CN107162410A - A kind of glass and preparation method thereof - Google Patents
A kind of glass and preparation method thereof Download PDFInfo
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- CN107162410A CN107162410A CN201710537860.2A CN201710537860A CN107162410A CN 107162410 A CN107162410 A CN 107162410A CN 201710537860 A CN201710537860 A CN 201710537860A CN 107162410 A CN107162410 A CN 107162410A
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- Prior art keywords
- glass
- ion
- ion exchange
- layer depth
- ceo
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C21/00—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
- C03C21/001—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions
- C03C21/002—Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface in liquid phase, e.g. molten salts, solutions to perform ion-exchange between alkali ions
Abstract
The invention discloses a kind of glass and preparation method thereof, it is related to glass technology field.One embodiment of the glass includes：A kind of ion exchangeable glass, on the basis of oxide, according to mass percent meter, including：SiO2, 48%~58%；Na2O, 11%~18%；Al2O3, 17%~30%；P2O5, 1%~6%；B2O3, 0%~2%；MgO, 1%~3%；ZnO, 0.5%~3%；Li2O, 0.3%~3%；ZrO2, 0.1%~1%；CeO2, 0.1%~0.3%；SnO2, 0.1%~0.3%.The embodiment can greatly improve the compression stress, surface compression layer depth and hardness of the glass surface compressive stress layers after ion exchange, with excellent anti-dropping capability and adhesion strength.
Description
Technical field
The present invention relates to glass technology field, more particularly to a kind of glass and preparation method thereof.
Background technology
By suitable ion-exchange process and the glass with higher compression stress and surface compression layer depth, by
In its excellent anti-dropping capability and adhesion strength, and it is able to be widely used in the fields such as mobile phone, flat board, computer, TV；
Simultaneously because its density is less than common soda-lime glass, the weight of electronic product can be reduced, the Product Experience of user is improved, so that
It is able to be applied to Portable touch control electronic panel field.
Electronic equipment is when by larger power or impact, and glass is more thin to be more easily damaged, and is that this people enters to thin glass
Ion-exchange process is gone so that the intensity of glass is improved.But the glass of different compositions passes through different ion exchanges
Technique, the performance of the glass of acquisition also varies.In order to improve intensity of the thin glass after suitable ion-exchange process,
It is necessary to probe into the composition of glass.
The content of the invention
In view of this, the embodiment of the present invention provides a kind of glass and preparation method thereof, can greatly improve and be handed over by ion
The intensity of the glass changed after technique.
To achieve the above object, one side according to embodiments of the present invention is there is provided a kind of ion exchangeable glass,
On the basis of oxide, according to mass percent meter, including：
SiO2, 48%~58%；
Na2O, 11%~18%；
Al2O3, 17%~30%；
P2O5, 1%~6%；
B2O3, 0%~2%；
MgO, 1%~3%；
ZnO, 0.5%~3%；
Li2O, 0.3%~3%；
ZrO2, 0.1%~1%；
CeO2, 0.1%~0.3%；
SnO2, 0.1%~0.3%.
Alternatively, according to mass percent meter, SiO2+Al2O3+P2O5+B2O3>=79%.
Alternatively, according to mass percent meter, 0.32%≤ZrO2+CeO2+SnO2≤ 1.3%.
Alternatively, according to quality meter, 0.5≤CeO2/SnO2≤1。
Alternatively, according to quality meter, 0.2≤(Al2O3+0.7P2O5+1.4B2O3)/1.7SiO2≤ 0.5, and/or, 0.65
≤(Al2O3+1.4B2O3)/(0.7P2O5+1.6Na2O+3.3Li2O)≤1。
Alternatively, according to quality meter, 0.03≤Li2O/(0.485Na2O+Li2O)≤0.3, and/or, 2B2O3/(P2O5+
1.429Al2O3)≤0.11。
Alternatively, according to mass percent meter, MgO+ZnO≤5%.
Alternatively, on the basis of oxide, according to mass percent meter, ion exchangeable glass includes：
SiO2, 48%~58%；
Na2O, 12%~17%；
Al2O3, 18%~27%；
P2O5, 1.5%~5.5%；
B2O3, 0%~1.3%；
MgO, 1%~3%；
ZnO, 0.5%~3%；
Li2O, 0.3%~3%；
ZrO2, 0.1%~1%；
CeO2, 0.1%~0.3%；
SnO2, 0.1%~0.3%.
Alternatively, on the basis of oxide, according to mass percent meter, ion exchangeable glass includes：
SiO2, 48%；
Na2O, 15.84%；
Al2O3, 30%；
P2O5, 1%；
B2O3, 0.27%；
MgO, 1.5%；
ZnO, 0.5%；
Li2O, 2.34%；
ZrO2, 0.1%；
CeO2, 0.15%；
SnO2, 0.3%.
Another aspect according to embodiments of the present invention there is provided a kind of preparation method of ion exchangeable glass, including：
The frit for the constituent that can form the glass that the embodiment of the present invention is provided on one side will be modulated into
Mixing；
Frit is melted and clarifying treatment, the ion exchangeable glass is obtained after cooling.
Alternatively, the ion exchangeable glass is shaped to plate glass.
Alternatively, the thickness of the plate glass is 1.1mm.
There is provided a kind of glass of process ion exchange, the process ion for other side according to embodiments of the present invention
The glass of exchange has a constituent for the glass that the embodiment of the present invention the provides on one side, and with from its surface internally
The compressive stress layers of extension.
