And NaNO3Mol ratio be 0.3-0.8:1)；If under optimum condition, alkali metal is mainly Na, then strengthen
Liquid is melting NaNO3And KNO3(NaNO3And KNO3Mol ratio be 0.5-2:1), if alkali metal is mainly K, be not suitable for doing
Chemical intensification treatment.In second chemical intensification treatment of secondary chemical intensification treatment, if the alkali metal in glass is main
It is Li, then forced fluid is melting LiNO3And NaNO3(LiNO3And NaNO3Mol ratio be 0-0.15:1)；If in optimum condition
Under, alkali metal is mainly Na, then forced fluid is melting NaNO3And KNO3(NaNO3And KNO3Mol ratio be 0-0.1:1)；If
Alkali metal is mainly K, then be not suitable for doing chemical intensification treatment.Those skilled in the art can determine specific according to actual conditions
The temperature and time (for example temperature can be 350-480 DEG C, and the time can be 0.5-15h) of chemical intensification treatment, Main Basiss
To obtain the ion exchange depth and surface compression stress value coordinated, this is well known to those skilled in the art, and no longer goes to live in the household of one's in-laws on getting married herein
State.Wherein, after first time chemical intensification treatment, before second chemical intensification treatment, by chemical enhanced place for the first time
Deionized water is used to clean drying after the glass annealing cooling that reason is obtained.
Fourth aspect, the invention provides the alkali silicate glass that the above method is prepared.
Under preferable case, alkali silicate glass of the invention, elastic modelling quantity is higher than 60GPa, and density is less than 2.7g/cm3,
Thermal coefficient of expansion in the range of 50-350 DEG C is less than 90 × 10-7/ DEG C, strain point temperature is higher than 550 DEG C, refractive index nDIt is less than
The corresponding transmitance of 1.55,550nm wavelength is more than 92%.
Wherein, under preferable case, (i.e. machining processes or second melting draw thin treatment) obtains before chemical intensification treatment
The fracture toughness K of the glass for arrivingICMore than 1.0MPam1/2。
Wherein, under preferable case, the fracture toughness K of the glass that chemical intensification treatment is obtainedICMore than 2MPam1/2, enter one
Step is preferably greater than 5MPam1/2, still more preferably more than 8MPam1/2。
Wherein, under preferable case, when thickness is more than 0.1mm, the glass surface obtained through chemical intensification treatment is formed
Compression stress be more than 600MPa, further preferably greater than 650MPa；Compression stress layer depth is more than 30 μm, further preferably greatly
In 35 μm.
Wherein, under preferable case, when thickness is more than 0.1mm, further preferably greater than 0.3mm, through secondary chemical enhanced place
The compression stress that the glass surface that reason is obtained is formed is more than 600MPa, further preferably greater than 650MPa；Compression stress layer depth
More than 60 μm, further preferably greater than 80 μm；
Wherein, under preferable case, when thickness is less than 0.1mm, the glass surface obtained through chemical intensification treatment is formed
Compression stress be more than 200MPa, further preferably greater than 300MPa；Compression stress layer depth is more than 5 μm, further preferably greatly
In 15 μm (such as 15-20 μm).
Wherein, under preferable case, when thickness is less than 0.1mm, the glass obtained through chemical intensification treatment it is minimum curved
Bilge radius are less than 35mm, are further preferably no larger than 30mm.
As it was previously stated, different technique can prepare the glass of different-thickness, it is each by float glass process, press over system, glass tube down-drawing etc.
Planting Conventional glassmaking methods can produce plate glass or thickness of the thickness more than 0.1mm<The flexible glass of 0.1mm, passes through
The thin method of second melting drawing can also produce flexible glass of the thickness less than 0.1mm.Preferably, machining processes or two
Secondary melting draws the thickness of the thin glass for processing and obtaining to be less than 0.1mm.
