CN102815859A - Tempered glass and manufacturing method thereof, measuring method for surface stress of tempered glass - Google Patents

Tempered glass and manufacturing method thereof, measuring method for surface stress of tempered glass Download PDF

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Publication number
CN102815859A
CN102815859A CN2012101745879A CN201210174587A CN102815859A CN 102815859 A CN102815859 A CN 102815859A CN 2012101745879 A CN2012101745879 A CN 2012101745879A CN 201210174587 A CN201210174587 A CN 201210174587A CN 102815859 A CN102815859 A CN 102815859A
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glass
compressive stress
chilled
painted opaque
transparent
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CN102815859B (en
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久野一秀
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AGC Inc
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Asahi Glass Co Ltd
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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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Abstract

The present invention provides tempered glass, wherein the compressive strength of the tempered glass having a low transmittance, a colored opaque portion in the visible light region can be calculated in a non-destructive manner and a manufacturing method thereof, and provides a measuring method for the surface stress of the tempered glass. The tempered glass of the present invention is formed by integrating a colored opaque glass and a transparent glass layer, and then forming a compressive stress layer on the surface of the integrated glass to form the tempered glass.

Description

The surface stress measuring method of chilled glass and method of manufacture thereof, this chilled glass
Technical field
The present invention relates to painted opaque glass and transparent glass range upon range of to carry out integrated chilled glass that forms and method of manufacture thereof.In addition, the invention still further relates to painted opaque glass and transparent glass range upon range of to carry out the surface stress measuring method of the integrated chilled glass that forms.
Background technology
For intelligent terminal such as smart mobile phone and LCD (Liquid Crystal Display: liquid-crystal display) framework of the electronics of watch-dog such as, consider that from the angle of processibility and cost normally used is resin or metal., in recent years, require the situation of designability to increase gradually, begin to attempt the starting material (patent documentation 1) of present original glass as framework to framework.According to patent documentation 1, in electronicss such as mobile phone,, think and to bring into play unique decorative effect with transparent feel through forming the framework main body with glass.
Electronics possesses display unit such as liquid crystal panel at the outside surface of equipment.Display unit has the tendency of high meticulous, high brightnessization, accompanies with it, and the tendency of high brightnessization is also arranged as the backlight of light source.Except shining display device side, also can arrive the back side of the framework that is installed in the outside from the light of light source at the device interior multiple reflection.Can not cause problem when using metal, but when using aforesaid glass, might see through framework, arrived by the slave unit visual observation from the light of light source with transparency as the starting material of framework.Therefore, when glass is used for framework, consider to make it have opacifying property with glass self is painted.
In addition, particularly for the electronics that can portably use, breakage that the fall impacting when considering by use causes and the contact wound that causes by long use, and require framework to have HS.
As the method that improves glass intensity, the general known method that forms compressive stress layers at glass surface.As the method that forms compressive stress layers at glass surface, representative method is: the air-cooled reinforcement (physical strengthening method) that will be heated near the glass pane surface cool quickly the softening temperature through air-cooled grade; And under the temperature below the second-order transition temperature through IX; The alkalimetal ion that the ionic radius of glass pane surface is little (being typically Li ion, Na ion) is exchanged for the chemical enhanced method of the bigger alkali ion of ionic radius (being typically for Li IX is Na ion or K ion, is the K ion for Na IX).
, for through forming the glass that compressive stress layers get, in qualitative control, be that the amount of compressive stress that purpose is measured compressive stress layers is important to confirm to possess intensity more than certain at above-mentioned glass surface.
The method of measuring surface compression stress as the amount of compressive stress of glass (below be also referred to as CS) and the surface compression stressor layers degree of depth (below be also referred to as DOL) with nondestructive mode is suggested and by practicability (for example, patent documentation 2).This measuring method has utilized following principle: owing to the compressive stress layers that forms at glass surface and other glass part different optical waveguides effects that show on specific refractory power that do not have compressive stress layers.
The prior art document
Patent documentation
Patent documentation 1: Japanese Patent Laid is opened the 2009-61730 communique
Patent documentation 2: Japanese Patent Laid is opened clear 53-136886 communique
Summary of the invention
Invent technical problem to be solved
; Measure the said apparatus of CS and DOL owing to be the light of propagating at the upper layer of glass to be penetrated observe with non-failure mode, so newly occurred the painted and problem that the low painted opaque glass of the transsmissivity in the visible region that make it have opacifying property can't be measured of above-mentioned glass self.Under this situation; Needing flexural strength to reach with the test such as (crack ignition load) destructive strength detection of crack initiation load and be used to measure birefringent sample processes; In the chemically reinforced glass; Except use EPMA (Electron Probe Micro Analyzer: electro-probe micro analyzer) and ESCA (Electron Spectroscopy for Chemical Analysis: the diffusion layer degree of depth etc. of ESCA) measuring potassium expends the method in man-hour very much; Do not measure the method for the amount of compressive stress of glass, and the precision of determination data is also low, lacks safety.
The purpose of this invention is to provide range upon range of, the chilled glass then strengthened integrated of painted opaque glass and transparent glass and the surface stress measuring method of method of manufacture and this chilled glass thereof to carry out.
The technical scheme that the technical solution problem is adopted
Chilled glass of the present invention is that painted opaque glass and transparent glass is range upon range of integrated to carry out, and the surface of the glass after integrated forms the chilled glass that compressive stress layers forms again.
In addition; Surface stress measuring method as the glass of another invention of the present invention is that painted opaque glass and transparent glass is range upon range of integrated to carry out; Be determined at the method for the amount of compressive stress of the compressive stress layers that the surface of the chilled glass after integrated forms, use the measured value of the amount of compressive stress of above-mentioned transparent glass part to calculate above-mentioned painted opaque glass part or the whole amount of compressive stress of above-mentioned chilled glass.