Alternatively, the compression stress of the compressive stress layers is more than 850MPa, and surface compression layer depth is more than 50 μm.
Alternatively, the compressive stress layers include potassium ion.
There is provided a kind of preparation method of the glass of process ion exchange, bag for still another aspect according to embodiments of the present invention
Include：
The frit for the constituent that can form the glass that the embodiment of the present invention is provided on one side will be modulated into
Melting, is configured to plate glass；
By the plate glass as carrying out ion exchange in ion exchange liquid.
Alternatively, the ion exchange liquid includes KNO3。
Alternatively, the temperature of ion exchange is 425 DEG C, and/or, the time of ion exchange is 2~10h.
One embodiment in foregoing invention has the following advantages that or beneficial effect：By adopting various oxides in glass
Use suitable adding proportion so that glass has larger cyberspace to be able to carry out ion exchange quickly and increase ion exchange
Intensity, greatly improve the compression stress and surface compression layer depth of the glass surface compressive stress layers after ion exchange；Pass through
A certain proportion of CeO is added in the constituent of glass2/SnO2Compound clarifier, it is possible to reduce the gas rate in glass；It is logical
Cross and a certain proportion of ZrO is added in reaction system2, the extension of crackle in glass can be slowed down, there is glass surface higher
Hardness.According to the present invention ion exchangeable glass, after ion-exchange process have excellent anti-dropping capability and
Adhesion strength.
The further effect that above-mentioned non-usual optional mode has adds hereinafter in conjunction with embodiment
With explanation.
Brief description of the drawings
Accompanying drawing is used to more fully understand the present invention, does not constitute inappropriate limitation of the present invention.Wherein：
Fig. 1 reaches showing for minimum time required during 50 μm of surface compression layer depth for the glass Jing Guo ion exchange
It is intended to.
Embodiment
The one exemplary embodiment of the present invention is explained below in conjunction with accompanying drawing, including the various of the embodiment of the present invention
Details should think them only exemplary to help understanding.Therefore, those of ordinary skill in the art should recognize
Arrive, various changes and modifications can be made to the embodiments described herein, without departing from scope and spirit of the present invention.Together
Sample, for clarity and conciseness, eliminates the description to known function and structure in following description.
In the present invention, each composition of glass is indicated on the basis of oxide, the content of each composition according to oxide matter
Percentage is measured to represent.Wherein, it is " on the basis of oxide ", it is assumed that as the raw material of the constituent of the glass of the present invention
Whole decomposition and inversions in melting such as oxide, nitrate for using are oxide, represent each composition composition contained in glass
Method；" being represented according to the mass percent of oxide " is, during using the gross mass of the generation oxide as 100%, glass
In the amount of each composition that contains.
Unless otherwise stated, the number range enumerated includes the upper and lower bound of the scope simultaneously, and described
Any range between scope.It will also be appreciated that the various features disclosed in the description can arbitrarily and all combination
Mode is used.
According to the ion exchangeable glass of the present invention, on the basis of oxide, including following constituent：SiO2,
Na2O, Al2O3, P2O5, B2O3, MgO, ZnO, Li2O, ZrO2, CeO2, SnO2。
SiO2It is to form the main oxide of glass, can participates in forming silicon-oxygen network.The SiO of high level2Shape can be increased
Point juxtaposition metamorphose amount needed for being limited crackle system into intensity, improves mechanical strength, chemical stability and the heat endurance of glass,
But SiO2The glass of too high levels or pure SiO2The fusion temperature of glass is too high, and the defects such as bubble, striped easily occurs.
SiO2Content reduction when, the compression stress of the compressive stress layers of glass after ion exchange, but SiO can be improved2Content it is too low
When, thermal coefficient of expansion increase, the resistance to sudden heating reduction of glass, and it is difficult to vitrifying, increased devitrification resistance deterioration.Therefore this hair
Bright SiO2The optimal scope of content is 48%~58%.
Al2O3It is the composition for improving weatherability, the crystallization tendency of glass can be reduced, chemical stability, the heat of glass is improved
Stability, mechanical strength, hardness.In alumina silicate glass, Al2O3It can participate in forming aluminum-oxygen network network, in the net of strengthened glass
There is provided bigger cyberspace while network structure, so that glass can have faster ion-exchange speed.Improve glass
Al in composition2O3Although content can improve the surface compression layer depth of glass, the fusing of glass improve strength of glass
Temperature and liquidus temperature also can significantly rise, so as to cause the production problem such as glass clarifying and homogenizing difficulty.In the present invention, lead to
Cross Al2O3Content be set to 16%~30% and the various oxides of other in glass is kept suitable ratio, can keep away
Exempt to cause the production problem such as glass clarifying and homogenizing difficulty, cause again glass have larger cyberspace be able to carry out quickly from
Son exchange and increase ion exchange intensity, greatly improve the glass surface compressive stress layers after ion exchange compression stress and
Surface compression layer depth.It is further preferred that Al2O3Content be 18%~27%.
Na2O is the composition for promoting frit melting.In order that glass has good ion-exchange capacity, it is necessary to contain
Na more than a certain amount of2O, just can guarantee that the compressive stress layers of glass surface after ion exchange has excellent compression stress
With surface compression layer depth.
