CN109678341A - Alkali-free glass compositions and alkali-free glass and application - Google Patents
Alkali-free glass compositions and alkali-free glass and application Download PDFInfo
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- CN109678341A CN109678341A CN201811512297.4A CN201811512297A CN109678341A CN 109678341 A CN109678341 A CN 109678341A CN 201811512297 A CN201811512297 A CN 201811512297A CN 109678341 A CN109678341 A CN 109678341A
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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
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
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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
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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
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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
- C03C4/00—Compositions for glass with special properties
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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
- C03C4/00—Compositions for glass with special properties
- C03C4/20—Compositions for glass with special properties for chemical resistant glass
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Abstract
The present invention relates to glass art, a kind of alkali-free glass compositions and alkali-free glass and preparation method thereof are disclosed.The alkali-free glass compositions include: on the basis of the total weight of alkali-free glass compositions, which contains the SiO of 58-64wt%2, 16-19wt% Al2O3, 7-13wt% B2O3+P2O5, 0.5-3.5wt% MgO, 4-8wt% CaO, 0.1-4wt% SrO, 0-2.5wt% BaO, 0-4wt% ZnO, the R less than 0.05wt%2O, wherein R2O is Li2O、Na2O、K2The sum of content of O.Glass mechanical strength with higher, the lesser density of composition preparation of the present invention, higher chemical corrosion resistance (i.e. high chemical stability), low thermal expansion coefficient (are lower than 38 × 10‑7/ DEG C), the excellent properties such as higher strain point temperature, can be used for preparing display device and/or area of solar cell, have a good application prospect.
Description
Technical field
The present invention relates to glass arts, and in particular to alkali-free glass compositions and alkali-free glass and application.
Background technique
LCD technology has become the key technology of modern most important picture transmission and reproduction.Liquid crystal display
Principle is imaged, is to be placed in liquid crystal between two panels electro-conductive glass, by the driving of two electric field between electrodes, causes twisted liquid crystal molecules
The field effect of nematic generates light and shade between power supply pass is opened and shows image to control lit transmissive or shielding function
Come, if adding colored filter, can show chromatic image.TFT liquid crystal display mode, with 600 times faster than old-fashioned LCD screen
Pixel response speed.Advanced silicon electrode is added, and greatly accelerates the pixel response speed of LCD screen, reduces what picture occurred
Delay phenomenon.Higher technical requirements are proposed to glass substrate, the geometric dimension of the substrate after processing must not heating condition
Influence, i.e., the thermal expansion coefficient of this kind of glass substrate wants small, according to glass substrate make in the stress resultant of production consider,
Best thermal expansion coefficient is 28 × 10-7/ DEG C or so.
For the glass substrate of TFT-LCD, need through technologies such as sputtering, chemical vapor depositions (CVD) in underlying substrate
Glass surface forms transparent conductive film, insulating film, semiconductor (polysilicon, amorphous silicon etc.) film and metal film, then passes through light
Etching (Photo-etching) technology forms various circuits and figure, if glass contains alkali metal oxide (Na2O, K2O,
Li2O), alkali metal ion diffuses into deposited semiconductor material during heat treatment, damages semiconductor film characteristic, therefore, glass
Glass should be free of alkali metal oxide, it is necessary to use alkali-free glass, it is preferred that with SiO2、Al2O3、B2O3And alkaline earth oxide
RO (RO=Mg, Ca, Sr, Ba) etc. is the silicate glass containing boron and aluminium without alkali of principal component.
Now with the quick universal of portable electronic device (such as laptop, smart phone, PDA), to accessory
Lightweight proposes requirements at the higher level.Thus to the composition of glass substrate, more stringent requirements are proposed, to guarantee to adapt to modern liquid crystal
The needs of display.Glass substrate must have the property that containing alkali metal oxide less than 1000ppm;Has chemical resistance;
Thermal expansion coefficient must be close with the silicon of thin film transistor (TFT);Strain point of glass is improved, to reduce thermal shrinking quantity;With lesser close
Degree, in order to carry and hold.
In addition to lightweight, the glass substrate for portable electronic device also needs to meet people and executes and enjoy all the time
By the requirement of commercial affairs and the recreation of higher level.Such demand requires also to be continuously improved to display performance, especially
The image quality of intelligent movable equipment, visual performance requirement outdoors are also being promoted.Under the guidance of this trend,
Display panel develops to the direction that lightening, ultra high-definition is shown, on the one hand, it is required that glass substrate should have it is lesser close
Degree;On the other hand, panel making technology manages temperature development to higher height;Monolithic glass passes through process simultaneously, and thickness reaches
0.25mm, 0.2mm, 0.1mm, 0.05mm are even more thin.
