CN105992749A - Alkali-free glass substrate and method for thinning alkali-free glass substrate - Google Patents
Alkali-free glass substrate and method for thinning alkali-free glass substrate Download PDFInfo
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- CN105992749A CN105992749A CN201480065338.3A CN201480065338A CN105992749A CN 105992749 A CN105992749 A CN 105992749A CN 201480065338 A CN201480065338 A CN 201480065338A CN 105992749 A CN105992749 A CN 105992749A
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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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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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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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
- H10K77/10—Substrates, e.g. flexible substrates
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/133302—Rigid substrates, e.g. inorganic substrates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The present invention relates to an alkali-free glass substrate which has been thinned down by 5 mum or more by means of hydrofluoric acid (HF) etching and has a plate thickness of 0.4 mm or less. This alkali-free glass substrate is composed of predetermined alkali-free glass, and this alkali-free glass substrate after thinning has a specific elastic modulus of 31 MNm/kg or more and a photoelastic constant of 30 nm/MPa/cm or less.
Description
Technical field
The present invention relates to be suitable as various glass substrate for display, photomask glass substrate,
Carry out thinning by the etch processes using Fluohydric acid. (HF) and contained substantially no alkali metal
The alkali-free glass substrate of oxide and the thining method of alkali-free glass substrate.
Background technology
In the past, for various glass substrate for display, the most from the teeth outwards formed metal or
The glass substrate of sull etc., it is desirable to characteristic shown below.
(1), time containing alkali metal oxide, alkali metal ion can spread in thin film and make membrane property
Deterioration, therefore, alkali metal ion to be contained substantially no.
(2) time for making to be exposed to high temperature in thin film formation process, can be by the deformation with glass
Contraction (thermal contraction) suppression produced with the structure stabilization of glass is wanted at bottom line, strain point
High.
(3) the various chemicals that quasiconductor is formed middle use to have sufficient chemical durability.
Particularly buffered hydrofluoric acid (BHF: Fluohydric acid. and the ammonium fluoride to the etching for SiOx, SiNx
Mixed liquor) and the etching of ITO in use the chemical liquids containing hydrochloric acid, the erosion of metal electrode
The various acid (nitric acid, sulphuric acid etc.) of use, the alkali durability to be had of anticorrosive additive stripping liquid controlling in quarter.
(4) internal and surface does not has defect (bubble, brush line, field trash, pit, scar etc.).
In addition to above-mentioned requirements, have also appeared situation as described below in recent years.
(5) lightness of display is required, it is desirable to glass itself is also the glass that density is little.
(6) lightness of display is required, it is desirable to thinning glass substrate.
(7) in addition to non-crystalline silicon (a-Si) type liquid crystal display up to now, hot place has also been made
Reason slightly higher polysilicon (p-Si) the type liquid crystal display of temperature (a-Si: about 350 DEG C → p-Si:350～
550℃)。
(8) improve to accelerate the liter gentleness cooling rate of heat treatment when liquid crystal display makes
Productivity ratio or improve resistance to sudden heating, it is desirable to the glass that the mean thermal expansion coefficients of glass is little.
On the other hand, dry etching is developed, and the requirement to resistance to BHF weakens.In order to make
Resistance to BHF is good, and the many uses of glass up to now contain the B of 6～10 moles of %2O3Glass
Glass.But, B2O3There is the tendency making strain point reduce.As without B2O3Or B2O3Contain
Measure the example of few alkali-free glass, have alkali-free glass as described below.
Patent Document 1 discloses the B containing 0～5 mole of %2O3Glass, but 50～
Mean thermal expansion coefficients at 350 DEG C is more than 50 × 10-7/℃。
The strain point of the alkali-free glass described in patent documentation 2 is high, can carry out based on float glass process
Shaping, it is considered as suitable for the purposes such as base plate for displaying, base board for optical mask.
Prior art literature
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 5-232458 publication
Patent documentation 2: Japanese Unexamined Patent Publication 10-45422 publication
Patent documentation 3: Japan's public table patent 2009-066624 publication again
Summary of the invention
The problem that invention is to be solved
On the other hand, middle-size and small-size liquid crystal display (LCD), organic el display (OELD),
Particularly in the field of the portable display such as mobile device, digital camera, mobile phone, aobvious
Show that the lightness of device, slimming have become important problem.In order to realize glass substrate further
Thinning, widely used following operation: after array light filter bonding process, to glass substrate
Etch processes is implemented on surface, makes thickness of slab thinning (thinning).Such as, following operation is carried out: utilize and contain
The surface of the glass substrate that thickness of slab is 0.4mm～0.7mm is entered by the etching solution having Fluohydric acid. (HF)
Row etch processes (hereinafter referred to as " hydrofluoric acid etch process "), making thickness of slab is 0.1mm～0.4mm
Glass substrate (with reference to patent documentation 3).
In the case of being processed thinning glass substrate by hydrofluoric acid etch, it is desirable to: (1) hydrogen fluorine
Etching speed when acid etching processes wants big；And the glass substrate after (2) etch processes to have
Sufficiently intensity.
But, although there is the solid-phase crystallization method manufacture method as the p-Si TFT of high-quality, but
In order to implement the method, it is desirable to improve strain point further.
