CN110304839A - A kind of intensifying method and fortified compositions of the glass of whiteware containing lithium - Google Patents
A kind of intensifying method and fortified compositions of the glass of whiteware containing lithium Download PDFInfo
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- CN110304839A CN110304839A CN201810257814.1A CN201810257814A CN110304839A CN 110304839 A CN110304839 A CN 110304839A CN 201810257814 A CN201810257814 A CN 201810257814A CN 110304839 A CN110304839 A CN 110304839A
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- fused salt
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- whiteware
- additive
- containing lithium
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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
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
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Abstract
The present invention provides the intensifying method and fortified compositions of a kind of glass of whiteware containing lithium, and the method includes using by NaNO3The fused salt of composition handles the glass of whiteware containing lithium, the method also includes the additives that the at a temperature of addition in the fused salt at 300 DEG C or more includes sodium carbonate and special adsorbent, the special adsorbent is selected from one of metasilicic acid, diatomite and aluminium oxide or a variety of, and it is 100:0.5~4:0.1~1 that additive amount, which is the weight ratio of the fused salt, sodium carbonate and special adsorbent,.The lithium ion in fused salt is held by adding sodium carbonate in the present invention, prevent lithium ion from coming back in whiteware glass, and the impurity in sodium nitrate fused salt is wrapped up in the present invention by special adsorbent and is deposited to reinforcing furnace bottom, so that the service life of fused salt greatly improves.The method of the invention successfully imports volume production, and the glass reinforced production efficiency of whiteware has obtained great promotion, and production cost is greatly reduced.
Description
Technical field
Back-cover or other component white (opaque) glass-ceramic of the present invention for mobile phone, tablet computer, Mac etc.
Chemical strengthening technique, the intensifying method and fortified compositions of specifically a kind of glass of whiteware containing lithium.
Background technique
Whiteware devitrified glass has the deep appearance and texture liked by market, and intensity is high after chemical strengthening, wear-resisting
Drop resistant is had excellent performance, thus is widely used in the back-covers such as mobile phone, wrist-watch, plate or other components.
Such as the whiteware devitrified glass of Corning Incorporated's exploitation is lithium base glass, chemical strengthening uses primary reinforcement work
Skill uses 100% sodium nitrate fused salt, the sodium ion exchange in lithium ion and fused salt in glass and it is white after being strengthened
Color glass-ceramic.
In the prior art in the NaNO using 100%3When fused salt strengthens the glass of whiteware containing lithium, with enhanced products number
Li in the fused salt of furnace is strengthened in the increase of amount+Concentration constantly rises, ion-exchange capacity decline, under the surface strength of product is significant
Drop, if its value is less than < 500Mpa, exceeds when using destructive four-point bending method test product surface strength after reinforcing
The minimum surface intensity value standard LSL that client determines.NaNO is corresponded to using this intensifying method3The service life of fused salt only 4 furnaces (such as
Every furnace strengthens 3360 glass of whiteware containing lithium).
That is, the production for completing a furnace product every in the prior art, can extract the four of 10 sample test products
Point bending stresses (4PB), if exceeding defined critical field LSL, i.e. stopping table production clears up furnace water, cleans table, add
Add new salt, puts into production next time.The technique is significant adverse to cost control, therefore this field needs a kind of new pottery of white containing lithium
The intensifying method of porcelain glass.
Patent of invention CN201210328761 provides a kind of manufacturing method of chemcor glass product, in chemical strengthening
In the service life that can keep fused salt in processing longlyer, the strengthened glass product of stability of characteristics can be obtained.The chemcor glass system
The manufacturing method of product includes ion-exchange process, and the ion-exchange process is by making the glassware of the composition containing Li and containing
The fused salt molten liquid for having ionic radius to be greater than the alkali metal element of Li contained in the glass is in contact, will be in the glassware
Li and the fused salt molten liquid in alkali metal carry out ion exchange.Wherein, in above-mentioned fused salt molten liquid, addition is selected from
NaF、KF、K3AlF6、Na2CO3、NaHCO3、K2CO3、KHCO3、Na2SO4、K2SO4、KAl(SO4)2、Na3PO4、K3PO4In at least
A kind of additive, the additive carry out above-mentioned ion-exchange process with solid state.