The mode for keeping glass thinning is presently mainly chemical reduction, specifically, uses hydrofluoric acid or buffered hydrofluoric acid solution
Glass substrate is corroded, thinning principle is as follows:
Main chemical reactions: 4HF+SiO2=SiF4+2H2O;
Secondary chemical reaction: RO+2H+=R2++H2O (R represents alkaline-earth metal etc.).
Surface quality and parent glass composition after chemical reduction technique and thinning glass substrate have certain relationship, existing
TFT-LCD base plate glass frequently occurs the bad deficient point such as " pit ", " sags and crests " during chemical reduction, increases and is produced into
This.Glass with high chemical stability has better surface quality after being thinned, therefore researches and develops high chemical stability
TFT-LCD base plate glass, it is possible to reduce the production costs such as second polishing promote product quality and yields, for large scale industry
Metaplasia production has larger benefit.And excessively slow hydrofluoric acid or buffered hydrofluoric acid solution corrosion rate can reduce thinning factory production efficiency.
According to the technical standard of liquid crystal display, it is special that the glass substrate of TFT-LCD must have basic physics below
Property:
1, the thermal expansion coefficient of glass substrate must be enough low, is not higher than 38 × 10-7/℃;
2, the strain point temperature of glass substrate should be higher than that 640 DEG C;
3, density is lower than 2.6g/cm3, and it is more lighter better.
But with the progress of LCD technology, curved-surface display, advanced lines panel propose one to the performance of glass substrate
A little new requirements require for example, can bear smaller radius of curvature in bending without rupturing, and large-size substrate is passing
Occurs sag of chain small as far as possible during defeated.This just needs glass substrate to improve bending strength, Young's modulus or than machines such as moduluses
Tool performance.And under normal conditions, the improvement (enhancing) of mechanical performance often brings middle warm area viscosity (strain point, annealing point, softening
Near point) and the undesirable variation of high-temperature region viscosity (forming temperature, fusion temperature etc.) appearance.Such as in practical alkali-free liquid-crystalline glasses
In composition, Al2O3, the oxides such as MgO, SrO, BaO increase improve Young's modulus, but deposit physics and chemistry in other respects
The drawbacks of capable of being deteriorated, for example, promoting Al2O3Content will lead to liquidus temperature and be substantially improved;Content of MgO is promoted, will lead to point
Mutually tendency increases, liquidus temperature is substantially improved and declines to a great extent with low temperature viscosity;SrO content and/or BaO content are promoted, can be led
It causes high temperature viscosity of glass to increase to be substantially increased with density, is unfavorable for improving than modulus.
CN105392743A discloses the alkali-free glass of a kind of high Young's modulus and Gao Bi elasticity modulus, and Young's modulus is
94.5GPa or more, than elasticity modulus be 34.5GPa/ (g/cm3) more than, but have the excessively high coefficient of expansion, 50-350 DEG C it
Between mean thermal expansion coefficients be all larger than 38 × 10-7/ DEG C, it is unable to satisfy TFT LCD technology requirement;
CN104211300A discloses a kind of alkali-free glass formula of high specific modulus, and elasticity modulus is higher than 82GPa, compares mould
Number is higher than 33GPa/ (g/cm3), while middle warm area viscosity with higher, strain point are higher than 720 DEG C.In order to reach above-mentioned mesh
Mark, this application have used more Al in composition2O3With less B2O3, to provide mechanical strength and Heat-resistant stable simultaneously
Property.But the compositing characteristic will lead to declining to a great extent for chemical-resistant stability, particularly hydrofluoric acid corrosion resistance, be unfavorable for current
The demand of lightening substrate manufacture.
Therefore, it needs a kind of while having both improved mechanical performance and the glass of other performances, to be suitble to TFT liquid crystal display
The requirement of technology.
Summary of the invention
The purpose of the invention is to overcome improvement glass machinery performance of the existing technology that can damage other performances (such as
Heat-resistant stability, chemical corrosion resistance) the problem of making it not be able to satisfy TFT LCD technology requirement, alkali-free glass group is provided
Close object and alkali-free glass and application.
To achieve the goals above, first aspect present invention provides a kind of alkali-free glass compositions, comprising: with alkali-free glass
On the basis of the total weight of glass composition, which contains the SiO of 58-64wt%2, 16-19wt% Al2O3、7-
The B of 13wt%2O3+P2O5, 0.5-3.5wt% MgO, 4-8wt% CaO, 0.1-4wt% SrO, 0-2.5wt% BaO,
The ZnO of 0-4wt%, the R less than 0.05wt%2O, wherein R2O is Li2O、Na2O、K2The sum of content of O.
Second aspect of the present invention provides the glass made of glass composition of the present invention.
Third aspect present invention provides the method that the glass composition as described in first aspect present invention prepares glass, the party
Method includes: to melt glass composition described in first aspect present invention, form, making annealing treatment, and machining processes.