It addition, based on technology for making glass, particularly melt, shape in requirement, need fall
The viscosity of low glass, particularly glass viscosity reach 104Temperature T during dPa s4。
It is an object of the invention to solve disadvantages mentioned above, it is provided that strain point is high, viscosity is low, special
It is that glass viscosity reaches 104Temperature T during dPa s4Etching when low, hydrofluoric acid etch processes
Even if even if speed is big, hydrofluoric acid etch process after intensity high thin be not easy to flexure and
Apply stress and be not easy to produce alkali-free glass substrate and the alkali-free glass substrate of the problems such as irregular colour
Thining method.
The method solving problem
The present invention provides a kind of alkali-free glass substrate, and it is for subtract by Fluohydric acid. (HF) etch processes
More than thin 5 μm, thickness of slab is the alkali-free glass substrate of below 0.4mm, above-mentioned alkali-free glass
Glass substrate is following alkali-free glass, thinning after the specific modulus of above-mentioned alkali-free glass substrate be
More than 31MNm/kg, photoelastic constant is below 30nm/MPa/cm.
The strain point of above-mentioned alkali-free glass is 680～735 DEG C, and the evenly heat at 50～350 DEG C is swollen
Swollen coefficient is 30 × 10-7～43 × 10-7/ DEG C, glass viscosity reaches 102Temperature T during dPa s2For
Less than 1710 DEG C, glass viscosity reaches 104Temperature T during dPa s4It it is less than 1310 DEG C, with base
A mole % meter in oxide contains:
MgO+CaO+SrO+BaO is 15.5～21,
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35,
CaO/ (MgO+CaO+SrO+BaO) is less than 0.50, SrO/ (MgO+CaO+SrO+BaO)
It is less than 0.50.
The alkali-free glass substrate of the present invention is by the ring utilizing a diameter of 30mm and R to be 2.5mm
The average failure load measured with ball (BOR) method of the ball of a diameter of 10mm is with thickness of slab 0.4mm
Conversion is preferably more than 300N.
It addition, the present invention provides the thining method of a kind of alkali-free glass substrate, wherein,
Above-mentioned alkali-free glass substrate is following alkali-free glass, by above-mentioned alkali-free glass substrate extremely
When a few interarea is impregnated in the etching solution (25 DEG C, 5%HF aqueous solution) containing Fluohydric acid. (HF)
The stripping quantity of per unit area and unit interval reaches 0.17 (mg/cm2)/minute more than under conditions of,
More than thinning for above-mentioned alkali-free glass substrate 5 μm.
The strain point of above-mentioned alkali-free glass is 680～735 DEG C, and the evenly heat at 50～350 DEG C is swollen
Swollen coefficient is 30 × 10-7～43 × 10-7/ DEG C, glass viscosity reaches 102Temperature T during dPa s2For
Less than 1710 DEG C, glass viscosity reaches 104Temperature T during dPa s4It it is less than 1310 DEG C, with base
A mole % meter in oxide contains:
MgO+CaO+SrO+BaO is 15.5～21,
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35,
CaO/ (MgO+CaO+SrO+BaO) is less than 0.50, SrO/ (MgO+CaO+SrO+BaO)
It is less than 0.50.
Invention effect
The strain point of the alkali-free glass substrate of the present invention is high, and glass viscosity reaches 104During dPa s
Temperature T4Low, etching speed when hydrofluoric acid etch processes is big, hydrofluoric acid etch process after strong
Degree height, is not easy to flexure even if thin, even and if applying stress and be not easy to produce irregular colour etc.
Problem, therefore, is suitable as at middle-size and small-size LCD, OLED, particularly mobile device, number
The thickness of slab used in the field of the portable displays such as code-phase machine, mobile phone is below 0.4mm
Glass sheet substrate.The alkali-free glass substrate of the present invention can also be as glass substrate for disc
Use.
Detailed description of the invention
Hereinafter, the thining method of the alkali-free glass substrate of the present invention is illustrated.
In the thining method of the alkali-free glass substrate of the present invention, use have employed so as under
State the alkali-free glass substrate of frit that the mode of glass composition is allocated.
The strain point of above-mentioned alkali-free glass is 680～735 DEG C, and the evenly heat at 50～350 DEG C is swollen
Swollen coefficient is 30 × 10-7～43 × 10-7/ DEG C, glass viscosity reaches 102Temperature T during dPa s2For
Less than 1710 DEG C, glass viscosity reaches 104Temperature T during dPa s4It it is less than 1310 DEG C, with base
A mole % meter in oxide contains:
MgO+CaO+SrO+BaO is 15.5～21,
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35,
CaO/ (MgO+CaO+SrO+BaO) is less than 0.50, SrO/ (MgO+CaO+SrO+BaO)
It is less than 0.50.
Then the compositing range of each composition is illustrated.SiO2Less than 63% (mole %, below
The most identical) time, strain point cannot fully improve, and thermal coefficient of expansion increases,
Density rises.It is preferably more than 64%, more preferably more than 65%, more preferably 66%
Above, particularly preferably more than 66.5%.It is preferably more than 66.5%, more preferably more than 67%.
During more than 74%, etching speed reduces, and the melting of glass reduces, and devitrification temperature rises.Excellent
Elect less than 70% as, more preferably less than 69%, more preferably less than 68%.