In the prior art by Na in being constituted by improving glass2O content improves strength of glass, although can so carry
The compression stress of high glass, but alkali content is too high to be greatly reduced the fusion temperature and liquidus temperature of glass, and cause tight
The volatilization problems of weight.In addition, too high Na2O content can also sharply increase the thermal coefficient of expansion (Thermal of glass
Expansion Coefficient, CTE), reduce the chemical stability of glass.
In the prior art by the part Na in by the way that glass is constituted2O replaces with K2O comes by the intensity of glass.Although
K+Can become much larger the cyberspace of glass, when ion exchange is carried out, K in glass+In the passage of statistical distribution
The easy access of ion exchange is formd, so the part Na during glass is constituted2O replaces with K2O can be carried to a certain extent
The surface compression layer depth of high glass；But the part Na during glass is constituted2O replaces with K2O can make the compression stress of glass big
Width declines.
In the present invention, by by Na2O content is set to 11%~18% and protects the various oxides of other in glass
Suitable ratio is held, has both been avoided that due to a series of too high caused production problems of alkali content, has caused glass to have larger net again
Network space is able to carry out ion exchange quickly and increases the intensity of ion exchange, greatly improves the glass surface after ion exchange
The compression stress and surface compression layer depth of compressive stress layers.It is further preferred that Na2O content is 12%~17%.
P2O5It is a kind of glass former, the fusion temperature of glass can be reduced.P2O5Can be with X2O3(X is B or Al) combines
Form [XPO4] network structure, on the one hand, the network structure can provide the space bigger than aluminum-oxygen network network, so as to significantly carry
The ion-exchange speed of high glass, on the other hand, the network structure make it that the network of glass is more complete, further lifts glass
Heat endurance, hardness and to shock proof mechanical property.But, excessive P is added in glass2O5Phosphorus content mistake can be caused
High and phosphorus volatilization problems；Phosphorus content is higher, reaches the ion exchange work required for a certain compression stress and surface compression layer depth
Skill is more complicated, takes longer；The P of too high amount2O5The tendency towards devitrification of glass and the chemical stability of reduction glass can also be increased.
Therefore P in the present invention2O5Optimum content be 1~6%, it is further preferred that for 1.5%~5.5%.
B2O3It is a kind of glass former, the fusion temperature of glass can be significantly reduced.B2O3It can participate in forming boron-oxygen network,
The rigidity of the boron-oxygen network is smaller than the rigidity of silicon-oxygen network structure, and glass body can be allowed to have bigger before crackle is formed
Deformation quantity.But the B of high content2O3Glass ion exchange capacity can be obviously reduced.Therefore B in the present invention2O3Optimum content be 0
~2%, it is further preferred that being 0~1.3%.
MgO is network modifying oxide, helps to reduce the fusion temperature of glass, improves the uniformity of glass, increases glass
The hydrolytic resistance of glass.MgO can also make glass tend towards stability, and improve the durability of glass, prevent glass from producing crystallization.But it is too high
The MgO of content can increase the tendency towards devitrification of glass, such as form forsterite (Mg2SiO4) etc. crystal, and can substantially suppress glass
Ion-exchange capacity.Therefore MgO optimum content is 1~3% in the present invention.
ZnO belongs to glass network intermediate, can be effectively reduced the fusion temperature of glass.When alkali metal ion in glass
Content it is higher when, ZnO can participate in being formed glass network, increase the integrality of glass network, improve intensity and the change of glass
Learn stability.But when ZnO content is too high, the tendency towards devitrification of glass can be increased, gahnite (ZnAl is such as formed2O4) or zinc silicate
(Zn2SiO4) etc. crystal, and can substantially suppress the ion-exchange capacity of glass.Therefore ZnO optimum content is 0.5 in the present invention
~3%.
Li2O is the fluxing agent in glass fusion process；During ion exchange, Li2O can be such that glass keeps very
High compression stress.But too high Li2The network structure of O meeting considerable damage glass, can not only make the mechanical performance of glass, change
Learn stability significantly to decline, can also bring the raising being greatly lowered with production cost of surface compression layer depth.Therefore originally
Li in invention2O optimum content is 0.3~3%.
ZrO2The chemical stability of glass can be improved, increases the case hardness of glass；In addition, ZrO2Glass shape can also be improved
Into the pressure needed for crackle, the drop impact resistance energy and scratch resistant performance of glass are improved.But the ZrO of too high amount2Can significantly it carry
The fusion temperature of high glass, and bring the defects such as calculus.Therefore ZrO in the present invention2Optimum content be 0.1~1%.
CeO2It is the fining agent in glass fusion process, the gas rate in glass can be reduced.If CeO2Content it is too low,
Clarification request can not be met；Due to CeO2There is strong absorption to black light, if CeO2Too high levels, glass can present bright
Aobvious yellow, causes glass in the decrease in transmission in visible ray short wavelength region and ultraviolet range, hinders the object of glass
Property.Therefore CeO in the present invention2Optimum content be 0.1~0.3%.
SnO2It is the fining agent in glass fusion process, the gas rate in glass can be reduced.If SnO2Content it is too low,
Sufficient clarifying effect can not be played；If SnO2Too high levels, then Sn can be separated out as metal.SnO in the present invention2It is optimal
Content is 0.1~0.3%.