The alkali-free glass made of glass composition of the present invention has high mechanical strength, suitable resistant to chemical etching
Property, excellent heat-resistant stability, specifically, the alkali-free glass have following performance standard:
A. crooked test maximum stress value σmax≥80MPa;And
B. crooked test maximum strain amount εmax≥1500×10-6。
In addition, other physical characteristics of the alkali-free glass can be stable reach:
(1) density≤2.49g/cm3;
(2) thermal expansion coefficient within the scope of 50-350 DEG C is lower than 38 × 10-7/℃;
(3) Young's modulus >=72GPa, than modulus >=30GPa (g/cm3);
(4) strain point TstIt is 650 DEG C -730 DEG C;
(5) liquidus temperature TL≤1200℃;
(6) viscosity is the corresponding temperature T of 200 pools200≤1630℃;
(7) hydrofluoric acid corrosion rate is 4mg/cm2-6.5mg/cm2;
(8) wavelength is transmitance >=50% at 308nm;
(9) 1200 DEG C of surface tension≤370mN/m;
(10) Vickers hardness >=580kgf/cm2;
(11) refractive index nD≤1.53.
Preferably, what the characteristic of the alkali-free glass can be stable reaches:
(1) crooked test maximum stress value σmax≥100MPa;And
(2) crooked test maximum strain amount εmax≥1600×10-6;
(3) density≤2.42g/cm3;
(4) thermal expansion coefficient within the scope of 50-350 DEG C is lower than 36 × 10-7/℃;
(5) Young's modulus >=73GPa, than modulus >=30.5GPa (g/cm3);
(6) strain point TstIt is 680 DEG C -700 DEG C;
(7) liquidus temperature TL≤1130℃;
(8) viscosity is the corresponding temperature T of 200 pools200≤1627℃;
(9) hydrofluoric acid corrosion rate is 4.5mg/cm2-5.2mg/cm2;
(10) wavelength is transmitance >=70% at 308nm;
(11) 1200 DEG C of surface tension≤360mN/m
(12) Vickers hardness >=620kgf/cm2;
(13) refractive index nD≤1.52.
Fourth aspect present invention provides the glass as described in second aspect of the present invention in display device and/or solar battery
In application.
Glass mechanical strength with higher (the i.e. high crooked test maximum stress value of composition preparation of the present invention
With crooked test maximum strain amount), higher chemical corrosion resistance (i.e. high chemical stability), low thermal expansion coefficient is (low
In 38 × 10-7/ DEG C), the excellent properties such as higher strain point temperature.The glass can be used for preparing display device and/or the sun
Energy battery, is particularly suitable for preparing the substrate glass substrate material of flat panel display product and/or screen surface protection glass-film
Layer material, the substrate glass substrate material of Flexible Displays product and/or surface encapsulation glass material and/or screen surface protection are used
Glass film layers material, the substrate glass substrate material of flexible solar battery, safety glass, bulletproof glass, intelligent automobile glass,
Intelligent transportation display screen, intelligent show window and smart card ticket and high thermal stability and mechanical stability glass material are needed for other
The application field of material.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
First aspect present invention provides a kind of alkali-free glass compositions, comprising: with the total weight of alkali-free glass compositions
On the basis of, which contains the SiO of 58-64wt%2, 16-19wt% Al2O3, 7-13wt% B2O3+P2O5、
The ZnO of BaO, 0-4wt% of SrO, 0-2.5wt% of CaO, 0.1-4wt% of MgO, 4-8wt% of 0.5-3.5wt%, it is less than
The R of 0.05wt%2O, wherein R2O is Li2O、Na2O、K2The sum of content of O.