Al2O3Improve Young's modulus, suppress thinning after flexure, and suppress the split-phase of glass,
Reduce thermal coefficient of expansion, improve strain point, destroy toughness value and improve and improve strength of glass, but
During less than 11.5%, not showing this effect, other additionally can be made to increase the composition expanded increases, knot
Really thermal expansion becomes big.Preferably more than 12%, preferably more than 12.5%, more preferably
More than 13%.During more than 16%, the melting of glass may be made to be deteriorated or make in devitrification temperature
Rise.It is preferably less than 15%, more preferably less than 14%, more preferably less than 13.5%.
B2O3The fusing improving glass is reactive, reduces devitrification temperature, improves resistance to BHF, but
This effect of insufficient performance when being less than 1.5%, additionally strain point becomes too high, or is utilizing
Mist degree easily occurs in BHF problem after processing.It is preferably more than 2%, more preferably more than 3%.
But, if crossing photoelastic constant at most to become big, easily produce in the case of being applied with stress
The problems such as irregular colour.It addition, B2O3During more than 5% thinning after surface roughness become big, subtract
Intensity step-down after thin.It addition, strain point reduces, Young's modulus diminishes.Be preferably 4.5% with
Under, more preferably less than 4%.
MgO does not improves proportion and improves Young's modulus, therefore, by improving specific modulus, it is possible to
The problem alleviating flexure.Do not increase expansion it addition, have in alkaline-earth metal and do not make strain point
The feature excessively reduced, also improves melting.Improve it addition, destroy toughness value and improve glass
Intensity.But this effect of insufficient performance during less than 5.5%, additionally other alkaline-earth metal ratios uprise,
Therefore density uprises.Preferably more than 6% and then more than 7%, more preferably more than 7.5%,
More than 8% and then more than 8%, preferably more than 8.1% and then more than 8.3%, particularly preferably
It is more than 8.5%.During more than 13%, devitrification temperature may rise.Preferably less than 12%, more excellent
Elect less than 11% as, particularly preferably less than 10%.
In alkaline-earth metal, CaO is only second to MgO and has raising specific modulus, do not increases expansion,
The feature maintaining relatively low by density and do not make strain point excessively reduce, also improves melting.Low
Will not show in 1.5% time and be added, by above-mentioned CaO, the effect brought.It is preferably more than 2%,
More preferably more than 3%, more preferably more than 3.5%, particularly preferably more than 4%.But
It is, during more than 12%, it is possible to devitrification temperature rises or is mixed into a large amount of as CaO raw material
Limestone (CaCO3Impurity in) i.e. phosphorus.It is preferably less than 10%, more preferably less than 9%,
More preferably less than 8%, particularly preferably less than 7%.
SrO improve melting without making the devitrification temperature of glass raise, but be less than 1.5% time,
Will not fully show this effect.Preferably more than 2%, more preferably more than 2.5%, the most excellent
Elect more than 3% as.But, during more than 9%, coefficient of expansion may increase.Be preferably 7% with
Under, more preferably less than 6%, less than 5%.
BaO is optional, but can contain to improve melting.But, time too much,
Expansion and the density that can make glass excessively increase, and are therefore set as less than 1%.It is preferably less than 1
%, more preferably less than 0.5%, further preferably contain substantially no.Contain substantially no and be
Refer to, do not contain in addition to inevitable impurity.
In order to improve Young's modulus, reduce glass melting temperature or in order to promote knot during calcining
Partial crystallization goes out, can be containing the ZrO of at most 2%2.During more than 2%, glass become unstable or
The relative dielectric constant ε of glass increases.It is preferably less than 1.5%, more preferably less than 1.0%,
More preferably less than 0.5%, particularly preferably contain substantially no.
If MgO, CaO, SrO, BaO are less than 15.5% in terms of total amount, then glass viscosity reaches
104Temperature T during dPa s4Uprise, may extremely shorten the floating shell throwing cellar for storing things when float forming
Body works, the life-span of heater.It addition, etching speed is slack-off, photoelastic constant becomes big,
And melting reduces.It is preferably more than 16%, more preferably more than 17%.If more than 21%,
Then may produce the difficult point that can not reduce thermal coefficient of expansion.Be preferably less than 20%, less than 19%,
And then less than 18%.
Meet above-mentioned by the total amount of MgO, CaO, SrO and BaO and meet following
Condition, can rise high Young's modulus, specific modulus in the case of not raising devitrification temperature, and then
The viscosity of glass, particularly T can be reduced4。
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35, preferably more than 0.37, and more excellent
Elect more than 0.4 as.
CaO/ (MgO+CaO+SrO+BaO) is less than 0.50, preferably less than 0.48, and more excellent
Elect less than 0.45 as.
SrO/ (MgO+CaO+SrO+BaO) is less than 0.50, preferably less than 0.40, and more excellent
Elect less than 0.30 as, more preferably less than 0.27, more preferably less than 0.25.
In the alkali-free glass of the present invention, due to Al2O3×(MgO/(MgO+CaO+SrO+BaO))
Young's modulus can be improved, the most preferably when being more than 4.3.Preferably more than 4.5, more preferably
It is more than 4.7, more preferably more than 5.0.
Na can be added for purposes such as electricity auxiliary heating2O、K2The alkali metal oxides such as O.