The method of manufacture of chilled glass of the present invention is for range upon range of to carry out the method for manufacture of the integrated chilled glass that forms with painted opaque glass and transparent glass; It is characterized in that; The amount of compressive stress of the compressive stress layers of the transparent glass part through measuring above-mentioned chilled glass is managed painted opaque glass part or the whole amount of compressive stress of chilled glass.
The effect of invention
According to the present invention; Even the part has low opaque the painted chilled glass of transsmissivity in the visible region; Also can calculate painted opaque glass part or the whole amount of compressive stress of chilled glass with nondestructive mode through measuring the amount of compressive stress of transparent part.
The simple declaration of accompanying drawing
Fig. 1 is the vertical view and the sectional view of a kind of implementation method of chilled glass of the present invention.
Fig. 2 is the vertical view and the sectional view of other implementation methods of chilled glass of the present invention.
Embodiment
Below, the present invention will be described.
Vertical view of the implementation method of chilled glass of the present invention shown in Fig. 1, Fig. 2 (a) and sectional view (b).In addition, (b) sectional view for the figure along the cross section of X-X direction in (a) vertical view is shown.Chilled glass 1 of the present invention is that painted opaque glass 10 and transparent glass 20 is range upon range of to carry out the integrated chilled glass that forms.As chilled glass of the present invention carry out range upon range of with incorporate form; Can be the form that the mode to surround columned transparent glass as shown in Figure 1 disposes painted opaque glass, perhaps as shown in Figure 2 with painted opaque glass and transparent glass range upon range of along the thickness of slab direction be lamellated form.In addition, as long as can painted opaque glass and transparent glass is integrated, then be not limited to above-mentioned form.
In addition, painted opaque glass of the present invention is meant through making wittingly and contains the glass that coloring components makes transsmissivity become lower than transparent glass in the glass.And, be meant owing to transsmissivity is low to be difficult to decide the glass of surface compression stress and surface compression layer depth with existing glass surface stress instrumentation.Better be glass, and the minimum value of the specific absorbance under the wavelength of 550nm～650nm is greater than 1.7mm with opacifying property -1In addition, transparent glass is meant the glass with light transmission, and better is that the peak of the specific absorbance under the wavelength of 550nm～650nm is lower than 1.7mm -1
Chilled glass of the present invention uses as the painted opaque glass framework of installing in for example electronics outside.
The outer surface of the mobile structure is such that: on the side of the surface configuration of a liquid crystal panel or an organic EL device and a display constituted by the key operation means, such as a touch screen or the configuration of the display device and the operation of such means is formed as one unit, and in its surrounding frame material surrounds (Japanese: the amount of green material).The face of opposite opposite side is made up of panel.And, partly there is the frame material at thickness as the equipment between the face of the face of a side and opposite side.These picture frame materials and frame material or panel and frame material also constitute one sometimes.
Painted opaque glass framework can be used as above-mentioned picture frame material, panel, frame material.In addition, as the shape of painted opaque glass framework, can be tabular, also can be picture frame material and frame material or panel and frame material the form as one concavity or the convex of structure.
Light source in the display unit of the set inside of electronics is made up of the light source that photodiode, organic EL, CCFL etc. send white light.Therefore, require painted opaque glass framework to have opacifying property so that this white light not can through painted opaque glass framework escape to equipment the outside, arrived by the slave unit visual observation.
The white light of light source is for being familiar with the light as white after using fluor with the multi-wavelength's of visible region photorecombination.Therefore, better be that glass contains coloring components, so that the specific absorbance under the wavelength of 380nm～780nm reaches 1mm in entire area -1More than.Through the specific absorbance under the wavelength that makes the visible region is 1mm -1More than, can under the situation that shade is not set in addition, absorb white light with the glass monomer, obtain enough opacifying propertys as painted opaque glass framework.The specific absorbance of glass under the wavelength of 380nm～780nm is lower than 1mm in entire area -1The time, even be glass, also can't obtain required opacifying property with adequate thickness with regard to the framework purposes, light might see through painted opaque glass framework.In addition, when painted opaque glass framework was configured as concavity or convex, at the thickness thinnest part, light might see through.During the thin thickness of painted opaque glass framework, the specific absorbance of the glass under the wavelength of 380nm～780nm is preferably 2mm in entire area -1More than, better be 3mm -1More than, be 4mm better further -1More than.
The method of calculation of above-mentioned specific absorbance are as follows.Mirror ultrafinish is carried out on two sides to sheet glass, measures thickness t.Measure the spectral-transmission favtor T (for example, using the ultraviolet-visible near infrared spectrometer V-570 of Japanese beam split Co., Ltd. system) of this sheet glass.Then, use relational expression T=10 -β tCalculate specific absorbance β.
In order to give glass with above-mentioned opacifying property; Better be to use such glass: as the coloring components in the glass; Molar percentage with the oxide compound benchmark representes, contains at least a kind of composition of 0.1～7% the MOX that is selected from Co, Mn, Fe, Ni, Cu, Cr, V, Bi.In addition, under the situation of using multiple coloring components, this content is represented their total amount.These coloring components are to make glass ribbon that the composition of required color arranged, and adopt the material of the effect of the light with the wavelength that absorbs above-mentioned visible region.If the coloring components in the glass is lower than 0.1%, even be glass then, also can't obtain opacifying property with adequate thickness with regard to the framework purposes, light might see through painted opaque glass framework.Better be that coloring components in the glass is more than 0.5%, the coloring components that is typically in the glass is more than 1%.In addition, if tinting material surpasses 7%, then glass might become unstable.Better be that tinting material is below 6.5%, being typically tinting material is below 6%.Painted opaque glass framework can suitably be selected the content of the coloring components in the glass according to thickness, so that the light of electronic equipment internal does not see through glass with shape etc. and thickness is different.