According to the present invention, on the basis of the total weight of alkali-free glass compositions, which contains: 58-64wt%
SiO2, such as SiO2Content can for 58wt%, 58.4wt%, 58.5wt%, 58.9wt%, 59.5wt%,
59.7wt%, 59.8wt%, 60wt%, 61.4wt%, 61.7wt%, 61.8wt%, 61.9wt%, 62wt%, 62.1wt%,
62.2wt%, 62.3wt%, 62.4wt%, 62.5wt%, 62.6wt%, 62.7wt%, 62.8wt%, 62.9wt%,
Appointing in 63wt%, 63.3wt%, 63.6wt%, 63.7wt%, 63.8wt%, 63.9wt%, 64wt% and these point values
Arbitrary value in two ranges constituted of anticipating;
The Al of 16-19wt%2O3, such as Al2O3Content can for 16wt%, 16.3wt%, 16.8wt%,
17.1wt%, 17.2wt%, 17.3wt%, 17.4wt%, 17.5wt%, 17.6wt%, 17.7wt%, 17.8wt%,
17.9wt%, 18wt%, 18.1wt%, 18.3wt%, 18.5wt%, 18.8wt%, 18.9wt%, 19wt% and these points
The arbitrary value in range that any two in value are constituted;
The B of 7-13wt%2O3+P2O5, such as B2O3、P2O5The sum of content can for 7wt%, 7.5wt%, 8wt%,
8.5wt%, 9wt%, 9.5wt%, 10wt%, 10.5wt%, 11wt%, 11.5wt%, 12wt%, 12.5wt%, 13wt%
And the arbitrary value in the range that is constituted of any two in these point values;
The MgO of 0.5-3.5wt%, for example, MgO content can for 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%,
0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%,
1.8wt%, 1.9wt%, 2.1wt%, 2.4wt%, 2.6wt%, 2.8wt%, 3wt%, 3.1wt%, 3.3wt%, 3.5wt%
And the arbitrary value in the range that is constituted of any two in these point values;
The CaO of 4-8wt%, for example, CaO content can for 4.1wt%, 4.4wt%, 4.8wt%, 5wt%,
5.2wt%, 5.3wt%, 5.4wt%, 5.5wt%, 5.6wt%, 5.7wt%, 5.8wt%, 5.9wt%, 6wt%,
6.1wt%, 6.2wt%, 6.3wt%, 6.4wt%, 6.6wt%, 6.8wt%, 7.1wt%, 7.2wt%, 7.3wt%,
The arbitrary value in range that any two in 7.5wt%, 7.7wt%, 8wt% and these point values are constituted;
The SrO of 0.1-4wt%, for example, SrO content can for 0.1wt%, 0.2wt%, 0.4wt%, 0.6wt%,
0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%,
1.6wt%, 1.7wt%, 1.8wt%, 1.9wt%, 2wt%, 2.1wt%, 2.2wt%, 2.3wt%, 2.4wt%,
2.5wt%, 2.6wt%, 2.7wt%, 2.8wt%, 2.9wt%, 3wt%, 3.1wt%, 3.2wt%, 3.3wt%,
Any two in 3.4wt%, 3.5wt%, 3.6wt%, 3.7wt%, 3.8wt%, 3.9wt%, 4wt% and these point values
The arbitrary value in range constituted;
The BaO of 0-2.5wt%, for example, BaO content can for 0wt%, 0.2wt%, 0.4wt%, 0.6wt%,
0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%,
1.6wt%, 1.7wt%, 1.8wt%, 1.9wt%, 2wt%, 2.1wt%, 2.2wt%, 2.3wt%, 2.4wt%, 2.5wt%
And the arbitrary value in the range that is constituted of any two in these point values;
The ZnO of 0-4wt%, for example, ZnO content can for 0wt%, 0.1wt%, 0.2wt%, 0.26wt%,
0.3wt%, 0.4wt%, 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 1.1wt%,
1.2wt%, 1.3wt%, 1.4wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.8wt%, 2wt%, 2.5wt%,
Appointing in the range that any two in 2.8wt%, 3wt%, 3.3wt%, 3.7wt%, 4wt% and these point values are constituted
Meaning value.
In the present invention, the alkali-free glass compositions are interpreted as not needing in the composition in addition adding alkali metal group
Point, the alkaline components can be added in the form of any simple substance or compound containing alkali metal element.The alkali metal
Including Li, Na and/or K.
In alkali-free glass compositions of the present invention, SiO2For glass former, if SiO2Content it is too low, be unfavorable for
The enhancing of endurance and corrosion resistance, it is excessively high to will cause the coefficient of expansion, and glass is caused to be easy devitrification;If SiO2Content increase,
Although facilitating glass lightweight, thermal expansion coefficient reduces, and strain point increases, and endurance increases, SiO2Too high levels
The high temperature viscosity that will cause alkali-free glass obtained increases, i.e., fusion temperature increases, and is unfavorable for melting in this way, and general kiln is difficult
To meet conventional high capacity smelting technology for material melt batch.It is therefore preferred that SiO2Content be 58-64wt%, this
Sample is conducive to endurance, mechanical strength and the high temperature viscosity of further taking into account gained alkali-free glass.
In alkali-free glass compositions of the present invention, work as Al2O3Content it is too low when, glass heat resistance is difficult to be promoted,
It is easy the erosion by extraneous aqueous vapor and chemical reagent;Work as Al2O3Content increase when, although facilitating strain point of glass, machinery
Intensity increases, but Al2O3Too high levels be easy to appear crystallization, while can glass be difficult to melt.Preferably, with alkali-free
On the basis of the total weight of glass composition, Al2O3Content be 17-18wt%, be conducive to advanced optimize gained alkali-free glass in this way
Heat resistance, endurance and the mechanical strength of glass, and improve crystallization property.