If being improved by the content of alkali metal oxide, then alkali metal ion can spread in the film and make film
Deterioration in characteristics, therefore, becomes problem when using as various base plate for displaying glass, but
If the content making the alkali metal oxide in glass composition is below 2000 molar ppm, then it is difficult to
Produce such problem.Below more preferably 1500 molar ppm, below 1300 molar ppm,
Below 1000 molar ppm.
It should be noted that in order to not make to have the alkali-free glass substrate of the present invention manufacturing to use
During display, metal or the sull of being located at glass surface produce deterioration in characteristics, preferably glass
Glass raw material contains substantially no P2O5.Mixed volume as impurity is preferably below 23 molar ppm,
Below more preferably 18 molar ppm, more preferably below 11 molar ppm, the most excellent
Elect below 5 molar ppm as.Additionally, in order to make glass easily recycle, preferably frit
Contain substantially no PbO, As2O3、Sb2O3。
In order to improve the melting of glass, clarification, formability, can be containing 1% in terms of total amount
Below, preferably less than 0.5%, more preferably less than 0.3%, further preferred less than 0.15%, special
The most preferably less than 0.1% ZnO, Fe2O3、SO3、F、Cl、SnO2.Preferably it is substantially free of
ZnO。
The manufacture of the alkali-free glass substrate of the present invention is such as implemented according to following steps.
The raw material of each composition is allocated in the way of reaching target component, it is put into continuously
In fusing stove, it is heated to 1500～1800 DEG C and makes it melt.By this melten glass forming device
It is configured to the glass tape of the tabular of regulation thickness of slab, cuts, thus after this glass tape is annealed
Alkali-free glass substrate can be obtained.
In the present invention, it is the glass tape of tabular preferably by float forming.
In the thining method of the alkali-free glass substrate of the present invention, by two to alkali-free glass substrate
At least one interarea in individual interarea carries out Fluohydric acid. (HF) etch processes, by this alkali-free glass substrate
More than thinning 5 μm.By thinning, it is possible to reduce the thickness of the display using alkali-free glass substrate
Degree, and display lightness can be made.
If the process of obstructed overetch carries out thinning but just uses thin plate, i.e. thickness of slab little from initially
Alkali-free glass substrate, then need greatly in the element manufacturing operation etc. implemented when display manufacturing
Thin plate operate, thus easily produce the carrying obstacle caused by deadweight flexure (such as, because removing
The generation etc. of the scar on substrate that contact during fortune is caused.The most identical), the rupturing of substrate
Etc. problem.More than the most thinning 10 μm, more than the most thinning 100 μm, especially
More than the most thinning 200 μm.
In the thining method of the alkali-free glass substrate of the present invention, thinning after alkali-free glass substrate
Thickness of slab is below 0.4mm.During more than 0.4mm, it is impossible to obtain the lightness of display, slim
The effect changed.More preferably below 0.35mm, more preferably below 0.25mm.
The thickness of slab carrying out thinning front alkali-free glass substrate is preferably more than 0.3mm.If being less than
0.3mm, then need to operate big thin plate in element manufacturing operation etc., thus easily produce
Raw because of the carrying obstacle caused by deadweight flexure, the problem such as rupture.More preferably more than 0.4mm,
Particularly preferably more than 0.45mm.But, if more than 0.75mm, then it is used for the light of display
Type, the thinning required time of slimming likely become long.More preferably 0.65mm
Hereinafter, more preferably below 0.55mm.
Chemical liquids for etch processes uses the chemical liquids comprising Fluohydric acid. (HF).Can also profit
It is etched processing by the chemical liquids of alkalescence, but comprises the etching speed of the chemical liquids of Fluohydric acid. more
Hurry up, and can further smoothly etch.The hydrofluoric acid concentration comprised in chemical liquids is more preferably 1
More than quality %, more preferably more than 3 mass %, more than particularly preferably 5 mass %.
It addition, in addition to Fluohydric acid., preferably add the hydrogen fluorine such as hydrochloric acid, nitric acid, sulphuric acid in chemical liquids
Acid beyond acid.
During etch processes, at least one interarea of alkali-free glass substrate is impregnated into and comprises Fluohydric acid.
Chemical liquids in.The scheduled time is impregnated, thus by alkali-free glass according to the Funing tablet in chemical liquids
Substrate attenuation ormal weight.
In etch processes, preferably the most any by stirring, bubbling, ultrasound wave, spray
More than one method makes chemical liquids flow.Can also utilize shake, rotate in the most any
More than one method makes alkali-free glass substrate move to replace making chemical liquids flow.
In the thining method of the alkali-free glass substrate of the present invention, in 5 mass % that impregnated in 25 DEG C
Time in Fluohydric acid. (HF), as the per unit area of etching speed index and the dissolution of unit interval
Amount reaches 0.17 (mg/cm2)/minute more than under conditions of implement etch processes.If being less than
0.17(mg/cm2)/minute, the most thinning required time likely becomes long.More preferably
0.18(mg/cm2)/minute more than.