For example, for the coloring components in the glass, through containing 1.5～6% Fe 2O 3, 0.1～1% Co 3O 4Combination, can process abundant absorbing wavelength and be the light in the visible region of 380nm～780nm, and absorb the glass of the light in the visible region fifty-fifty.In other words, obtain in desire under the situation of glass of black in color,, become sometimes and be brown, blueness or green black because coloring components makes that the absorption characteristic of specific wavelength is low.Relative with it, through adopting above-mentioned coloring components, can show as so-called pitch-dark.As the combination of the coloring components except that above-mentioned that can obtain this characteristic, 0.01～4% Fe can give an example 2O 3, 0.2～3% Co 3O 4, 1.5～6% NiO combination; 1.5～6% Fe 2O 3, 0.1～1% NiO combination; 0.01～4% Fe 2O 3, 0.05～2% Co 3O 4, 0.05～2% NiO, 0.05～2% Cr 2O 3Combination; 0.01～4% Fe 2O 3, 0.05～2% Co 3O 4, 0.05～2% NiO, 0.05～2% MnO combination etc.
Painted opaque glass and transparent glass then can be the glass of any composition so long as can form the glass of compressive stress layers with air-cooled reinforcement or chemical enhanced method on the surface of glass.As the method that forms compressive stress layers on the surface of glass, when using chemical enhanced method,, then can obtain to have high-intensity glass if use following glass as glass or transparent glass beyond the coloring components of painted opaque glass, thereby preferred.
Ideal glass is to represent with the accurate molar percentage of following oxide-base, contains 55～80% SiO 2, 3～16% Al 2O 3, 0～12% B 2O 3, 5～16% Na 2O, 0～4% K 2O, 0～15% MgO, 0～3% CaO, 0～18% ∑ RO (R is Mg, Ca, Sr, Ba, Zn), 0～1% ZrO 2
Below, for the composition of above-mentioned glass, as be not particularly limited, then use molar percentage to represent that its content describes.
SiO 2Being the composition that forms the glass skeleton, is neccessary composition.If SiO 2Be lower than 55%, then as the stability decreases of glass, perhaps weathering resistance descends.Better be SiO 2Be more than 60%.Be more preferably SiO 2Be more than 65%.
If SiO 2Surpass 80%, then the viscosity of glass increases, and meltbility significantly descends.Better be SiO 2Be below 75%, to be typically SiO 2Be below 70%.
Al 2O 3Being to improve the weathering resistance of glass and the composition of chemical enhanced characteristic, is neccessary composition.If Al 2O 3Be lower than 3%, then weathering resistance descends.Better be Al 2O 3Be more than 4%, to be typically Al 2O 3Be more than 5%.
If Al 2O 3Surpass 16%, then the viscosity of glass uprises, and is difficult to fusion in heterogeneity.Better be Al 2O 3Be below 14%, to be typically Al 2O 3Be below 12%.
B 2O 3Being the composition that improves the weathering resistance of glass, is not neccessary composition, can contain as required.Contain B 2O 3The time, if be lower than 4%, then might can't obtain obvious effects for improving weathering resistance.Better be B 2O 3Be more than 5%, to be typically B 2O 3Be more than 6%.
If B 2O 3Surpass 12%, then might produce the brush line that causes by volatilization, make decrease in yield.Better be B 2O 3Be below 11%, to be typically B 2O 3Be below 10%.
Na 2O is the composition of raising glass melting property, and is used for forming the surface compression stressor layers through IX, is neccessary composition.If Na 2O less than 5%, then meltbility is poor, and is difficult to form required surface compression stressor layers through IX.Better be Na 2O more than 7%, is typically Na 2O is more than 8%.
If Na 2O surpasses 16%, and then weathering resistance descends.Better be Na 2O below 15%, is typically Na 2O is below 14%.
K 2O is the composition that improves glass melting property, and has the effect that increases the ion-exchange speed in chemical enhanced, though be not neccessary composition therefore, is the composition that preferably contains.Contain K 2During O,, then might obvious effects can't be obtained, perhaps obvious effects can't be obtained for improving ion-exchange speed for improving meltbility if be lower than 0.01%.Be typically K 2O is more than 0.3%.
If K 2O surpasses 4%, and then weathering resistance descends.Better be K 2O below 3%, is typically K 2O is below 2%.
MgO is the composition that improves glass melting property, is not neccessary composition, can contain as required.When containing MgO,, then obvious effects might can't be obtained for improving meltbility if be lower than 3%.Being typically MgO is more than 4%.
If MgO surpasses 15%, then weathering resistance descends.Better be that MgO is below 13%, being typically MgO is below 12%.
CaO is the composition that improves glass melting property, can contain as required.When containing CaO,, then obvious effects might can't be obtained for improving meltbility if be lower than 0.01%.Being typically CaO is more than 0.1%.
If CaO surpasses 3%, then chemical enhanced characteristic descends.Better be that CaO is below 1%, being typically CaO is below 0.5%, is more preferably not contain CaO in fact.
RO (R is Mg, Ca, Sr, Ba, Zn) is the composition that improves glass melting property, is not neccessary composition, can contain any more than a kind as required.Under this situation, the total ∑ RO of the content of RO (R is Mg, Ca, Sr, Ba, Zn) then might meltbility descend if be lower than 1%.Better be that ∑ RO is more than 3%, being typically ∑ RO is more than 5%.