But for above-mentioned 100% NaNO3Fused salt (itself can bring some impurity such as calcium ion or magnesium ion into) in fused salt
For, it adds the above-mentioned salt containing potassium and (it is few to contain sodium ion in whiteware glass, is not required to the exchange of potassium sodium, thus adds potassium in fused salt
Salt can bring unwanted element in product into) obviously it is unfavorable for entirely strengthening.Adding above-mentioned is, for example, Na2CO3、Na2SO4With
Na3PO4At least one additive when, NaNO3The service life of fused salt is not improved or the raising of fused salt service life is unobvious.
Therefore, this field urgently develop a kind of whiteware containing lithium it is glass reinforced when NaNO3The method that the fused salt service life improves.
Summary of the invention
Therefore, the present invention provides a kind of intensifying method of glass of whiteware containing lithium, including uses by NaNO3Composition melts
The glass of whiteware containing lithium described in salt treatment, the method also includes in the fused salt 300 DEG C or more at a temperature of be added
Additive comprising sodium carbonate and special adsorbent, the special adsorbent are in metasilicic acid, diatomite and aluminium oxide
It is one or more, and it is 100:0.5~4:0.1 that additive amount, which is the weight ratio of the fused salt, sodium carbonate and special adsorbent,
~1.
In a specific embodiment, the reinforcing temperature of the glass of whiteware containing lithium is 420~450 DEG C, and every
The enhanced time of the furnace glass of whiteware containing lithium is 5~9 hours.
In a specific embodiment, the weight ratio of the fused salt, sodium carbonate and special adsorbent is 100:1~2:
0.2~0.5.
In a specific embodiment, the special adsorbent is metasilicic acid and/or aluminium oxide.
In a specific embodiment, after the additive is added in fused salt, make fused salt within standing 2 hours or more
It comes into full contact with to react with additive and is put into the glass of whiteware containing lithium to be fortified in fused salt again.
In a specific embodiment, after the additive is added in fused salt, again molten after standing 3~40 hours
Salt is put into the glass of whiteware containing lithium to be fortified.
In a specific embodiment, the additive and fused salt are added into fused salt and additive stands reaction process
In, the temperature of fused salt is maintained at 420~450 DEG C.
Another object of the present invention provides a kind of fortified compositions of glass of whiteware containing lithium, including by NaNO3Composition
Fused salt and additive, the additive include sodium carbonate and special adsorbent, the special adsorbent be selected from metasilicic acid, silicon
One of diatomaceous earth and aluminium oxide are a variety of, and the weight ratio of fused salt, sodium carbonate and special adsorbent is 100:0.5 in composition
~4:0.1~1.
The present invention at least has the following beneficial effects:
1) lithium ion in fused salt is held by adding sodium carbonate in the present invention, prevents lithium ion from coming back to white pottery
In porcelain glass, at the same sodium carbonate in fused salt impurity calcium ion and magnesium ion etc. also there is certain constraint to act on, and the present invention
In by special adsorbent by sodium nitrate fused salt calcium ion and the impurity such as magnesium ion wrap up and deposit to reinforcing furnace bottom, it is special
Foreign ion in sodium carbonate can also be locked and bring reinforcing furnace bottom by adsorbent, so that the service life of fused salt substantially mentions
It is high.
2) the method for the invention successfully imports volume production, and the glass reinforced production efficiency of whiteware has obtained greatly mentioning
It rises, and production cost is greatly reduced.
Detailed description of the invention
Fig. 1 is whiteware glass 4PB value (four-point bending intensity) variation diagram after strengthening in comparative example 1.
Fig. 2 is whiteware glass 4PB value (four-point bending intensity) variation diagram after strengthening in embodiment 1.
Specific embodiment
The present invention is described in detail by following examples and comparative examples and attached drawing.
Comparative example 1
As shown in Figure 1, being provided in comparative example 1 existing to the strong of white glass-ceramic (healthy and free from worry whiteware glass 9667)
Change method, the sodium nitrate using 100% are fused salt, and every furnace is strengthened 7 hours at 430 DEG C.The average 4PB value of first furnace product is
756MPa, the average 4PB value of the 4th furnace product are 526MPa.The four-point bending intensity value decline of every furnace product is quickly.