By the thinning alkali-free glass substrate of the method for the present invention thinning after intensity high.Specifically
For, by use a diameter of 30mm, R be 2.5mm ring (cross section of ring for circle, R is
The radius of this circle) and ball (BOR) method of ball of a diameter of 10mm (make want to be evaluated one
The table of side is placed face down on ring), to the alkali-free glass substrate after thinning through etch processes one
The average failure load that the interarea (wanting the surface of the side being evaluated) of side is measured is with plate
Thick 0.4mm conversion is preferably more than 300N.Herein, the diameter of ring refers to by cross section
The diameter of a circle of centre, in the case of the ring of diameter 30mm, R=2.5mm, the external diameter of ring
It is 25mm for 35mm, innermost diameter.
It addition, average failure load refers to, the mensuration of breaking load based on BOR method is implemented
The repeatedly meansigma methods of thus obtained measurement result.It addition, in embodiment described later, real
Execute the mensuration of 5 breaking loads based on BOR method, the meansigma methods of their measurement result is made
For average failure load.
If the average failure load measured by BOR method is less than 300N with thickness of slab 0.4mm conversion,
Then the surface strength of alkali-free glass substrate is low, the glass substrate such as during operation when display manufacturing
Rupture etc. and (such as, the alkali-free glass substrate after element manufacturing to be mentioned it with supporting pin etc.
In the operation of class, glass substrate ruptures), thinning after intensity may become problem.More
It is preferably more than 350N.
The thickness of slab conversion utilizing BOR method is carried out according to below step.
In BOR method, square being inversely proportional to of stress and the thickness of slab produced at glass baseplate surface,
Therefore, the thickness of slab of glass substrate is being set to t (mm), the destruction obtained by BOR method is being carried
When lotus is set to w (N), W=w can be passed through with breaking load W (N) of thickness of slab 0.4mm conversion
×0.16/t2Relational expression obtain.
By in the method for present invention alkali-free glass substrate after thinning, thinning after alkali-free glass
The interarea through etch processes side (wanting the surface of the side being evaluated) of substrate based on
The surface strength of three-point bending is preferably more than 500MPa.If less than 500MPa, then will use
Have thinning after the display of alkali-free glass substrate when using as portable display, having can
Can easily produce problems such as rupturing.More preferably more than 800MPa, more preferably
More than 1000MPa, particularly preferably more than 1200MPa, most preferably more than 1500MPa.
The interarea through etch processes side of the alkali-free glass substrate after thinning (is wanted to comment
The surface of the side of valency) surface strength based on three-point bending measure as follows.To comment
Under the state that valency face is protected with sealing member, with chain-dotted line device (point scriber), glass substrate is drawn
Line, after cutting, the sealing member in evaluation face of tearing, by uncrossed side be arranged in the way of lower across
On for three-point bending fixture that 10mm, R are 1.5mm.With the fixture that R is 1.5mm from
The line side extruding of upper surface, breaking load time thus calculates surface based on three-point bending
Intensity.
If there being scar on evaluation face, being then low-intensity, therefore, needing do not contacting after thinning
Maintain under the state in evaluation face.In bend test, in the case of end face exists and destroys starting point,
Then measure is end face strength rather than surface strength, thus when being positioned at face only with starting point
Result of the test, obtains average failure load.
It addition, in this specification, measure average failure load by BOR method or by three-point bending
Environment set during lotus is temperature 22 ± 2 DEG C, humidity 40 ± 10%.
For the alkali-free glass substrate that the method by the present invention is thinning, thinning after alkali-free
The surface roughness of the interarea through etch processes side of glass substrate is 1 μ in AFM measures
Ra square for m is preferably below 0.75nm.If more than 0.75nm, then alkali-free glass substrate
Intensity is likely to decrease.More preferably below 0.7nm.
The strain point of the alkali-free glass substrate of the present invention is more than 680 DEG C and less than 735 DEG C.
Owing to the strain point of the alkali-free glass substrate of the present invention is more than 680 DEG C, therefore can press down
Thermal contraction when panel processed manufactures.It addition, the manufacture method as p-Si TFT can apply profit
By the method for laser annealing.More preferably more than 685 DEG C, more preferably more than 690 DEG C.
Further, since the strain point of the alkali-free glass substrate of the present invention is more than 680 DEG C, therefore
(such as, thickness of slab is below 0.7mm, is preferably below 0.5mm, more to be suitable to high strain-point purposes
It is preferably base plate for displaying or the illumination substrate of organic EL of below 0.3mm, or
Thickness of slab is base plate for displaying or the illumination of below 0.3mm, the preferably thin plate of below 0.1mm
With substrate).
Due to thickness of slab be below 0.7mm, further for below 0.5mm, further for 0.3mm
It is in the shaping of glass sheet of below 0.1mm there to be pull-out speed during shaping below, further
The tendency accelerated, therefore the fictive temperature of glass easily rises, the compression (compaction) of glass
Easily increase.Now, if high strain-point glass, then compression can be suppressed.
On the other hand, if strain point is less than 735 DEG C, then without by floating throwing cellar for storing things and floating throwing cellar for storing things
The temperature of outlet arranges get Tai Gao, is pointed in floating throwing is stored and the hardware in downstream is stored in floating throwing
Life-span produce impact few.More preferably less than 725 DEG C, more preferably less than 715 DEG C,
Particularly preferably less than 710 DEG C.
Further, since the plane strain of glass improves, it is therefore desirable to throwing cellar for storing things outlet entrance from floating
The part of annealing furnace improves temperature, but without temperature now is arranged get Tai Gao.Therefore, no
Can cause load to adding the heater hankering using, the impact on the life-span generation of heater is few.