If ∑ RO (R is Mg, Ca, Sr, Ba, Zn) surpasses 18%, then weathering resistance descends.Better be that ∑ RO is below 15%, being more preferably ∑ RO is below 13%, and being typically ∑ RO is below 11%.
ZrO 2Being the composition that increases ion-exchange speed, is not neccessary composition, can contain in the scope that is lower than 1%.If ZrO 2 Surpass 1%, meltbility variation then might take place to residue in the situation in the glass as melts not.Be typically and do not contain ZrO 2
(SiO 2+ Al 2O 3+ B 2O 3)/(∑ R 2The O+CaO+SrO+BaO+ coloring components) expression forms the ratio of total amount of total amount and main modified oxide of mesh-shape oxide compound of the network of glass; If this ratio is lower than 4, the destructive probability when then after chemical enhanced processing, imposing impression might become big.Better be that this ratio is more than 4.2, being typically this ratio is more than 4.4.If this ratio surpasses 6, the then viscosity of glass increase, meltbility descend.Better be that this ratio is below 5.5, being more preferably this ratio is below 5.In addition, ∑ R 2O representes Na 2O, K 2O, Li 2The total amount of O.
SO 3Being the composition that plays a role as finings, is not necessary composition, can contain as required.Contain SO 3The time, if be lower than 0.005%, the clarification that then can't obtain to expect.Better be SO 3Be more than 0.01%, to be more preferably SO 3Be more than 0.02%.SO preferably 3Be more than 0.03%.In addition, if SO 3Surpass 0.5%, then can become the generation source of bubble on the contrary, might make the burn through of glass slack-off, the bubble number increases.Better be SO 3Be below 0.3%, to be more preferably SO 3Be below 0.2%.SO preferably 3Be below 0.1%.
SnO 2Being the composition that plays a role as finings, is not necessary composition, can contain as required.Contain SnO 2The time, if be lower than 0.005%, the clarification that then can't obtain to expect.Better be SnO 2Be more than 0.01%, to be more preferably SnO 2Be more than 0.05%.In addition, if SnO 2Surpass 1%, then can become the generation source of bubble on the contrary, might make the burn through of glass slack-off, the bubble number increases.Better be SnO 2Be below 0.8%, to be more preferably SnO 2Be below 0.5%.SnO preferably 2Be below 0.3%.
TiO 2Being the composition that improves the weathering resistance of glass, is not neccessary composition, can contain as required.Contain TiO 2The time, if be lower than 0.005%, then might can't obtain obvious effects for improving weathering resistance.Better be TiO 2Be more than 0.01%, to be typically TiO 2Be more than 0.1%.
If TiO 2 Surpass 1%, then glass becomes unstable, and devitrification might take place.Better be TiO 2Be below 0.8%, to be typically TiO 2Be below 0.6%.
Li 2O is the composition that improves glass melting property, is not neccessary composition, can contain as required.Contain Li 2During O,, then obvious effects might can't be obtained for improving meltbility if be lower than 1%.Better be Li 2O more than 3%, is typically Li 2O is more than 6%.
If Li 2O surpasses 15%, and then weathering resistance might descend.Better be Li 2O below 10%, is typically Li 2O is below 5%.
SrO is the composition that is used to improve glass melting property, is not neccessary composition, can contain as required.When containing SrO,, then obvious effects might can't be obtained for improving meltbility if be lower than 1%.Better be that SrO is more than 3%, being typically SrO is more than 6%.
If SrO surpasses 15%, then weathering resistance and chemical enhanced characteristic might descend.Better be that SrO is below 12%, being typically SrO is below 9%.
BaO is the composition that is used to improve glass melting property, is not neccessary composition, can contain as required.When containing BaO,, then obvious effects might can't be obtained for improving meltbility if be lower than 1%.Better be that BaO is more than 3%, being typically BaO is more than 6%.
If BaO surpasses 15%, then weathering resistance and chemical enhanced characteristic might descend.Better be that BaO is below 12%, being typically BaO is below 9%.
ZnO is the composition that is used to improve glass melting property, is not neccessary composition, can contain as required.When containing ZnO,, then obvious effects might can't be obtained for improving meltbility if be lower than 1%.Better be that ZnO is more than 3%, being typically ZnO is more than 6%.
If ZnO surpasses 15%, then weathering resistance might descend.Better be that ZnO is below 12%, being typically ZnO is below 9%.
In addition, as the finings of glass, can contain Sb in the scope of not damaging target capabilities 2O 3, Cl, F, other composition.Contain under the situation of such composition, the content sum of these compositions better is below 1%, and being typically is below 0.5%.
Breakage that fall impacting when considering by use causes and the contact damage that is caused by long use, the painted opaque glass framework that requires to be contained in the electronics outside has HS.
As the method that improves glass intensity, above-mentioned air-cooled reinforcement (physical strengthening method) and chemical enhanced method are known as forming the technology of compressive stress layers at glass surface.
Painted opaque glass framework is difference with employed position, but under flat situation such as for example panel, thickness adopts the thickness below the 2mm usually mostly.If the sheet glass to thin like this adopts air-cooled reinforcement, then can be difficult to form compressive stress layers, thereby can not obtain the high-intensity characteristic of target because of surperficial and inside are difficult to the formation temperature difference.In addition, when adopting air-cooled reinforcement,, probably damage planarity for thin especially sheet glass, and might damage texture as decoration element because cooling temperature is inhomogeneous.Considering from these aspects, better is to utilize the latter's chemical enhanced method to strengthen.
Be arranged at the method for amount of compressive stress of the compressive stress layers of glass surface as mensuration, known following method.