In alkali-free glass compositions of the present invention, B2O3、P2O5As the matrix for constituting glass, it can be individually created glass,
They be added can reinforcing glass chemical stability, mechanical performance, while B2O3、P2O5It is also good fluxing agent, high temperature item
High temperature viscosity can be reduced under part, and glass melting temperature can be greatly reduced, it is also helpful for During Vitrification in vitro;B, which has, when low temperature takes by force
The trend for taking free oxygen makes structure tend to the low temperature difficulty for closely improving glass, prevents the generation of crystallization.But it is excessive
B2O3Strain point of glass can be made to be greatly reduced.Preferably, on the basis of the total weight of alkali-free glass compositions, B2O3With P2O5Weight
The sum of amount content meets 7wt% < B2O3+P2O5≤ 13wt%;It is further preferred that 8.8wt%≤B2O3+P2O5≤ 11wt%.
In alkali-free glass compositions of the present invention, adding appropriate ZnO helps to reduce crystallization temperature, and then inhibits analysis
Crystalline substance, and can reduce high temperature viscosity of glass is conducive to eliminate bubble, at the same have below softening point promoted glass intensity,
Hardness, endurance, the effect for reducing thermal expansion coefficient of glass.Theoretically, ZnO in alkali-free glass, draws as network outer body
After entering glass, generally with [ZnO under high temperature4] form exist, compared with [ZnO6] glass structure is more loose, with the glass for being free of ZnO
It being compared under same high temperature state, the glass viscosity containing ZnO is smaller, and atomic motion speed is bigger, nucleus can not be formed,
It needs to further decrease temperature, is just conducive to the formation of nucleus, thus reduce the crystallization ceiling temperature of glass.And ZnO content
Excessively the strain point of glass can be made to be greatly lowered, be unfavorable for the promotion of glass substrate thermal stability.
In alkali-free glass compositions of the present invention, MgO, CaO, SrO, BaO belong to alkaline earth oxide, they
The high temperature viscosity that can effectively reduce glass is added to improve the meltbility and formability of glass, and the strain of glass can be improved
Point.In addition, MgO, BaO have the characteristics that improve alkali-free glass chemical stability and mechanical stability.But alkaline-earth metal oxide
The content of object can excessively be such that the density of alkali-free glass increases, the incidence raising of crackle, devitrification, split-phase.
In a preferred embodiment, which contains the SiO of 61-63wt%2, 17-18wt%
Al2O3, 8.8-11wt% B2O3+P2O5, 1.1-2.7wt% MgO, 5.4-7.7wt% CaO, 1.6-3.6wt%
The ZnO of BaO, 0wt% of SrO, 0wt%, the R less than 0.05wt%2O, wherein R2O is Li2O、Na2O、K2The sum of content of O.
In alkali-free glass compositions of the present invention, it is further preferred that the total weight with alkali-free glass compositions is
Benchmark, SiO2And Al2O3The sum of content Q meets Q > 75wt%;It is further preferred that 75wt% < Q < 82wt%;It is further excellent
Selection of land, 78wt% < Q < 81wt%, in this way can the alkali-free glass obtained by improving to the maximum extent chemical resistance, corrosion-resistant
Property, heat resistance, machinability and mechanical strength, while reducing the probability for crystallization occur.
In alkali-free glass compositions of the present invention, although B2O3、P2O5It is all good fluxing agent, so that raw material melts
More easily.But B2O3/(B2O3+P2O5) weight percentage than it is too low when, can be to a certain degree such as down to 0.1 or 0.01
Upper raising liquidus temperature, while can also damage chemical corrosion resistance.Preferably, B2O3、(B2O3+P2O5) weight ratio B2O3/
(B2O3+P2O5) > 0.1, such as can be appointing in 0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9,1 and these point values
Arbitrary value in two ranges constituted of anticipating;It is further preferred that 0.8 < B2O3/(B2O3+P2O5)≤1。
In composition of the present invention, alkaline earth oxide such as MgO, CaO, SrO, BaO can effectively reduce glass
High temperature viscosity, but R ' O/ (B2O3+P2O5) weight ratio it is too high or too low can all bring undesirable influence, wherein R ' be MgO,
The sum of CaO, SrO, BaO and ZnO content.Work as R ' O/ (B2O3+P2O5) it is lower when, when being, for example, less than 0.5, glass can be significantly reduced
Thermal stability is (here, use strain point temperature TstCharacterize the thermal stability of glass, TstHigher, the thermal stability of glass is higher),
Liquidus temperature can increase simultaneously;And work as R ' O/ (B2O3+P2O5) it is higher when, such as when higher than 1.9, can also improve the liquid of glass
Liquidus temperature, the increase of simultaneous thermal expansion coefficient.It is preferred that 0.5 < R ' O/ (B2O3+P2O5) < 1.9, such as
It can be any one value in 0.6,0.8,1,1.2,1.4,1.6,1.8 and above-mentioned numerical value in any two institute compositing range;
Further preferably 0.9 < R ' O/ (B2O3+P2O5) < 1.3, still more preferably 1.0 < R ' O/ (B2O3+P2O5) < 1.2, more
Further preferably R ' O/ (B2O3+P2O5)=1.1.