It addition, order the same reason for strain, the glass of the alkali-free glass substrate of the present invention
Change transition temperature and be preferably more than 730 DEG C, more preferably more than 740 DEG C, more preferably
More than 750 DEG C.Additionally, it is preferred that be less than 780 DEG C, more preferably less than 775 DEG C, special
You Xuanwei less than 770 DEG C.
Additionally the alkali-free glass substrate of present invention mean thermal expansion coefficients at 50～350 DEG C is
30×10-7～43 × 10-7/ DEG C, resistance to sudden heating is big, can improve productivity ratio when panel manufactures.
In the alkali-free glass substrate of the present invention, the mean thermal expansion coefficients at 50～350 DEG C is preferably
35×10-7/ DEG C more than.Mean thermal expansion coefficients at 50～350 DEG C is preferably 42 × 10-7/ DEG C with
Under, more preferably 41 × 10-7/ DEG C below, more preferably 40 × 10-7/ DEG C below.
Further, the proportion of the alkali-free glass substrate of the present invention is preferably less than 2.62, more preferably
It is less than 2.60, more preferably less than 2.58.
It addition, the viscosities il of the alkali-free glass substrate of the present invention is 102Temperature during pool (dPa s)
T2It is less than 1710 DEG C, more preferably less than 1700 DEG C, more preferably less than 1690 DEG C,
Particularly preferably less than 1680 DEG C, less than 1670 DEG C, therefore fusing is easier to.
Further, the viscosities il of the alkali-free glass substrate of the present invention is 104Temperature T during pool4For
Less than 1310 DEG C, preferably less than 1305 DEG C, more preferably less than 1300 DEG C, further preferably
For less than 1300 DEG C, less than 1295 DEG C, less than 1290 DEG C, be suitable to float forming.
It addition, for shaping transfiguration based on float glass process easily, the alkali-free glass substrate of the present invention
Devitrification temperature is preferably less than 1315 DEG C.Be preferably less than 1300 DEG C, less than 1300 DEG C, 1290 DEG C
Hereinafter, more preferably less than 1280 DEG C.It addition, become float forming, the ginseng of fusion formability
Examine temperature T of value4(glass viscosity η is 104Temperature during pool, unit: DEG C) with devitrification temperature it
Difference (T4-devitrification temperature) it is preferably more than-20 DEG C, more than-10 DEG C, it is more than 0 DEG C further, more
It is preferably more than 10 DEG C, more preferably more than 20 DEG C, particularly preferably more than 30 DEG C.
Devitrification temperature in this specification refers to, add by platinum ware pulverize glass particle,
Control the electric furnace for uniform temperature carries out 17 hours heat treatments, shown by the optics after heat treatment
Micro mirror observation, separates out the maximum temperature of crystallization on the surface of glass and inside and does not separate out crystallization
The meansigma methods of minimum temperature.
It addition, the specific modulus of the alkali-free glass substrate of the present invention is more than 31MNm/kg.If it is low
In 31MNm/kg, then easily produce cause because deadweight flexure carrying obstacle, the problem such as rupture.
It is preferably more than 32MNm/kg, more preferably more than 33MNm/kg.
It addition, the Young's modulus of the alkali-free glass substrate of the present invention is preferably more than 78GPa, more
It is preferably more than 79GPa, more than 80GPa and then more than 81GPa, more preferably 82GPa
Above.
It addition, the photoelastic constant of the alkali-free glass substrate of the present invention is preferably 30nm/MPa/cm
Below.
The stress produced when panel of LCD manufacturing process, LCD device use
Glass substrate can be made to have birefringence, the most sometimes observe that black display becomes Lycoperdon polymorphum Vitt, liquid
The phenomenon that the contrast of crystal display reduces.By photoelastic constant is set to
Below 30nm/MPa/cm, can suppress less by this phenomenon.It is preferably 29nm/MPa/cm
Hereinafter, more preferably below 28.5nm/MPa/cm, more preferably 28nm/MPa/cm with
Under.
It addition, for the alkali-free glass substrate of the present invention, if considering to guarantee the appearance of other physical property
Yi Xing, photoelastic constant is preferably more than 23nm/MPa/cm, more preferably 25nm/MPa/cm
Above.
It should be noted that can measure photoelastic at mensuration wavelength 546nm by disk compression method
Property constant.
It addition, the relative dielectric constant of the alkali-free glass substrate of the present invention is preferably more than 5.6.
The touch panel of described such interior insert-type in Japanese Unexamined Patent Publication 2011-70092 publication
In the case of (being provided with touch inductor in panel of LCD), from the sense of touch inductor
From the viewpoint of answering the raising of sensitivity, the reduction of driving voltage, saving power, glass substrate
Relative dielectric constant be advisable with higher.By relative dielectric constant is set to more than 5.6, touch
The induction sensitivity touching induction apparatus improves.It is preferably more than 5.8, more preferably more than 6.0, enters
One step is preferably more than 6.2, and particularly preferably more than 6.4.
It should be noted that relative dielectric can be measured by the method described in JIS C-2141
Constant.