SiO2、Al2O3、P2O5And B2O3It can participate in forming silicon-oxygen network, aluminum-oxygen network network, [XPO respectively4] network and boron-
On the one hand oxygen network, these network structures can improve the ion-exchange capacity and speed of glass, on the other hand can lift glass
The performances such as heat endurance, hardness and resistance impact.Each above-mentioned network structure has one in terms of space size and structural capacity
Determine difference, in order to improve the integrality of glass network, further enhance the fracture toughness and stability of glass, it is preferred real at some
Apply in example, by percentage to the quality, SiO2+Al2O3+P2O5+B2O3>=79%.
In the glass constituent system of the present invention, ZrO2、CeO2With SnO2Between there is interaction, also, with matter
Percentages are measured, as 0.32%≤ZrO2+CeO2+SnO2When≤1.3%, the hardness and clarifying effect of glass are significantly improved.
CeO2Decomposition temperature be 1300~1400 DEG C, SnO2Decomposition temperature be more than 1500 DEG C, so by using
CeO2/SnO2Compound clarifier, it is ensured that discharge bubble can be continued in different temperature stages during glass melting, so as to obtain
Clarifying effect more preferably glass.Work as CeO2And SnO2Mass ratio when reaching certain limit, the gas in glass can be greatly reduced
Rate, the two cooperates with mutually the clarifying effect promoted to be significantly larger than exclusive use any of which fining agent or two kinds of clarifications
Clarifying effect when agent is used alone it is directly cumulative.Work as CeO2And SnO2Mass ratio it is too high or too low when, CeO2And SnO2's
Mutually collaboration facilitation effect is not obvious；Also, work as CeO2And SnO2Mass ratio it is too high when, it is also possible to glass can be made near purple
Outer light have a strong absorption and yellow or there is the precipitation of Sn metals.In certain embodiments, in mass, 0.5≤CeO2/
SnO2≤1。
In certain embodiments, in mass, 0.2≤(Al2O3+0.7P2O5+1.4B2O3)/1.7SiO2≤0.5.Have
The glass of the glass composition of the relational expression is met, more [AlPO can be formed4] network structure and [BPO4] network structure, so that
Further enhance the mechanical property of silicon-oxygen network.[AlPO in addition4] cyberspace it is larger, can accelerate glass ion hand over
Throw-over degree, and make the compressive stress layers of the glass surface after ion-exchange process that there is higher compression stress and surface to press
Contracting layer depth.
In further embodiments, in mass, the constituent of glass meets following relation：0.65≤(Al2O3+
1.4B2O3)/(0.7P2O5+1.6Na2O+3.3Li2O)≤1.More [AlPO can be formed by meeting the glass of above-mentioned condition4] network
Structure and [BPO4] network structure, so as to further enhance the mechanical property of silicon-oxygen network.[AlPO in addition4] cyberspace compared with
Greatly, the ion-exchange speed of glass can be accelerated, and have the compressive stress layers of the glass surface after ion-exchange process
There is higher compression stress and surface compression layer depth.
Na2O and Li2O content has shadow to the compression stress and surface compression layer depth of the compressive stress layers of glass surface
Ring, for example, the Na more than a certain amount of must be contained2O, just can guarantee that the compressive stress layers of glass surface after ion exchange has
Excellent compression stress and surface compression layer depth；During ion exchange, Li2O can make glass keep very high
Compression stress, but too high Li2Surface compression layer depth can be greatly reduced in O.In addition, Na in glass constituent2O and Li2O
Content influence compression stress and surface compression layer depth in terms of there is reciprocation, seek compression stress and surface compressive layer
Balance between depth, in certain embodiments, in mass, 0.03≤Li2O/(0.485Na2O+Li2O)≤0.3.If
Li2O/(0.485Na2O+Li2O value) is more than 0.3, although the glass after ion exchange can be made to have very high pressure
Stress under compression, but surface compression layer depth can significantly decline；If Li2O/(0.485Na2O+Li2O value) is less than 0.03, though then
The compressive stress layers of the glass after ion exchange, which can so be made, has an excellent surface compression layer depth, but compression stress
It can decline to a great extent.
Although boron oxygen network structure is rigidly smaller than silica network, there is bigger shape before glass body formation crackle can be allowed
Variable, but the B of high content2O3Glass ion exchange capacity can be obviously reduced.In order to seek between deformation quantity and ion-exchange capacity
Balance, in certain embodiments, the constituent of glass meets following relation：In mass, 2B2O3/(P2O5+
1.429Al2O3)≤0.11。
Although MgO and ZnO can reduce the fusion temperature of glass and prevent devitrification of glass, the two to glass from
Sub- exchange capacity and speed have certain inhibitory action, in order to seek the balance between above-mentioned various influences, in some implementations
In example, the constituent of glass meets following relation：By percentage to the quality, MgO+ZnO≤5%.
In some preferred embodiments, on the basis of oxide, according to mass percent meter, ion exchangeable glass
Including：
SiO2, 48%；
Na2O, 15.84%；
Al2O3, 30%；
P2O5, 1%；
B2O3, 0.27%；
MgO, 1.5%；
ZnO, 0.5%；
Li2O, 2.34%；
ZrO2, 0.1%；
CeO2, 0.15%；
SnO2, 0.3%.
Another aspect according to embodiments of the present invention there is provided a kind of preparation method of ion exchangeable glass, including：
The frit for the constituent that can form the glass that the embodiment of the present invention is provided on one side will be modulated into
Mixing；
Frit is melted and clarifying treatment, ion exchangeable glass is obtained after cooling.