In alkali-free glass compositions of the present invention, the weight ratio of MgO, CaO also will affect glass combination raw material
Liquidus temperature, such as when MgO/CaO ratio is excessively high, the liquidus temperature of glass combination raw material can be also obviously improved, no
Conducive to the industrialization manufacture of glass.It is preferred that MgO, CaO content ratio, 0.1 < MgO/CaO < 0.9, such as can be
0.2,0.3,0.4,0.5,0.6,0.7,0.8 and these point values in the constituted range of any two in arbitrary value, into one
Walk preferably 0.15 < MgO/CaO < 0.5.
In alkali-free glass compositions of the present invention, the weight ratio of SrO, CaO also will affect glass combination raw material
Liquidus temperature, such as when SrO/CaO ratio is excessively high, the liquidus temperature of glass combination raw material can be also obviously improved, no
Conducive to the industrialization manufacture of glass.It is preferred that SrO, CaO content ratio SrO/CaO > 0.01, for example, can for 0.05,
0.1,0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5,0.55,0.6,0.65,0.8 and these point values in it is any
Arbitrary value in two constituted ranges;Preferably 0.2 < SrO/CaO < 0.6, more preferably 0.3 < SrO/CaO < 0.45.
According to the present invention, in the alkali-free glass compositions, on the basis of the total weight of alkali-free glass compositions, BaO
Content be less than 2wt%;Preferably, the content of BaO is less than 1.5wt%;It is further preferred that the content of BaO is less than 1wt%;
It is further preferred that the content of BaO is less than 0.005wt%, it is further preferred that being free of BaO.
According to the present invention, in the alkali-free glass compositions, on the basis of the total weight of alkali-free glass compositions, ZnO
Content be less than 2wt%;Preferably, the content of ZnO is less than 1.2wt%;It is further preferred that the content of ZnO is less than
0.8wt%;It is further preferred that the content of ZnO is less than 0.005wt%;It is further preferred that being free of ZnO.
According to the present invention, the alkali-free glass compositions also contain chemical fining agent, with the gross weight of alkali-free glass compositions
On the basis of amount, the content of clarifying agent is not more than 1wt%.The chemical fining agent can be selected according to the prior art, such as institute
Stating chemical fining agent can be sn-containing compound, such as tin oxide.
Second aspect of the present invention provides glass made of the glass composition described in first aspect present invention, the glass
It has the following performance:
A. crooked test maximum stress value σmax≥80MPa;And
B. crooked test maximum strain amount εmax≥1500×10-6。
Preferably, the crooked test maximum stress value σ of the glassmax>=100MPa, it is further preferred that σmax≥
120MPa, it is further preferred that σmax≥130MPa;Preferably, crooked test maximum strain amount εmax≥1600×10-6, excellent
Selection of land, εmax≥1700×10-6, it is highly preferred that εmax≥1800×10-6。
Preferably, the glass also has the following performance:
(1) viscosity is the corresponding temperature T of 200 pools200≤ 1630 DEG C, preferably T200≤1627℃;
(2) liquidus temperature TL≤ 1200 DEG C, preferably TL≤1130℃;
(3) strain point TstIt is 650-730 DEG C, preferably 680 DEG C -700 DEG C, more preferably 680 DEG C -695 DEG C;
(4) Young's modulus >=72GPa and than modulus >=30GPa (g/cm3), it is preferable that Young's modulus >=73GPa and compare mould
Number >=30.5GPa/ (g/cm3);And
(5) hydrofluoric acid corrosion rate is 4-6.5mg/cm2, preferably 4.5-5.3mg/cm2, more preferably 4.5-5.2mg/
cm2。
According to the present invention, the glass also has the following performance:
(6) density is lower than 2.49g/cm3, it is preferably lower than 2.42g/cm3;
(7) thermal expansion coefficient within the scope of 50-350 DEG C is lower than 38 × 10-7/ DEG C, it is preferably lower than 36 × 10-7/℃;
(8) wavelength is transmitance >=50% at 308nm, preferably >=70%;
(9) 1200 DEG C of surface tension≤370mN/m, preferably≤360mN/m;
(10) Vickers hardness >=580kgf/cm2, preferably >=620kgf/cm2;
(11) refractive index nD≤1.53, preferably≤1.52.
The mechanical strength with higher of glass described in second aspect of the present invention (i.e. high crooked test maximum stress value and
Crooked test maximum strain amount), while having both low-density, higher chemical corrosion resistance (i.e. high chemical stability), low
Thermal expansion coefficient (is lower than 38 × 10-7/ DEG C), the excellent properties such as higher strain point temperature.