5th aspect, display is being prepared the invention provides glass composition of the present invention or alkali silicate glass
Device and/or solar cell and the application in other fields for needing the low fragility high tenacity glass material of high intensity, it is excellent
The screen of light guide panel material, flat board or Flexible Displays product in electing as preparing plane or flexible liquid crystal display part backlight module
Curtain surface protection glass material, the substrate glass substrate material of Flexible Displays product, plane and/or flexible solar battery
The cover-plate glass material of substrate glass material, plane and/or flexible solar battery, safety glass, bulletproof glass, intelligent automobile
Application in glass, intelligent transportation display screen, intelligent show window and smart card ticket.
Embodiment
Below will the present invention will be described in detail by embodiment.It is unless otherwise instructed, used in following examples
Each material can be by commercially available, unless otherwise instructed, and method used is the conventional method of this area.
In following examples and comparative example, glass density is determined with reference to ASTM C-693, unit is g/cm3。
50-350 DEG C of thermal expansion coefficient of glass is determined using horizontal expander instrument with reference to ASTM E-228, unit is 10-7/
℃。
Glass Young's modulus is determined using material mechanical test machine with reference to ASTM C-623, unit is GPa.
Determine the strain points of glass using 3 testers with reference to ASTM C-336, unit for DEG C.
The refractive index n of glass is determined using WAY-2S Abbe refractometersD。
The corresponding transmitance of 550nm wavelength of glass is determined using UV-2600 ultraviolet-uisible spectrophotometers.
Glass surface compression stress (unit is MPa) and compression stress layer depth are determined using FSM-6000LE surface stress meters
Degree (unit for μm).
With reference to ASTM E-1820 glass breakage toughness K is determined using universal testing machine and VickersIC, unit is
MPa·m1/2。
Minimum bending radius of the thickness less than 0.1mm glass is tested using bilge radius tester.
Embodiment 1-9
Each component is weighed according to the glass composition shown in table 1, is mixed, compound poured into platinum crucible, Ran Hou
Heated 4 hours in 1430 DEG C of resistance furnace, and bubble is discharged using the stirring of platinum rod.The glass metal that will be melted is poured into not
In rust steel cast iron grinding tool, the both bulk glasses product of regulation is configured to, then by glassware in the lehr, annealed 2 hours, closed
Close power supply furnace cooling to 25 DEG C.Glassware is cut, ground, polished, the glass of the 80*80*1mm for obtaining will be polished
The surface of product is cleaned up with deionized water, and 450 DEG C of melting NaNO is put into after preheated stove preheating3And KNO3(NaNO3With
KNO3Mol ratio be 1.2：1) treatment 10h in, is cleaned up using deionized water after annealing cooling, dried, then preheated
430 DEG C of melting NaNO is placed in after stove preheating3And KNO3Mixed liquor (NaNO3And KNO3Mol ratio be 0.005:1) treatment in
0.5h, is cleaned up and is dried after annealing cooling using deionized water, glass finished-product is obtained stand-by.Respectively to each glass finished-product
Various performances are measured, and the results are shown in Table 1.
Table 1
Embodiment 10-15, comparative example 1-3
According to the method for embodiment 1, unlike, the performance of compound composition (correspondence glass composition) and the product for obtaining
Measurement result is shown in Table 2.
Table 2
Comparative example 4
According to the method for embodiment 1, unlike, the compound composition of comparative example 4 (correspondence glass composition) and obtain
The performance measurement result of product is shown in Table 3, and (that is, the thickness of the glass that comparative example 4 is obtained is 1mm, and has been carried out secondary chemical enhanced
Treatment).
Embodiment 16-17, comparative example 5-8
Respectively by embodiment 16 (correspondence glass composition is with embodiment 2), (the correspondence glass same embodiment of composition of embodiment 17
9), the glassware that comparative example 5-8 (correspondence glass composition is not with comparative example 1-4) polishing is obtained carries out second melting and draws thin place
Reason, obtains the glassware of 80*50*0.08mm, in preheating furnace after the surface deionized water of the glassware is cleaned up
Inside preheated, be subsequently placed into 410 DEG C of melting KNO3Middle treatment 2.5h, takes out and is cooled to 25 DEG C after annealing cooling, spend
Ionized water is cleaned up and dried, and glass finished-product is obtained stand-by.The various performances to each glass finished-product are measured respectively, as a result
It is shown in Table 3 (wherein, the thickness of the glass that comparative example 8 is obtained is 0.08mm, and has carried out a chemical intensification treatment).