During ion exchangeable glass is prepared, each that can be enumerated using first aspect present invention is constituted into
It is divided into raw material.Those skilled in the art should connect, during glass is prepared, and some physics may occur for glass ingredient
Chemical change so that exist between the constituent of raw material components and final obtained glass must difference, therefore, this area
Technical staff can also use other raw material components, as long as the raw material components can form one side of the embodiment of the present invention
The constituent of the glass of offer.
According to actual conditions, ion exchangeable glass can will be shaped to plate glass or both bulk glasses, the plate
Shape glass can be surface plate, and the platy structure that can also be bent, such as 3D cover plates, the present invention are not specially limited to this,
In some embodiments, by ion exchangeable glass be shaped to thickness be 1.1mm plate glass, for example, by machine cuts,
The techniques such as corase grind, fine grinding, polishing by ion exchangeable glass processing into thickness be 1.1mm plate glass.
There is provided a kind of glass of process ion exchange, the process ion for other side according to embodiments of the present invention
The glass of exchange has a constituent for the glass that the embodiment of the present invention the provides on one side, and with from its surface internally
The compressive stress layers of extension.
In certain embodiments, the compression stress of compressive stress layers is more than 850MPa, and surface compression layer depth is 50 μm
More than.
During ion exchange, nexine is answered in the compression that the salt ion that part ion is exchanged in liquid enters glass.For example,
When ion exchange liquid includes sylvite, compressive stress layers include potassium ion.
There is provided a kind of preparation method of the glass of process ion exchange, bag for still another aspect according to embodiments of the present invention
Include：
The frit for the constituent that can form the glass that the embodiment of the present invention is provided on one side will be modulated into
Melting, is configured to plate glass；
By the plate glass as carrying out ion exchange in ion exchange liquid.
Those skilled in the art can carry out ion friendship using ion exchange liquid commonly used in the art and ion-exchange process
Change, for example, ion exchange liquid includes KNO3；For another example the temperature of ion exchange be 425 DEG C, and/or, ion exchange when
Between be 2~10h.
It is illustrative to the glass of the present invention and preparation method thereof below based on some embodiments.
Embodiment 1-25
Each raw material components of glass are weighed, after being sufficiently mixed in mixer, are put into platinum crucible, and at 1670 DEG C
High temperature furnace under carry out 6h fusing and clarification.Glass metal is poured into graphite jig and is molded, and it is small in insulation half at 710 DEG C
When, furnace cooling afterwards obtains glass blocks.Again by machine cuts and roughly grind, fine grinding, be polished to thickness be 1.1mm tabular
Glass.
Table 1, table 2 are corresponding with composition and glass that table 3 lists glass ion exchangeable in embodiment 1-25 molten
Changing temperature, (glass metal viscosity is 102Temperature during dPas), density, modulus of elasticity, modulus of shearing, Poisson's ratio, molal volume,
Thermal coefficient of expansion (Thermal Expansion Coefficient, CTE), strain optical coefficient.Wherein, the measurement of fusion temperature is adopted
Measured with model ZH9866 glass High Temperature Rotating viscosity measuring instrument；Glass density uses model MH-200 direct-reading
Formula precision balance densimeter is measured；The modulus of elasticity of glass, modulus of shearing, Poisson's ratio are measured using WH-ki modulus of elasticity
Instrument is measured；The thermal coefficient of expansion of glass is measured using resistance to DIL 420PC thermal dilatometers of speeding, and takes room temperature to 300 DEG C
Average value；Strain optical coefficient (Stress-optical Coefficient, SOC) is determined by radial compression method.
The composition and measurement index of ion exchangeable glass in the embodiment 1-8 of table 1
The composition and measurement index of ion exchangeable glass in the embodiment 9-16 of table 2
| 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | |
| SiO2 | 49.37 | 49.35 | 57.92 | 48.00 | 51.86 | 48.00 | 48.00 | 53.22 |
| Na2O | 11.00 | 18.00 | 12.66 | 16.78 | 16.24 | 15.84 | 16.00 | 14.44 |
| Al2O3 | 25.37 | 27.23 | 17.00 | 30.00 | 26.14 | 30.00 | 26.00 | 25.51 |
| P2O5 | 5.94 | 1.54 | 5.95 | 1.00 | 1.00 | 1.00 | 3.16 | 1.51 |
| B2O3 | 1.81 | 0.91 | 0.00 | 0.00 | 0.00 | 0.27 | 2.00 | 0.00 |
| Li2O | 2.23 | 0.41 | 0.36 | 0.74 | 1.46 | 2.34 | 0.30 | 3.00 |
| MgO | 2.32 | 1.30 | 2.48 | 2.00 | 1.72 | 1.50 | 3.00 | 1.00 |
| ZnO | 0.90 | 0.76 | 2.48 | 0.50 | 1.25 | 0.50 | 1.10 | 1.00 |
| ZrO2 | 0.66 | 0.18 | 0.77 | 0.37 | 0.12 | 0.10 | 0.10 | 0.12 |
| CeO2 | 0.18 | 0.14 | 0.17 | 0.30 | 0.10 | 0.15 | 0.15 | 0.10 |
| SnO2 | 0.23 | 0.17 | 0.21 | 0.30 | 0.10 | 0.30 | 0.20 | 0.10 |
| Fusion temperature (DEG C) | 1637 | 1656 | 1550 | 1656 | 1617 | 1636 | 1644 | 1595 |
| Density (g/cm3) | 2.390 | 2.424 | 2.373 | 2.449 | 2.441 | 2.434 | 2.388 | 2.420 |
| Modulus of elasticity (GPa) | 84.01 | 79.39 | 78.51 | 80.71 | 80.51 | 82.37 | 81.62 | 81.68 |
| Modulus of shearing (GPa) | 35.01 | 32.81 | 32.82 | 33.30 | 33.34 | 34.04 | 33.73 | 33.95 |
| Poisson's ratio | 0.200 | 0.210 | 0.196 | 0.212 | 0.208 | 0.210 | 0.210 | 0.203 |
| Molal volume (cm3/mol) | 31.73 | 30.27 | 30.81 | 30.26 | 29.46 | 30.15 | 30.99 | 29.61 |
| CTE(×10-7/℃) | 75.3 | 88.9 | 75.4 | 86.9 | 88.8 | 87.6 | 84.7 | 88.5 |
| SOC(nm/cm/MPa) | 30.2 | 28.5 | 29.9 | 28.7 | 29.2 | 29.4 | 28.6 | 30.0 |
The composition and measurement index of ion exchangeable glass in the embodiment 17-25 of table 3
| 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| SiO2 | 58.00 | 54.99 | 52.83 | 48.00 | 61.00 | 59.50 | 58.00 | 58.00 | 54.00 |
| Na2O | 12.88 | 12.98 | 11.00 | 18.00 | 16.30 | 11.50 | 18.00 | 10.00 | 14.00 |
| Al2O3 | 17.86 | 24.53 | 24.59 | 25.00 | 17.00 | 21.00 | 13.78 | 17.00 | 18.00 |
| P2O5 | 5.39 | 2.89 | 6.00 | 6.00 | 0.00 | 0.00 | 1.20 | 6.00 | 2.00 |
| B2O3 | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 | 3.00 | 0.20 | 1.21 | 1.00 |
| Li2O | 0.30 | 1.34 | 2.29 | 0.30 | 0.00 | 0.00 | 3.00 | 2.00 | 6.00 |
| MgO | 1.87 | 1.51 | 1.06 | 1.00 | 5.40 | 5.00 | 3.00 | 3.00 | 2.00 |
| ZnO | 3.00 | 0.50 | 0.94 | 1.00 | 0.00 | 0.00 | 1.50 | 2.00 | 2.00 |
| ZrO2 | 0.43 | 1.00 | 0.92 | 0.36 | 0.30 | 0.00 | 1.00 | 0.50 | 1.00 |
| CeO2 | 0.13 | 0.13 | 0.13 | 0.13 | 0.00 | 0.00 | 0.16 | 0.14 | 0.00 |
| SnO2 | 0.14 | 0.13 | 0.25 | 0.21 | 0.00 | 0.00 | 0.16 | 0.15 | 0.00 |
| Fusion temperature (DEG C) | 1605 | 1631 | 1626 | 1578 | 1589 | 1662 | 1561 | 1608 | 1622 |
| Density (g/cm3) | 2.381 | 2.397 | 2.370 | 2.369 | 2.444 | 2.385 | 2.431 | 2.372 | 2.384 |
| Modulus of elasticity (GPa) | 1605 | 1631 | 1626 | 1578 | 1589 | 1662 | 80.56 | 81.93 | 85.47 |
| Modulus of shearing (GPa) | 2.381 | 2.397 | 2.370 | 2.369 | 2.444 | 2.385 | 33.34 | 34.33 | 35.50 |
| Poisson's ratio | 0.195 | 0.198 | 0.196 | 0.211 | 0.207 | 0.197 | 0.208 | 0.194 | 0.204 |
| Molal volume (cm3/mol) | 30.64 | 30.57 | 31.96 | 32.21 | 27.26 | 28.67 | 27.55 | 30.46 | 28.72 |
| CTE(×10-7/℃) | 75.6 | 75.7 | 75.1 | 87.1 | 86.7 | 78.5 | 95.6 | 76.5 | 96.4 |
| SOC(nm/cm/MPa) | 30.07 | 28.84 | 28.99 | 28.70 | 29.02 | 28.61 | 29.8 | 30.3 | 30.6 |
KNO by the glass obtained by embodiment 1-25 at 425 DEG C3Ion exchange is carried out in fused salt, after ion exchange terminates,
The compression stress (Compression Stress, CS) and surface compression layer depth (Depth of of glass are measured respectively
Compression Layer, DOL).The sequence number of the corresponding glass of the embodiment is used as using the numbering of embodiment respectively.Table 4 and table
5 show KNO of the serial number 1-25 glass at 425 DEG C3Fused salt intermediate ion exchanges the compression stress and surface measured by after 2h
Layer depth is compressed, table 6 and table 7 show KNO of the serial number 1-25 glass at 425 DEG C3Fused salt intermediate ion is surveyed after exchanging 3h
The compression stress and surface compression layer depth obtained, table 8 and table 9 show KNO of the serial number 1-25 glass at 425 DEG C3Fused salt
Intermediate ion exchanges compression stress and surface compression layer depth measured after 4h, and table 10 and table 11 show serial number 1-25's
KNO of the glass at 425 DEG C3Fused salt intermediate ion exchanges compression stress and surface compression layer depth measured after 6h, table 12 and table
13 show KNO of the serial number 1-25 glass at 425 DEG C3Fused salt intermediate ion exchanges the compression stress and table measured by after 10h
Face pressure contracting layer depth.