Embodiment 1
As shown in Fig. 2, the present invention provides a kind of intensifying method of glass of whiteware containing lithium, including use by NaNO3Group
At fused salt handle the glass of whiteware containing lithium, the method also includes in the fused salt 430 DEG C at a temperature of add
Entering includes the additive of sodium carbonate and special adsorbent, stands reaction 2 hours or more and adds whiteware glass to be fortified,
The special adsorbent is selected from one of metasilicic acid, diatomite and aluminium oxide or a variety of, and additive amount is described molten
The weight ratio of salt, sodium carbonate and special adsorbent is 100:1~2:0.2~0.5.
In a specific embodiment, the reinforcing temperature of the glass of whiteware containing lithium is 420~450 DEG C, and every
The enhanced time of the furnace glass of whiteware containing lithium is 5~9 hours.
Specifically, additive formulations and ratio are fused salt in the present embodiment: Na2CO3: Al2O3=1:1wt%:
0.5wt%.The Al being added in the present invention2O3Can be with adsorbing contaminant ion, such as Ca, Mg foreign ion brought into fused salt is eliminated
Its adverse effect to product strength；And the Na being added in the present invention2CO3The Li being precipitated from whiteware glass can be eliminated+It is right
The intensity effect of reinforcing.After importing this additive, the furnace water service life is promoted to 10 furnaces, raising efficiency 150% by 4 original furnaces.I.e.
The service life for strengthening furnace water is 2.5 times originally.
Comparative example 2
It only include aluminium oxide in additive, without containing sodium carbonate, other conditions are all same as Example 1.
Experiment discovery, when only not having to sodium carbonate with aluminium oxide, one is obtained the enhanced products of six furnaces qualification.First furnace is to
The average 4PB intensity value (units MPa) of the product of six furnaces is respectively 932,885,802,708,646 and 521, more any than not adding
4 furnaces of additive are compared, and 2 furnaces are increased.It can be seen that from the experimental data in first furnace, because strengthening lithium ion in fused salt
Content is few, and strengthens the calcium ion in fused salt and magnesium ion has enumerated in full detail and has been oxidized aluminium absorption and deposits to furnace bottom.Thus first furnace is strong
The four-point bending intensity value for changing product is maintained at a higher level.And increase with furnace number is strengthened, the lithium ion in fused salt
Be carbonated not in time in sodium carbonate constraint, thus later in several furnaces the four-point bending intensity value of product declines rapidly.Cause
This, when being only additive with aluminium oxide, increases service life of sodium nitrate fused salt that the effect is unsatisfactory.
Comparative example 3
It only include sodium carbonate in additive, without salic, other conditions are all same as Example 1.
Experiment discovery when not having to aluminium oxide, can also obtain altogether the enhanced products of six furnaces qualification only with sodium carbonate.First
The average 4PB intensity value (units MPa) of product of furnace to the 6th furnace is respectively 785,748,692,643,581 and 538, than not adding
Add 4 furnaces of any additive to compare, also increases 2 furnaces.From the experimental data can be seen that because lack special adsorbent to by
The sedimentation removal of impurities of the calcium ion and magnesium ion brought into sodium nitrate fused salt acts on, thus in first furnace, the four-point bending of product is strong
Angle value just only maintains one not counting high level.And because having added sodium carbonate in fused salt, constraint is primarily served from glass
Be discharged into the effect of the lithium ion in fused salt, also can to by being brought into sodium nitrate fused salt calcium ion and magnesium ion play it is slight
Constraint effect, thus it is inviolent in the decline of the four-point bending intensity value of the enhanced products of the 2nd~6 furnace.But it generally speaking, only uses
When sodium carbonate is additive, it is also unsatisfactory that effect is increased to the service life of sodium nitrate fused salt.
In addition, being equably sprinkled into described add from the top for strengthening furnace specifically, additive in the present invention is solid particle
Add agent, then the reaction product of the fused salt added with additive is allowed slowly to be settled down to furnace bottom.