Table 3
Embodiment 18-21, comparative example 9-12
Respectively by embodiment 18-21 (correspondence glass composition is with embodiment 2,8,9,13), comparative example 9-12 (correspondence glass groups
Into respectively with comparative example 1-4) surface of the glassware of 80*80*1mm that obtains of polishing cleans up with deionized water, then
Preheated in preheating furnace, be subsequently placed into 430 DEG C of melting KNO3Middle treatment 4h, takes out and is cooled to 25 after annealing cooling
DEG C, cleaned up with deionized water and dried, glass finished-product is obtained stand-by.The various performances to each glass finished-product are surveyed respectively
It is fixed, the results are shown in Table 4.
Table 4
Data in table 1-4 are compared and is understood, the method for the present invention utilizes the SiO containing certain content2、B2O3、P2O5、
Al2O3、Li2O、Na2O、K2O, MgO, CaO, SrO, BaO, ZnO and RE2O3The glass for preparing of glass composition, have concurrently
Low fragility, good intensity and toughness.Glass composition of the invention or alkali silicate glass can be used to prepare display device
And/or solar cell, particularly for prepare light guide panel material in plane or flexible liquid crystal display part backlight module, flat board or
Flexible Displays product screen surface protection with glass material, the substrate glass substrate material of Flexible Displays product, plane and/or
The cover-plate glass material of the substrate glass material, plane and/or flexible solar battery of flexible solar battery, safety glass,
Bulletproof glass, intelligent automobile glass, intelligent transportation display screen, intelligent show window, smart card ticket and need low fragility for other
The field of high tenacity glass material.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned implementation method
Detail, in range of the technology design of the invention, various simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned specific embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy is no longer separately illustrated.
Additionally, can also be combined between a variety of implementation methods of the invention, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (16)
1. a kind of glass composition, it is characterised in that on the basis of the weight of said composition, in terms of oxide, said composition
SiO containing 40-80wt%2+B2O3+P2O5, 3-25wt% Al2O3, 10-25wt% Li2O+Na2O+K2O, 0-15wt%
MgO+CaO+SrO+BaO, 0-5wt% ZnO and 0-5wt% RE2O3, wherein, said composition contains B2O3And P2O5In
At least one, and contain ZnO and RE2O3In at least one.
2. composition according to claim 1, it is characterised in that on the basis of the weight of said composition, in terms of oxide,
B2O3Content be 0-30wt%；
Preferably, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 1-10wt%；
Preferably, on the basis of the weight of said composition, in terms of oxide, B2O3Content be 15-25wt%.
3. composition according to claim 1 and 2, it is characterised in that on the basis of the weight of said composition, with oxide
Meter, P2O5Content be 0-20wt%, preferably 4-16wt%.
4. the composition according to any one in claim 1-3, it is characterised in that the weight with said composition is as base
Standard, in terms of oxide, SiO2Content be 40-75wt%.
5. the composition according to any one in claim 1-4, it is characterised in that the weight with said composition is as base
Standard, in terms of oxide, the content of ZnO is 0.2-5wt%, preferably 0.5-4wt%.
6. the composition according to any one in claim 1-5, it is characterised in that the weight with said composition is as base
Standard, in terms of oxide, RE2O3Content be 0.01-5wt%, preferably 0.3-3wt%；
Preferably, RE2O3It is rare earth oxide Y2O3、La2O3、Gd2O3、Ce2O3、Yb2O3And Lu2O3In at least one, and with weight
Amount percentages, Y2O3+La2O3>0wt%.
7. the composition according to any one in claim 1-6, it is characterised in that by weight percentage, 0.6<
Na2O/(Li2O+Na2O+K2O)<1。
8. the composition according to any one in claim 1-7, it is characterised in that the weight with said composition is as base
Standard, in terms of oxide, the content of MgO is 1-6wt%.
9. the composition according to any one in claim 1-8, it is characterised in that the composition also contains clarification
Agent, the fining agent is preferably at least one in sulfate, nitrate, tin oxide, stannous oxide, chloride and fluoride；
On the basis of the weight of said composition, the content of fining agent is not more than 1wt%.