The 1-12 flint glass F ion exchanges 2h of table 4 compression stress and surface compression layer depth
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| CS(MPa) | 992 | 1001 | 966 | 968 | 998 | 987 | 1021 | 896 | 975 | 1030 | 878 | 999 |
| DOL(μm) | 42 | 39 | 41 | 42 | 44 | 43 | 45 | 36 | 42 | 45 | 32 | 51 |
The 13-25 flint glass F ion exchanges 2h of table 5 compression stress and surface compression layer depth
| 13 | 14 | 15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| CS(MPa) | 1015 | 1059 | 995 | 1043 | 882 | 932 | 943 | 1015 | 1050 | 850 | 1041 | 851 | 1070 |
| DOL(μm) | 41 | 50 | 44 | 40 | 32 | 43 | 50 | 52 | 31 | 26 | 29 | 30 | 25 |
The 1-12 flint glass F ion exchanges 3h of table 6 compression stress and surface compression layer depth
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| CS(MPa) | 981 | 993 | 962 | 958 | 994 | 980 | 1017 | 890 | 970 | 1024 | 872 | 993 |
| DOL(μm) | 51 | 47 | 53 | 53 | 56 | 53 | 55 | 43 | 54 | 56 | 40 | 60 |
The 13-25 flint glass F ion exchanges 3h of table 7 compression stress and surface compression layer depth
| 13 | 14 | 15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| CS(MPa) | 1007 | 1055 | 990 | 1039 | 876 | 927 | 938 | 1010 | 1038 | 836 | 1034 | 840 | 1065 |
| DOL(μm) | 52 | 60 | 53 | 51 | 41 | 52 | 58 | 62 | 35 | 31 | 34 | 32 | 27 |
The 1-12 flint glass F ion exchanges 4h of table 8 compression stress and surface compression layer depth
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| CS(MPa) | 974 | 987 | 951 | 954 | 985 | 973 | 1014 | 887 | 964 | 1018 | 862 | 989 |
| DOL(μm) | 62 | 57 | 61 | 62 | 65 | 62 | 65 | 55 | 66 | 63 | 51 | 69 |
The 13-25 flint glass F ion exchanges 4h of table 9 compression stress and surface compression layer depth
| 13 | 14 | 15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| CS(MPa) | 1003 | 1050 | 984 | 1036 | 865 | 923 | 932 | 1004 | 1031 | 825 | 1023 | 836 | 1062 |
| DOL(μm) | 60 | 68 | 62 | 59 | 52 | 61 | 68 | 70 | 39 | 35 | 38 | 34 | 29 |
The 1-12 flint glass F ion exchanges 6h of table 10 compression stress and surface compression layer depth
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| CS(MPa) | 950 | 966 | 932 | 929 | 966 | 953 | 990 | 865 | 946 | 1000 | 840 | 965 |
| DOL(μm) | 66 | 61 | 67 | 65 | 70 | 66 | 69 | 59 | 71 | 67 | 56 | 73 |
The 13-25 flint glass F ion exchanges 6h of table 11 compression stress and surface compression layer depth
| 13 | 14 | 15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| CS(MPa) | 973 | 1025 | 960 | 950 | 845 | 890 | 867 | 951 | 1020 | 811 | 1002 | 830 | 1051 |
| DOL(μm) | 66 | 73 | 66 | 63 | 57 | 65 | 72 | 74 | 43 | 40 | 41 | 37 | 32 |
The 1-12 flint glass F ion exchanges 10h of table 12 compression stress and surface compression layer depth
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | |
| CS(MPa) | 842 | 841 | 830 | 821 | 836 | 815 | 846 | 781 | 808 | 810 | 752 | 820 |
| DOL(μm) | 70 | 65 | 71 | 72 | 75 | 70 | 76 | 63 | 76 | 72 | 63 | 78 |
The 13-25 flint glass F ion exchanges 10h of table 13 compression stress and surface compression layer depth
| 13 | 14 | 15 | 16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
| CS(MPa) | 834 | 840 | 820 | 846 | 755 | 789 | 780 | 832 | 961 | 721 | 965 | 812 | 1023 |
| DOL(μm) | 73 | 78 | 70 | 67 | 65 | 71 | 77 | 80 | 48 | 51 | 47 | 43 | 38 |
Fig. 1 reaches the minimum time required during 50 μm of surface compression layer depth for the glass Jing Guo ion exchange,
Compression stress value below icon for correspondence glass now.Wherein 21, KNO of the 23-25 flint glass Fs at 425 DEG C3Fused salt intermediate ion
It is respectively 48 μm, 47 μm, 43 μm, 38 μm, not up to 50 μm to exchange surface compression layer depth after 10h；Although 22 flint glass Fs
Surface compression layer depth has reached 51 μm, but its compression stress is smaller, only 721MPa.
From the data in table 1-13 it can be found that KNO of the 1-20 flint glass Fs at 425 DEG C3It is small that fused salt intermediate ion exchanges 2-4
When, the surface compression layer depth of glass can at least reach 50 μm, and now the stress value of glass in more than 850MPa.No. 21 and
The alkali content of 23 flint glass Fs is higher, although the glass after ion exchange can be made to have a larger compression stress value, but glass
Cyberspace it is smaller, surface compression layer depth and ion-exchange speed are much smaller than 1-20 flint glass Fs.After ion exchange 10h,
The surface compression layer depth of 21 flint glass Fs just reach 48 μm, the surface compression layer depth of 23 flint glass Fs just reach 47 μm.