Third aspect present invention provides the method that the glass composition as described in first aspect present invention prepares glass, the party
Method includes: to melt glass composition described in first aspect present invention, form, making annealing treatment, and machining processes.Institute
State the glass finished-product that glass can be any shape, for example, glass plate.
In third aspect present invention the method, before melt composition, first the various components of composition are mixed
Uniformly.Melting, molding condition can be selected according to the prior art, such as the condition of melt process includes: temperature lower than 1630
DEG C, the time is greater than 1h.Those skilled in the art can specific temperature and time determines according to actual conditions, it is no longer superfluous herein
It states.
In third aspect present invention the method, under preferable case, the condition of annealing includes: that temperature is higher than 720
DEG C, the time is greater than 0.1h.Those skilled in the art can specific annealing temperature and time determines according to actual conditions, herein not
It repeats again.
In third aspect present invention the method, for machining processes, there is no particular limitation, can be ability
The common various machining modes in domain, such as can be cut for the product for obtaining annealing, grind, polish.
Preferably, this method further include: second melting is carried out to the product that machining processes obtain and draws thin processing.
Preferably, the machining processes are controlled or second melting draws the condition of thin processing to be less than to prepare thickness
The glass plate of 0.1mm.
Fourth aspect present invention provides the glass as described in second aspect of the present invention in display device and/or solar battery
In application.
Alkali-free glass of the present invention can be used for preparing display device and/or solar battery, and it is flat to be particularly suitable for preparation
Plate shows the substrate glass substrate material of product and/or the lining of screen surface protection glass film layers material, Flexible Displays product
Bottom glass substrate material and/or surface encapsulation glass material and/or screen surface protection glass film layers material, flexible solar
Substrate glass substrate material, safety glass, bulletproof glass, intelligent automobile glass, intelligent transportation display screen, the intelligent show window of battery
The application field of high thermal stability and mechanical stability glass material is needed with smart card ticket and for other.
The present invention will be described in detail by way of examples below.
In following embodiment, unless otherwise instructed, each raw material used can be commercially available, unless otherwise instructed,
Used test method is the conventional method of this field.
Glass density, unit g/cm are measured referring to ASTM C-6933。
Referring to the thermal expansion coefficient of glass that ASTM E-228 uses horizontal expander instrument to measure 50-350 DEG C, unit 10-7/
℃。
Glass Young's modulus, unit GPa are measured referring to ASTM C-623;It is obtained by the ratio calculation of Young's modulus and density
To than modulus, unit is GPa/ (g/cm3)。
Glass high temperature viscosity-temperature curve is measured using rotation high-temperature viscosimeter referring to ASTM C-965, wherein 200P viscosity pair
The temperature T answered200, unit is DEG C;The corresponding temperature T of 35000P viscosity35000, unit is DEG C.
Glass liquidus temperature T is measured using temperature gradient furnace method referring to ASTM C-829L, unit is DEG C.
Glass annealing point T is measured using annealing point strain point tester referring to ASTM C-336aWith strain point Tst, unit is
℃。
Glass Vickers hardness, unit kgf/cm are measured using Vickers referring to ASTM E-3842。
Glass 1200 is measured using high temperature surface tension instrument (Beijing Xu Hui new master Science and Technology Ltd., model ZLXS-II)
DEG C surface tension, unit mN/m.
Using Shanghai optical instrument factory WAY-2S type Abbe refractometer, the refractive index n of glass is measured at room temperatureD。
Glass transmitance is measured using ultraviolet-visible spectrophotometer, glass sample takes 308nm with a thickness of 0.5mm respectively
Locate transmitance, unit %.
Hydrofluoric acid corrosion rate refers to that the alkali-free glass substrate of unit area is in the HF that concentration is 10 weight % at 20 DEG C
The weight that 20min loss is impregnated in solution, is denoted as CHF, unit mg/cm2。
Crooked test refers to that three-point bending strength is tested, and thinks carefully Science and Technology Co., Ltd.'s production in length and breadth using Shenzhen
The bending strength tester of WAW-500W model measures.Wherein, glass sample length >=120mm, sheet thickness >
0.1mm, lower support and upperpush rod diameter are 3mm, and lower support span L is 110mm, and glass sheet sample load fall off rate is
10mm/min.Crooked test maximum strain amount εmaxRefer to that glass substrate stress maximal destruction into fracture process strains;Bending
Test maximum stress value σmaxRefer to glass substrate stress maximal destruction stress into fracture process, unit MPa.εmaxWith
σmaxIt is calculated according to the following equation respectively:Wherein, F is maximum when glass sheet sample is broken
Load, unit N;L is lower support span, unit mm;D is maximum displacement when glass sheet sample is broken, unit mm;
B is glass sheet sample width, unit mm;H is glass sheet sample thickness, unit mm.