The compressive stress layers of glass surface is compared with the glass part beyond the compressive stress layers, and specific refractory power is high.And, this specific refractory power from the bottom of compressive stress layers to surperficial monotone increasing.In addition, the double refraction of this compressive stress layers also increases absolute value monotonously towards the surface.Therefore; Exist and the relation curve of distinguishing corresponding two degree of depth and specific refractory power perpendicular to the light of glass surface vibration and the light that is parallel to glass surface; Produce different optical waveguides effects; Through the interference fringe image that obtains more thus, can calculate surface compression stress, the surface compression stressor layers degree of depth as the amount of compressive stress of chilled glass.
Above-mentioned use in the measuring method of amount of compressive stress of chilled glass of optical waveguides effect, must obtain by the interference fringe image that forms by bright fringes or dark fringe that produces perpendicular to the light of glass surface vibration and the light that is parallel to the glass surface vibration.
But; In this measuring method, chilled glass is because of containing coloring components when painted, and light is used as the absorptions such as metals ion of coloring components when the upper layer of chilled glass is propagated; Thereby be difficult to use the light of ejaculation to discern interference fringe image, be difficult to measure.
Chilled glass of the present invention is that painted opaque glass and transparent glass is range upon range of to carry out the integrated chilled glass that forms, and for this integrated glass that forms, adopts enhancement method on the surface compressive stress layers to be set.Then, the measuring method of amount of compressive stress of non-failure mode of optical waveguides effect that used above-mentioned utilization is measured the amount of compressive stress of transparent glass part.Use the measured value of the amount of compressive stress of this transparent glass part, calculate painted opaque glass part or the whole amount of compressive stress of chilled glass.By this, can confirm painted opaque glass part or the whole amount of compressive stress of chilled glass with nondestructive mode.
Need make the light transmission of the wavelength of visible region with the incorporate transparent glass of painted opaque glass, so that can measure through the measuring method of the above-mentioned amount of compressive stress of utilizing the optical waveguides effect.Therefore, for the optical transmission rate of the wavelength that improves the visible region, better be that transparent glass does not contain coloring components in glass.But,, then also can in glass, contain a certain amount of coloring components as long as do not hinder mensuration.In addition, the peak of the specific absorbance of the light of transparent glass under the wavelength of 550nm～650nm also can be lower than 1.7mm -1Transparent glass with this specific absorbance comprises the glass of water white glass and colored transparent.If have the transparent glass of this specific absorbance, then can measure amount of compressive stress exactly by enough existing surface stress determinators.
In the surface stress measuring method of chilled glass of the present invention, it is characterized in that using the measured value of amount of compressive stress of compressive stress layers on the surface of transparent glass part, calculate painted opaque glass part or the whole amount of compressive stress of chilled glass.
As this method, better comprise: measure the operation of having carried out the surface stress characteristic of above-mentioned painted opaque glass and above-mentioned transparent glass after the intensified process by identical conditions respectively; Use the surface stress characteristic of above-mentioned painted opaque glass and above-mentioned transparent glass to confirm to be used for the operation of IC that amount of compressive stress according to above-mentioned transparent glass calculates the amount of compressive stress of above-mentioned painted opaque glass; Measure the operation of the above-mentioned transparent glass amount of compressive stress partly of above-mentioned chilled glass with nondestructive mode; Calculate the operation of the whole amount of compressive stress of above-mentioned painted opaque glass part or above-mentioned chilled glass with the measured value of the amount of compressive stress of using above-mentioned transparent glass part and above-mentioned IC.
In the chemical enhanced processing, the parameter that the surface stress characteristic of the glass of gained is exerted an influence has that intensified process condition (kind of melting salt, concentration, temperature, treatment time), glass are formed, the thermal history of glass, follow residual stress that the shaping of glass produces etc.Therefore; Under same intensified process condition, painted opaque glass and transparent glass are carried out intensified process, destroy and the sample method for processing is measured separately surface stress characteristic (measuring the operation of having carried out the surface stress characteristic of above-mentioned painted opaque glass and above-mentioned transparent glass after the intensified process by identical conditions respectively) with following.In addition; When carrying out this intensified process; Both can painted opaque glass and transparent glass is range upon range of integrated to carry out, also can not carry out range upon range ofly, integrated, but consider the thermal history of glass and the influence of shaping; Better be to after carrying out intensified process through range upon range of, the integrated glass that forms, painted opaque glass separated with transparent glass measure.As the surface stress characteristic, the following determination object of can giving an example: as the surface compression stress of the amount of compressive stress of glass (below be also referred to as CS) and surface compression layer depth (DOL), flexural strength, crack initiation load, potassium diffusion layer degree of depth etc.In addition, for chemical enhanced processing, in the intensified process operation of reality, the intensified process condition changes sometimes, therefore better is to use multiple intensified process condition, measures surface stress characteristic separately.
Then; The surface stress characteristic that use records confirms to be used for to calculate according to the amount of compressive stress of transparent glass the IC (using the surface stress characteristic of above-mentioned painted opaque glass and above-mentioned transparent glass to confirm to be used for the operation of IC that amount of compressive stress according to above-mentioned transparent glass calculates the amount of compressive stress of above-mentioned painted opaque glass) of the amount of compressive stress of painted opaque glass.Particularly, both the surface stress characteristic under the specific intensified process condition is drawn a diagram, confirm IC.For example, use the measured value that has the flexural strength of correlationship with CS, the CS of painted opaque glass is confirmed as IC with respect to the degree of the CS of transparent glass.Better be that suitable surface stress characteristic and multiple intensified process condition are carried out this step respectively, confirm the IC of each amount of compressive stress and intensified process condition.