The alkali-free glass substrate of the present invention amount of contraction when heat treatment is preferably less.Liquid crystal surface
During plate manufactures, different from color filter side heat treatment step in array side.Therefore, particularly at height
In fine panel, when the percent thermal shrinkage of glass is big, exists and asking of the skew put occurs when chimeric
Topic.It should be noted that the evaluation of percent thermal shrinkage can be measured according to following order.
After sample being kept 10 minutes at a temperature of glass transition temperature+100 DEG C, with per minute
40 DEG C are cooled to room temperature.Herein, the total length measuring sample (is set to L0).Then, with per hour
100 DEG C are heated to 600 DEG C, keep 80 minutes at 600 DEG C, with per hour 100 DEG C of coolings
To room temperature, again measure the total length of sample, measure the receipts of sample before and after the heat treatment of 600 DEG C
Contracting amount (is set to Δ L).Ratio (Δ L/L by the sample total length before heat treatment with amount of contraction0) it is set to heat receipts
Shrinkage.In above-mentioned evaluation methodology, percent thermal shrinkage is preferably below 100ppm, more preferably 80ppm
Hereinafter, more preferably below 60ppm, be below 55ppm further, particularly preferably
Below 50ppm.
Embodiment
(embodiment 1～6, comparative example 1,2)
The raw material of each composition is allocated in the way of becoming the composition of target shown in table 1, utilizes
Melting furnaces melt continuously, carry out plate forming by float glass process, obtain alkali-free glass substrate.
After obtained glass substrate is carried out mirror ultrafinish, by utilize 8 mass % Fluohydric acid .s,
The mixed acid of 10 mass % hydrochloric acid carries out the etching of the one side of glass substrate while carrying out bubbling
Process so that thickness of slab becomes 0.4mm from 0.7mm, thus carries out thinning.
Use thinning after glass substrate, by using a diameter of 30mm, R=2.5mm
Ball (BOR) method of the SUS ball of SUS ring and a diameter of 10mm is implemented 5 times to destroy to carry
The mensuration of lotus, carries the average failure with thickness of slab 0.4mm conversion obtained by these measurement results
Lotus is shown in Table 2.
It addition, obtained at by step similar to the above by thickness of slab etching by following method
Manage in the case of 30 μm, the surface roughness in etch processes face.Show the result in following table
In 2.
[assay method of surface roughness based on AFM]
For the etch processes face of glass substrate, Park Systems company is utilized to manufacture
XE-HDM, is set as 1Hz by sweep speed, obtains the surface roughness Ra that 1 μm is square.
Further, the index of etching speed when processing as hydrofluoric acid etch, according to following
When step to being impregnated into 25 DEG C, in the hydrofluoric acid aqueous solution of 5 mass % by alkali-free glass substrate
The stripping quantity of per unit area and unit interval is evaluated.Show the result in table 2.Include
Number represent value of calculation.
[assay method of the stripping quantity of per unit area and unit interval]
To being cut into after alkali-free glass substrate square for 40mm is carried out through mirror ultrafinish,
Quality measurement.The 5 mass % Fluohydric acid .s of 25 DEG C impregnate 20 minutes, measures the matter after dipping
Amount.Calculated surface area by sample size, by Mass lost amount divided by surface area after, then divided by
Dip time, thus obtains the stripping quantity of per unit area and unit interval.
It should be noted that about the alkali-free glass substrate obtained by above-mentioned steps, also measure
Strain point, Young's modulus, specific modulus, photoelastic constant, relative dielectric constant.By result
It is shown in Table 2.
[table 1]
[table 2]
Describe the present invention in detail above and with reference to specific embodiment, but not
Depart from the scope of the present invention and can make various changes and modifications in the case of spirit, this for
It is apparent from for those skilled in the art.
The Japanese patent application 2013-246801 that the application proposed based on November 28th, 2013,
Its content is incorporated in this specification with the form of reference.
Claims (3)
1. an alkali-free glass substrate, it is for be thinned 5 μm by Fluohydric acid. (HF) etch processes
Above, thickness of slab is the alkali-free glass substrate of below 0.4mm, under described alkali-free glass substrate is
State alkali-free glass, thinning after the specific modulus of described alkali-free glass substrate be more than 31MNm/kg,
Photoelastic constant is below 30nm/MPa/cm,
The strain point of described alkali-free glass is 680～735 DEG C, and the evenly heat at 50～350 DEG C is swollen
Swollen coefficient is 30 × 10-7～43 × 10-7/ DEG C, glass viscosity reaches 102Temperature T during dPa s2For
Less than 1710 DEG C, glass viscosity reaches 104Temperature T during dPa s4It it is less than 1310 DEG C, with base
A mole % meter in oxide contains:
MgO+CaO+SrO+BaO is 15.5～21,
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35, CaO/ (MgO+CaO+SrO+
BaO) being less than 0.50, SrO/ (MgO+CaO+SrO+BaO) is less than 0.50.
2. alkali-free glass substrate as claimed in claim 1, wherein, described alkali-free glass substrate
By utilizing the ball of the ball of ring that a diameter of 30mm and R is 2.5mm and a diameter of 10mm
(BOR) the average failure load that method measures is scaled more than 300N with thickness of slab 0.4mm.