10. a kind of method for preparing alkali silicate glass, it is characterised in that the method includes will be any one in claim 1-9
Glass described in carries out melt process, forming processes, annealing and machining processes successively with composition,
Preferably, the method also includes that the product obtained to machining processes carries out chemical intensification treatment, it is further preferred that
The chemical intensification treatment is a chemical intensification treatment or secondary chemical intensification treatment.
11. methods according to claim 10, it is characterised in that the method also includes：It is right before chemical intensification treatment
The product that machining processes are obtained carries out second melting and draws thin treatment；
Preferably, the machining processes or second melting is controlled to draw the condition of thin treatment to prepare thickness less than 0.1mm
Glass；
The product that machining processes preferably for thickness more than 0.1mm are obtained, carries out a chemical intensification treatment or two
Secondary chemical intensification treatment；
The product that machining processes preferably for thickness more than 0.3mm are obtained, carries out secondary chemical intensification treatment；
The product that machining processes preferably for thickness less than 0.1mm are obtained, carries out a chemical intensification treatment.
The alkali silicate glass that method described in 12. claims 10 or 11 is prepared.
13. alkali silicate glass according to claim 12, it is characterised in that the elastic modelling quantity of the alkali silicate glass
Higher than 60GPa, density is less than 2.7g/cm3, the thermal coefficient of expansion in the range of 50-350 DEG C is less than 90 × 10-7/ DEG C, strain point temperature
Degree is higher than 550 DEG C, refractive index nDTransmitance corresponding less than 1.55,550nm wavelength is more than 92%.
The 14. alkali silicate glass according to claim 12 or 13, it is characterised in that obtained before the chemical intensification treatment
Glass fracture toughness KICMore than 1.0MPam1/2；And/or
The fracture toughness K of the glass that the chemical intensification treatment is obtainedICMore than 2MPam1/2, further preferably greater than 5MPa
m1/2, still more preferably more than 8MPam1/2。
The 15. alkali silicate glass according to any one in claim 12-14, it is characterised in that thickness is more than 0.1mm
When, the compression stress that the glass surface obtained through chemical intensification treatment is formed is more than 600MPa, preferably greater than 650MPa；Pressure
Stress under compression layer depth is more than 30 μm, preferably greater than 35 μm；
When thickness is more than 0.1mm, preferably greater than 0.3mm, the compression that the glass surface obtained through secondary chemical intensification treatment is formed
Stress is more than 600MPa, preferably greater than 650MPa；Compression stress layer depth is more than 60 μm, preferably greater than 80 μm；
When thickness is less than 0.1mm, the compression stress that the glass surface obtained through chemical intensification treatment is formed more than 200MPa,
Preferably greater than 300MPa；Compression stress layer depth is more than 5 μm, preferably greater than 15 μm；
Preferably, when thickness is less than 0.1mm, the minimum bending radius of the glass obtained through chemical intensification treatment is less than
35mm, is further preferably no larger than 30mm.
In glass composition or claim 12-15 in 16. claim 1-9 described in any one described in any one
Application of the alkali silicate glass in display device and/or solar cell is prepared, is preferably preparing plane or flexible liquid crystal
Screen surface protection glass material, the flexibility of light guide panel material, flat board or Flexible Displays product in display device backlight module
Show the substrate glass material of substrate glass substrate material, plane and/or flexible solar battery of product, plane and/or soft
Cover-plate glass material, safety glass, bulletproof glass, intelligent automobile glass, intelligent transportation display screen, the intelligence of property solar cell
Application in show window and smart card ticket.
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| CN113582539A (en) * | 2021-08-30 | 2021-11-02 | 郑州大学 | Aluminosilicate glass and application |
| CN113582539B (en) * | 2021-08-30 | 2023-06-16 | 郑州大学 | Aluminosilicate glass and application |
| CN116177902A (en) * | 2023-04-26 | 2023-05-30 | 秦皇岛星箭特种玻璃有限公司 | Preparation method of flexible glass |
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