After confirming IC; Utilize the measuring method do not destroy the amount of compressive stress of measuring sample (for example, above-mentioned use the measuring method of amount of compressive stress of optical waveguides effect) to measure the amount of compressive stress of the transparent glass part of chilled glass (measuring the operation of amount of compressive stress of the above-mentioned transparent glass part of above-mentioned chilled glass with nondestructive mode).In this operation, importantly measure measuring sample with nondestructive mode.Therefore, the chilled glass after painted opaque glass and transparent glass become one is arranged on the surface stress determinator under the situation of not carrying out sample processing, the determination part branch of transparent glass part and device is adapted measure.Thus, through later operation, can calculate amount of compressive stress to all chilled glasses with nondestructive mode for ensuring the quality of products.
Then; The measured value and the IC of the amount of compressive stress of the transparent glass part that use records with nondestructive mode calculate the whole amount of compressive stress of painted opaque glass part or chilled glass (using measured value and the above-mentioned IC of the amount of compressive stress of above-mentioned transparent glass part to calculate the operation of the whole amount of compressive stress of above-mentioned painted opaque glass part or above-mentioned chilled glass).For IC, can consider the intensified process condition of chilled glass operation, use predetermined suitable intensified process condition.Thus; Even under the situation that the amount of compressive stress of painted opaque glass can't be measured through nondestructive mode; Also can use the measured value of the amount of compressive stress of transparent glass part, calculate the amount of compressive stress of painted opaque glass part.
In addition; Knowing in advance and can the amount of compressive stress of painted opaque glass part and transparent glass part be regarded as under the roughly the same situation; Perhaps under the situation of amount of compressive stress with the transparent glass part, also can regard the measured value of transparent glass amount of compressive stress partly as painted opaque glass part or the whole amount of compressive stress of chilled glass as chilled glass integral intensity management object.In the surface stress measuring method of glass of the present invention, above-mentioned situation also is contained in following notion: use to measure the transparent glass part amount of compressive stress and value, calculate painted opaque glass part or the whole amount of compressive stress of chilled glass.
Painted opaque glass can be the painted opaque glass that in transparent glass, contains above-mentioned coloring components.Thus; Painted opaque glass is identical with each components in proportions that the glass of transparent glass except coloring components is formed; Therefore can ignore the variation of the IC that causes when the intensified process condition changes, the operation of calculating the surface stress characteristic of painted opaque glass or chilled glass becomes easy.In addition, can make the thermal expansivity of glass separately roughly the same.
Painted opaque glass and transparent glass also can be through cooling off under the painted opaque glass of fused and the transparent glass state of contact that is in solid state making heating, painted opaque glass being solidified carry out range upon range of, the integrated glass that forms.Thus, can entrained air and impurity between painted opaque glass and transparent glass, in designability, good attractive in appearance, and both sharp outlines, also be suitable for transparent glass is given the situation of other following functions.
In addition, painted opaque glass and transparent glass better be glass temperature in 25～300 ℃ scope separately the difference of thermal expansivity of glass 0～5 * 10 -7/ ℃ scope in.Thus, with aforesaid method both when integrated, can be suppressed the breakage of glass in carrying out incorporate process.
As painted opaque glass and transparent glass is range upon range of to carry out incorporate method, can use the manufacturing process of glass: painted opaque glass heating is made its fused first operation with following operation; Make the painted opaque glass that is in molten state and be configured as second operation that the bar-shaped transparent glass that is in solid state contacts; Cool off making under the painted opaque glass that is in molten state and the transparent glass state of contact that is in solid state, make painted opaque glass solidified the 3rd operation.As the manufacturing process of such glass, the following three kinds of forms of can giving an example.
(first form)
In above-mentioned second operation, has following operation: at upper end and lower ending opening and take in the operation of inserting the transparent glass that is in solid state in the container of the painted opaque glass that is in molten state; The operation that the painted opaque glass that will be in molten state and the transparent glass that is in solid state are extracted from the lower end of said vesse simultaneously.
(second form)
In above-mentioned second operation, have following operation: the transparent glass that will be in solid state is positioned over the operation in the mould; The transparent glass that will be in solid state is positioned over the operation in the mould; Make the painted opaque glass that is in molten state flow into the operation in the mould.
(the 3rd form)
In above-mentioned second operation, have following operation: the transparent glass that will be in solid state is placed on the operation on the travelling belt; Make the painted opaque glass that is in molten state flow out to the operation on the above-mentioned travelling belt continuously.
In arbitrary form, can before second operation, have operation to the transparent glass preheating that is in solid state.
In addition, in arbitrary form, also can after above-mentioned the 3rd operation, have the orthogonal direction cutting of the above-mentioned painted opaque glass after integrated and transparent glass edge and the long side direction of above-mentioned transparent glass, the operation of grinding.
In addition, also can not use above-mentioned painted opaque glass and transparent glass range upon range ofly carrying out incorporate method, carry out range upon range of, incorporate additive method (bonding, sealing, engaging etc.) after will being formed separately separately and carry out integrated and use.Importantly,, the transparent glass in the chilled glass partly is used for surface stress measures among the present invention with painted opaque glass with transparent glass is range upon range of carries out intensified process to carry out the integrated glass that forms.
Above-mentioned molten state is meant that the viscosity of glass comprises log η=5.0 (processing temperature), and glass is in the situation of soft condition thus.In addition, solid state is meant that the viscosity of glass does not comprise log η=7.6 (softening temperature), and glass is in the situation of hard state thus.
Chilled glass of the present invention can be as the painted opaque glass framework that is contained in the electronics outside.Therefore chilled glass has HS owing to possess compressive stress layers on the surface, particularly can perform well in the painted opaque glass framework of the electronics that mobile phone etc. portably uses.In addition therefore good on designability owing to possess distinctive quality sense of glass and high quality sense, can be well as the decoration element of electronics.