3. a thining method for alkali-free glass substrate, wherein,
Described alkali-free glass substrate is following alkali-free glass, by described alkali-free glass substrate extremely
When a few interarea is impregnated in the etching solution (25 DEG C, 5%HF aqueous solution) containing Fluohydric acid. (HF)
The stripping quantity of per unit area and unit interval reaches 0.17 (mg/cm2)/minute more than under conditions of,
More than thinning for described alkali-free glass substrate 5 μm,
The strain point of described alkali-free glass is 680～735 DEG C, and the evenly heat at 50～350 DEG C is swollen
Swollen coefficient is 30 × 10-7～43 × 10-7/ DEG C, glass viscosity reaches 102Temperature T during dPa s2For
Less than 1710 DEG C, glass viscosity reaches 104Temperature T during dPa s4It it is less than 1310 DEG C, with base
A mole % meter in oxide contains:
MgO+CaO+SrO+BaO is 15.5～21,
MgO/ (MgO+CaO+SrO+BaO) is more than 0.35, CaO/ (MgO+CaO+SrO+
BaO) being less than 0.50, SrO/ (MgO+CaO+SrO+BaO) is less than 0.50.
Applications Claiming Priority (3)
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| JP2013-246801 | 2013-11-28 | ||
| JP2013246801 | 2013-11-28 | ||
| PCT/JP2014/081293 WO2015080171A1 (en) | 2013-11-28 | 2014-11-26 | Alkali-free glass substrate and method for thinning alkali-free glass substrate |
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| CN105992749B CN105992749B (en) | 2020-11-03 |
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| JP (1) | JP6447510B2 (en) |
| KR (1) | KR102249898B1 (en) |
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| CN111757856A (en) * | 2018-02-22 | 2020-10-09 | 康宁股份有限公司 | Alkali-free borosilicate glass with low post-HF-etch roughness |
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| KR20230148860A (en) * | 2014-11-28 | 2023-10-25 | 에이지씨 가부시키가이샤 | Liquid crystal display panel |
| JP6813023B2 (en) * | 2016-04-05 | 2021-01-13 | Ａｇｃ株式会社 | Glass plate structure |
| CN106746601B (en) * | 2016-12-30 | 2019-06-04 | 东旭集团有限公司 | It is used to prepare the composition, glassware and purposes of glass |
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| JP2000302475A (en) * | 1999-04-12 | 2000-10-31 | Carl Zeiss:Fa | Aluminosilicate glass not containing alkali, and its use |
| CN102076625A (en) * | 2008-06-25 | 2011-05-25 | 旭硝子株式会社 | Method for etching alkali-free glass substrate and display device |
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| EP1996525B1 (en) * | 2006-02-10 | 2019-05-22 | Corning Incorporated | Glass compositions having high thermal and chemical stability and methods of making thereof |
| KR20090066624A (en) | 2007-12-20 | 2009-06-24 | 주식회사 엘지화학 | Thermaplastic flame retardant resin composition improved scratch resistance |
| JP5712922B2 (en) * | 2009-07-02 | 2015-05-07 | 旭硝子株式会社 | Alkali-free glass and production method |
| CN103429547A (en) * | 2011-12-28 | 2013-12-04 | 安瀚视特控股株式会社 | Glass substrate for flat panel displays and method for manufacturing same |
| EP3444229A1 (en) * | 2012-12-21 | 2019-02-20 | Corning Incorporated | Glass with improved total pitch stability |
| JP2017007870A (en) * | 2013-11-13 | 2017-01-12 | 旭硝子株式会社 | Manufacturing method of sheet glass |
| JP2017030976A (en) * | 2013-12-04 | 2017-02-09 | 旭硝子株式会社 | Finish polishing method of glass substrate and non-alkali glass substrate finish polished by such method |
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- 2014-11-26 KR KR1020167013811A patent/KR102249898B1/en active IP Right Grant
- 2014-11-26 WO PCT/JP2014/081293 patent/WO2015080171A1/en active Application Filing
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| JPH09263421A (en) * | 1996-03-28 | 1997-10-07 | Asahi Glass Co Ltd | Alkali-free glass and flat display panel |
| JP2000302475A (en) * | 1999-04-12 | 2000-10-31 | Carl Zeiss:Fa | Aluminosilicate glass not containing alkali, and its use |
| CN102076625A (en) * | 2008-06-25 | 2011-05-25 | 旭硝子株式会社 | Method for etching alkali-free glass substrate and display device |
| JP2012082130A (en) * | 2010-10-06 | 2012-04-26 | Corning Inc | Alkali-free glass composition having high thermal and chemical stability |
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| CN111757856A (en) * | 2018-02-22 | 2020-10-09 | 康宁股份有限公司 | Alkali-free borosilicate glass with low post-HF-etch roughness |
| CN111757856B (en) * | 2018-02-22 | 2023-08-22 | 康宁股份有限公司 | Alkali-free borosilicate glass with low HF post-etch roughness |
Also Published As
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| TWI639571B (en) | 2018-11-01 |
| JPWO2015080171A1 (en) | 2017-03-16 |
| KR102249898B1 (en) | 2021-05-11 |
| TW201529518A (en) | 2015-08-01 |
| CN105992749B (en) | 2020-11-03 |
| JP6447510B2 (en) | 2019-01-09 |
| WO2015080171A1 (en) | 2015-06-04 |
| KR20160091332A (en) | 2016-08-02 |
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