Embodiment 1-24 and comparative example 1-3
According to the compositing formula of alkali-free glass compositions shown in table 1, each component is mixed, then heats 10 at 1600 DEG C
Hour, and uniform speed slow stirs.The glass metal melted is poured into stainless steel cast iron grinding tool, defined blocky glass is configured to
Glass product, then by glassware corresponding annealing point T in the lehraLower annealing 2 hours closes power supply furnace cooling to 25
℃.Glassware is cut, ground, is polished, is then cleaned up and is dried with deionized water, is made with a thickness of 0.5mm
Glass finished-product.The various performances of each glass finished-product are measured respectively, the results are shown in Table 2.
It can be seen that the glass (such as embodiment 1-23) of glass composition preparation of the present invention by the result of table 1-3
Crooked test maximum stress value σmax≥80MPa;Crooked test maximum strain amount εmax≥1500×10-6, and thermally expand and be
Number is lower, is not higher than 38 × 10-7/ DEG C, the strain point temperature of glass is higher than 650 DEG C, and density is lower than 2.49g/cm3, with comparison
The example glass phase ratio has obvious better performance.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of alkali-free glass compositions, comprising: on the basis of the total weight of alkali-free glass compositions, which contains
The SiO of 58-64wt%2, 16-19wt% Al2O3, 7-13wt% B2O3+P2O5, 0.5-3.5wt% MgO, 4-8wt%
The ZnO of BaO, 0-4wt% of SrO, 0-2.5wt% of CaO, 0.1-4wt%, the R less than 0.05wt%2O, wherein R2O is
Li2O、Na2O、K2The sum of content of O.
2. composition according to claim 1, wherein the glass composition contains the SiO of 61-63wt%2, 17-18wt%
Al2O3, 8.8-11wt% B2O3+P2O5, 1.1-2.7wt% MgO, 5.4-7.7wt% CaO, 1.6-3.6wt%
The ZnO of BaO, 0wt% of SrO, 0wt%, the R less than 0.05wt%2O, wherein R2O is Li2O、Na2O、K2The sum of content of O.
3. composition according to claim 1 or 2, wherein B2O3/(B2O3+P2O5) weight ratio > 0.1;Preferably,
B2O3/(B2O3+P2O5) weight ratio meet 0.8 < B2O3/(B2O3+P2O5)≤1。
4. composition according to claim 1 or 2, wherein R ' O/ (B2O3+P2O5) weight ratio meet 0.5 < R ' O/
(B2O3+P2O5) < 1.9, preferably 0.9 < R ' O/ (B2O3+P2O5) < 1.3, more preferably 1.0 < R ' O/ (B2O3+P2O5) <
1.2, wherein R ' O is the sum of MgO, CaO, SrO, BaO and ZnO content.
5. composition according to claim 1 or 2, wherein the weight ratio of MgO/CaO meets 0.1 < MgO/CaO < 0.9,
Preferably 0.15 < MgO/CaO < 0.5.
6. composition according to claim 1 or 2, wherein SrO/CaO weight ratio meets SrO/CaO > 0.01;Preferably
0.2 < SrO/CaO < 0.6, more preferably 0.3 < SrO/CaO < 0.45.
7. composition according to claim 1 or 2, wherein SiO2+Al2O3The sum of weight content Q > 75wt%;It is preferred that
Ground, Q meet 75wt% < Q < 82wt%, it is highly preferred that 78wt% < Q < 81wt%.
8. glass made of the glass composition described in any one of claim 1-7, the glass is had the following performance:
A. crooked test maximum stress value σmax≥80MPa;And
B. crooked test maximum strain amount εmax≥1500×10-6。
9. glass according to claim 8, wherein the glass has the following performance:
(1) viscosity is the corresponding temperature T of 200 pools200≤ 1630 DEG C,
(2) liquidus temperature TL≤ 1200 DEG C,
(3) strain point TstIt is 650-730 DEG C,
(4) Young's modulus >=72GPa and than modulus >=30GPa/ (g/cm3), and
(5) hydrofluoric acid corrosion rate is 4mg/cm2-6.5mg/cm2;
Preferably, the glass has the following performance:
(1) viscosity is the corresponding temperature T of 200 pools200≤ 1627 DEG C,
(2) liquidus temperature TL≤ 1130 DEG C,
(3) strain point TstIt is 680 DEG C -695 DEG C,
(4) Young's modulus >=73GPa and than modulus >=30.5GPa/ (g/cm3), and
(5) hydrofluoric acid corrosion rate is 4.5mg/cm2-5.3mg/cm2。
10. the application of claim 8,9 glass in display device or solar battery.
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