In addition; ロ go body), running indicator is with the function more than at least a kind of transmittance section when chilled glass was used as painted opaque glass framework, transparent glass can possess signal transmitting and receiving portions such as the light-receiving part that is selected from the digital camera that is built in electronics, telepilot, logotype (Japanese:.Thus, transparent glass not only can be used for the surface stress of glass to be measured, and can also give multiple function.
The method of manufacture of chilled glass is for range upon range of to carry out the method for manufacture of the integrated chilled glass that forms with painted opaque glass and transparent glass; It manages painted opaque glass part or the whole amount of compressive stress of chilled glass through the amount of compressive stress of the compressive stress layers of the transparent glass part of the above-mentioned chilled glass of mensuration.
In addition; Method of manufacture as chilled glass; Better have:, above-mentioned painted opaque glass is solidified carry out range upon range of, incorporate operation through cooling off making under the painted opaque glass that is in molten state and the transparent glass state of contact that is in solid state; To comprise the above-mentioned painted opaque glass and the mode of above-mentioned transparent glass above-mentioned incorporate glass cutting is become tabular operation; Form the reinforcement operation that compressive stress layers is processed chilled glass with the surface of tabular glass after cutting; The amount of compressive stress of the compressive stress layers of the transparent glass part through measuring above-mentioned chilled glass is managed painted opaque glass part or the whole amount of compressive stress of chilled glass.Thus, can calculate the painted opaque glass that directly to measure amount of compressive stress and the amount of compressive stress of chilled glass with nondestructive mode.Therefore, the production management of chilled glass and quality guarantee become easily, can boost productivity.
In addition; Managing painted opaque glass part or the whole amount of compressive stress of chilled glass is meant; Can enumerate a following example: according to the measured value of the amount of compressive stress of the compressive stress layers of the transparent glass of above-mentioned chilled glass part; The surface that is adjusted at the plate glass after the cutting forms compressive stress layers with the intensified condition in the reinforcement operation of processing chilled glass, so that the condition that painted opaque glass part or the whole amount of compressive stress of chilled glass drop in the suitable scope is carried out production management.In addition; Particular content as above-mentioned management; Also can give an example: according to the measured value of the amount of compressive stress of the compressive stress layers of the transparent glass of above-mentioned chilled glass part; The surface of confirming the plate glass after cutting forms compressive stress layers with the intensified condition in the reinforcement operation of processing chilled glass, gets rid of the not glass in required scope of the whole amount of compressive stress of painted opaque glass part or chilled glass.
Embodiment
As painted opaque glass, prepare by the following plate glass of forming the black in color that constitutes: the molar percentage with the oxide compound benchmark is represented, contains 61.9% SiO 2, 11.5% Na 2O, 3.9% K 2O, 10.6% MgO, 5.8% Al 2O 3, 2.4% ZrO, 0.4% Co 3O 4, 3.3% Fe 2O 3, 0.4% SO 3In addition, as transparent glass, prepare by the following transparent plate glass that is that constitutes of forming: the molar percentage with the oxide compound benchmark is represented, contains 64.3% SiO 2, 12.0% Na 2O, 4.0% K 2O, 11.0% MgO, 6.0% Al 2O 3, 2.5% ZrO, 0.01% Fe 2O 3, 0.1% SO 3In addition, transparent glass is with the Co as coloring components 3O 4, Fe 2O 3Glass after from painted opaque glass, removing.With the KNO of this glass-impregnated in 450 ℃ 3In the melting salt 6 hours, carry out chemical enhanced processing.
Then, for painted opaque glass and transparent glass, measure the potassium diffusion depth with four-point bending test (the bending strength test methods of JIS R 1601 fine ceramicss), EPMA through chemical enhanced processing.
In addition, for the transparent glass through chemical enhanced processing, (it is made to roll over former making, FSM-6000LE) measures surface compression stress and surface compression layer depth to use the glass surface taseometer.
Here, there is certain correlationship between the intensity that obtains by four-point bending test of glass and the surface compression stress.In addition, there is certain correlationship between the potassium diffusion depth and the surface compression stressor layers degree of depth.Utilize these relations,, calculate the IC that is used for calculating the surface compression stress of painted opaque glass according to the surface compression taseometer of transparent glass according to the painted opaque glass of four-point bending test and the intensity data of transparent glass.In addition, according to the potassium diffusion depth data of painted opaque glass and transparent glass, calculate the IC that is used for calculating the surface compression stressor layers degree of depth of painted opaque glass according to the surface compression stressor layers hydrobarometer of transparent glass.
Then, as chilled glass, make above-mentioned painted opaque glass and transparent glass is range upon range of to carry out the integrated chilled glass that forms.As integral method, preparing is shaped in advance is solidified into columned transparent glass, and it is built in the mould with solid state.Then; After making the painted opaque glass that is in molten state that is coloured to black flow in the mould that is built-in with the transparent glass that is in solid state, cooling is in the painted opaque glass of molten state and painted opaque glass and transparent glass is integrated.Then, glass edge after integrated and the orthogonal direction of the long side direction of columned transparent glass are cut into the thickness of 1mm, again facet is carried out attrition process.Thus, obtain painted opaque glass shown in Figure 1 10 and the transparent glass 10 integrated chilled glasses that form 1.
Then, for the transparent glass part of chilled glass, use the glass surface taseometer to measure the surface compression stress and the surface compression stressor layers degree of depth.Then, use the surface compression stress of above-mentioned IC, transparent glass and the measured value of the surface compression stressor layers degree of depth, calculate the surface compression stress and the surface compression stressor layers degree of depth of painted opaque glass.
In addition, the surface compression stress and the surface compression stressor layers degree of depth in order to calculate chilled glass precompute the IC relevant with the intensity data of transparent glass and chilled glass and get final product.