B content is too high in 22 flint glass Fs, very strongly weakens the ion-exchange capacity of glass, and glass after ion exchange
The compressive stress layers of glass occur in that larger stress relaxation.As the KNO at 425 DEG C3Fused salt intermediate ion is exchanged after 10h, No. 22 glass
When the surface compression layer depth of glass reaches 51 μm, corresponding compression stress value only has 721MPa.
It is due to that alkali metal content is too low although 24 flint glass F cyberspaces are big, causes ion exchange power serious not
Foot, therefore, compression stress value and surface compression layer depth after its ion exchange are far smaller than under same ion give-and-take conditions
The compression stress value and surface compression layer depth of 1-20 flint glass Fs.When 24 flint glass Fs are in 425 DEG C of KNO3Fused salt intermediate ion is exchanged
After 10h, compression stress value and surface compression layer depth are still relatively low, only 812MPa and 43 μm.
Li too high levels in the composition of 25 flint glass Fs, cause in ion exchange process is carried out, and causes network excessive
It is jammed, so its compression stress value under same ion give-and-take conditions is much larger than other glass.Inside glass network it is excessive
It is jammed seriously to hinder migration of the ion to depth direction, therefore surface compression of 25 flint glass Fs under same ion give-and-take conditions
Layer depth is much smaller than other glass, as shown in table 13, in 425 DEG C of KNO3Fused salt intermediate ion is exchanged after 10h, surface compression layer depth
Degree only reaches 38 μm.
Above-mentioned embodiment, does not constitute limiting the scope of the invention.Those skilled in the art should be bright
It is white, depending on design requirement and other factors, can occur various modifications, combination, sub-portfolio and replacement.It is any
Modifications, equivalent substitutions and improvements made within the spirit and principles in the present invention etc., should be included in the scope of the present invention
Within.
Claims (10)
1. a kind of ion exchangeable glass, it is characterised in that on the basis of oxide, according to mass percent meter, including：
SiO2, 48%~58%；
Na2O, 11%~18%；
Al2O3, 17%~30%；
P2O5, 1%~6%；
B2O3, 0%~2%；
MgO, 1%~3%；
ZnO, 0.5%~3%；
Li2O, 0.3%~3%；
ZrO2, 0.1%~1%；
CeO2, 0.1%~0.3%；
SnO2, 0.1%~0.3%.
2. glass as claimed in claim 1, it is characterised in that according to mass percent meter, SiO2+Al2O3+P2O5+B2O3≥
79%.
3. glass as claimed in claim 1, it is characterised in that according to mass percent meter, 0.32%≤ZrO2+CeO2+SnO2
≤ 1.3%.
4. glass as claimed in claim 1, it is characterised in that according to quality meter, 0.5≤CeO2/SnO2≤1。
5. glass as claimed in claim 1, it is characterised in that according to quality meter, 0.2≤(Al2O3+0.7P2O5+1.4B2O3)/
1.7SiO2≤ 0.5, and/or, 0.65≤(Al2O3+1.4B2O3)/(0.7P2O5+1.6Na2O+3.3Li2O)≤1。
6. glass as claimed in claim 1, it is characterised in that according to quality meter, 0.03≤Li2O/(0.485Na2O+Li2O)
≤ 0.3, and/or, 2B2O3/(P2O5+1.429Al2O3)≤0.11。
7. glass as claimed in claim 1, it is characterised in that according to mass percent meter, MgO+ZnO≤5%.
8. a kind of preparation method of ion exchangeable glass, it is characterised in that including：
The frit for being modulated into the constituent that can form claim 1-7 any one glass is mixed；
The frit is melted and clarifying treatment, the ion exchangeable glass is obtained after cooling.
9. a kind of glass of process ion exchange, it is characterised in that the glass of the process ion exchange has such as claim
The constituent of any described glass of 1-7, and with the compressive stress layers extended inward from its surface.
10. a kind of preparation method of the glass of process ion exchange, it is characterised in that including：
The frit melting for the constituent that can form claim 1-7 any one glass will be modulated into, be configured to plate
Shape glass；
By the plate glass as carrying out ion exchange in ion exchange liquid.
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| CN108821568A (en) * | 2018-07-27 | 2018-11-16 | 彩虹显示器件股份有限公司 | A kind of high surface hardness glass of alkali metal containing and preparation method thereof |
| WO2020177271A1 (en) * | 2019-03-07 | 2020-09-10 | 科立视材料科技有限公司 | Lithium-containing glass having low softening point |
| CN110642514A (en) * | 2019-10-10 | 2020-01-03 | 清远南玻节能新材料有限公司 | Aluminosilicate glass, tempered glass, preparation methods of aluminosilicate glass and tempered glass, cover plate, back plate and device |
| CN110981187A (en) * | 2019-12-05 | 2020-04-10 | 四川旭虹光电科技有限公司 | Alkali-containing glass and strengthening method thereof |
| CN110981187B (en) * | 2019-12-05 | 2022-05-31 | 四川虹科创新科技有限公司 | Alkali-containing glass and strengthening method thereof |
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