By this, can confirm painted opaque glass part or the whole amount of compressive stress of chilled glass with nondestructive mode.
(other embodiment)
As above, the present invention has been carried out detailed explanation, but the present invention is not limited to above-mentioned concrete example,, then can carries out various distortion and change as long as in not departing from the scope of the present invention based on above-mentioned concrete example.For example, in the above-mentioned explanation, the glass that painted opaque glass is recited as black is illustrated, but painted tone is not limited to black, can adopt various tones.In addition, transparent glass is as long as the surface stress instrumentation level pressure stress under compression amount of the enough glass of ability then also can be a colored transparent glass.
Also have, in the above-mentioned embodiment, the situation that painted opaque glass is used as the painted opaque glass framework of electronics is illustrated, but also can be used for other purposes.In addition, also can with painted opaque glass and transparent glass range upon range of with carry out integrated after, be configured as the framework shape of intelligent terminals such as smart mobile phone through press molding, after it is carried out intensified process as framework.
The possibility of utilizing on the industry
Surface stress measuring method according to chilled glass of the present invention, glass; Even the part has low opaque the painted chilled glass of transsmissivity in the visible region; Also can calculate painted opaque glass part or the whole amount of compressive stress of chilled glass with nondestructive mode through measuring the amount of compressive stress of transparent part.The qualitative control that therefore, can perform well in strength of glass is regarded as the important painted opaque glass framework that for example is contained in the portable electric appts outside.
The explanation of symbol
1 ... Chilled glass, 10 ... Colored glass, 20 ... Transparent glass.

Claims (14)

1. chilled glass is characterized in that, painted opaque glass and transparent glass is range upon range of integrated to carry out, and the surface of the glass after integrated forms compressive stress layers again.
2. chilled glass as claimed in claim 1 is characterized in that, the measured value of the amount of compressive stress of the said compressive stress layers of said transparent glass is used to calculate the said painted opaque glass or the amount of compressive stress of said chilled glass.
3. chilled glass as claimed in claim 2; It is characterized in that; In said painted opaque glass; As the coloring components in the glass, represent with the molar percentage of oxide compound benchmark, contain at least a kind of composition of 0.1～7% the MOX that is selected from Co, Mn, Fe, Ni, Cu, Cr, V, Bi.
4. chilled glass as claimed in claim 3 is characterized in that, said painted opaque glass is for containing the glass of said coloring components in said transparent glass.
5. like each described chilled glass in the claim 1～4, it is characterized in that the peak of the specific absorbance of said transparent glass under the wavelength of 550nm～650nm is lower than 1.7mm -1
6. like each described chilled glass in the claim 1～5; It is characterized in that; Through cooling off under said painted opaque glass after the fusion and the said transparent glass state of contact that is in solid state making heating, with said painted opaque glass solidify come range upon range of integrated to carry out.
7. like each described chilled glass in the claim 1～6, it is characterized in that, said painted opaque glass and said transparent glass in glass temperature is 25 ℃～300 ℃ scope separately the difference of thermal expansivity of glass 0～5 * 10 -7/ ℃ scope in.
8. painted opaque glass framework is characterized in that, is made up of each described chilled glass in the claim 1～7.
9. painted opaque glass framework as claimed in claim 8 is characterized in that, said transparent glass possesses and is selected from camera with light-receiving part, signal transmitting and receiving portion, logotype, the running indicator at least a above function with the transmittance section.
10. electronics is characterized in that, claim 8 or 9 described painted opaque glass frameworks are equipped with in the outside.
11. the measuring method of the surface stress of glass; It is for range upon range of integrated to carry out with painted opaque glass and transparent glass; Be determined at the method for the amount of compressive stress of the compressive stress layers that the surface of the chilled glass after integrated forms; It is characterized in that, use to measure said transparent glass part amount of compressive stress and value calculate said painted opaque glass part or the whole amount of compressive stress of said chilled glass.
12. the surface stress measuring method of glass as claimed in claim 11 is characterized in that, comprising:
Measure the operation of having carried out the surface stress characteristic of said painted opaque glass and said transparent glass after the intensified process by identical conditions respectively;
Use the surface stress characteristic of said painted opaque glass and said transparent glass to confirm to be used for the operation of IC that amount of compressive stress according to said transparent glass calculates the amount of compressive stress of said painted opaque glass;
Measure the operation of the said transparent glass amount of compressive stress partly of said chilled glass with nondestructive mode; With
Use measured value and the said IC of the amount of compressive stress of said transparent glass part to calculate the operation of the whole amount of compressive stress of said painted opaque glass part or said chilled glass.
13. the method for manufacture of chilled glass; It is for range upon range of to carry out the method for manufacture of the integrated chilled glass that forms with painted opaque glass and transparent glass; It is characterized in that; The compressive stress layers of the compressive stress layers of the transparent glass part through measuring said chilled glass is managed painted opaque glass part or the whole amount of compressive stress of chilled glass.
14. the method for manufacture of chilled glass as claimed in claim 13 is characterized in that,
Have:
Through cooling off making under the painted opaque glass that is in molten state and the transparent glass state of contact that is in solid state, said painted opaque glass is solidified carry out range upon range of, incorporate operation;
To comprise the said painted opaque glass and the mode of said transparent glass said incorporate glass cutting is become tabular operation; With
The surface of the tabular glass after cutting forms the reinforcement operation that compressive stress layers is processed chilled glass,
The amount of compressive stress of the compressive stress layers of the transparent glass part through measuring said chilled glass is managed painted opaque glass part or the whole amount of compressive stress of chilled glass.
CN201210174587.9A 2011-06-09 2012-05-30 Strengthening glass and manufacture method, the surface stress assay method of this strengthening glass Expired - Fee Related CN102815859B (en)

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