In the embodiment of the present invention 1, added with additive sodium nitrate fused salt after strengthening 10 furnaces whiteware containing lithium glass, furnace
The white solid particle height of bottom sediments is not high.Even if but having used this above-mentioned addition of addition again in the fused salt after 10 furnaces
Agent can make the service life of fused salt slightly extend again, such as the four-point bending intensity value of the enhanced products after the 11st furnace still closes
Lattice.But for comprehensively considering, the operation achievement that additive is added again is too small, has no improvement to total reinforcing efficiency.
Therefore, the sodium nitrate fused salt service life is significantly improved in order to obtain, needs to use sodium carbonate and special in the present invention
Adsorbent combination can achieve the goal.
In addition, inventor can not use other salt such as sodium phosphate to replace the carbonic acid in the additive through overtesting discovery
Sodium, when using sodium phosphate to cooperate as the component of additive and the special adsorbent, the glass product stress after reinforcing is different
Often, the stress value of glass is low, each point stress data disorder observed, Stress non-homogeneity between the divided glass of same furnace, difference
It is very big.It is thus impossible to replace the sodium carbonate in the present invention using sodium phosphate or other salt.In addition, sodium bicarbonate is because of meeting of being heated
It decomposes and generates gas, so that strengthening process becomes dangerous, thus the additive in the present invention does not use sodium bicarbonate yet.
In a specific embodiment, the reinforcing temperature of the glass of whiteware containing lithium is 420~450 DEG C, and every
The enhanced time of the furnace glass of whiteware containing lithium is 5~9 hours.When reinforcing temperature is too low, the enhanced time needed is too long；Strengthen
When temperature is too high, sodium nitrate is easily decomposed to nitrite and unfavorable to strengthening.Enhanced time is too short be easy to cause it is glass reinforced
Depth it is inadequate；Stress is too high when enhanced time is too long, and glass easily bursts.And according to the difference of thickness of glass, enhanced time is omited
Different such as thicker glass uses longer enhanced time.
In a specific embodiment, the special adsorbent is metasilicic acid and/or aluminium oxide.
In the present invention, the special adsorbent is played the calcium ion and magnesium ion brought into sodium nitrate fused salt package and band
Move its effect for depositing to furnace bottom.Graphite and active carbon drive these impurity to deposit to furnace bottom, thus the present invention because can not be successfully
It is middle to cannot get good fused salt cleaning effect when being combined as additive using graphite or active carbon and sodium carbonate.The present invention
In, especially preferred special adsorbent is metasilicic acid and/or aluminium oxide, because diatomite carry impurity deposit to the speed of furnace bottom compared with
Slowly, thus after diatomite is added in the fused salt in the present invention, needing to spend can make impurity all deposit to for 18 hours or so
Furnace bottom；And when using metasilicic acid and/or aluminium oxide, probably standing 3 hours may make impurity all smoothly to deposit to furnace bottom.
In the present invention, the impurity such as calcium ion and magnesium ion for bringing into sodium nitrate fused salt are even common to simple glass
The influence of reinforcing generation containing lithium glass is simultaneously little, but these impurity are strong to the four-point bending of the reinforcing of the glass of whiteware containing lithium
Angle value but influences significantly.Thus improve the service life of fused salt in the present invention by above-mentioned additive.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of intensifying method of the glass of whiteware containing lithium, including use by NaNO3The fused salt processing of composition is described containing lithium white
Glass-ceramic includes sodium carbonate and special suction the method also includes the at a temperature of addition in the fused salt at 300 DEG C or more
Attached dose of additive, the special adsorbent are selected from one of metasilicic acid, diatomite and aluminium oxide or a variety of, and additive
Dosage is that the weight ratio of the fused salt, sodium carbonate and special adsorbent is 100:0.5~4:0.1~1.
2. intensifying method according to claim 1, which is characterized in that the reinforcing temperature of the glass of whiteware containing lithium is
420~450 DEG C, and the enhanced time of every furnace whiteware containing lithium glass is 5~9 hours.
3. intensifying method according to claim 1, which is characterized in that the weight of the fused salt, sodium carbonate and special adsorbent
Amount is than being 100:1~2:0.2~0.5.
4. intensifying method according to claim 1, which is characterized in that the special adsorbent is metasilicic acid and/or oxidation
Aluminium.
5. intensifying method described according to claim 1~any one of 4, which is characterized in that be added by the additive
After in fused salt, stand 2 hours more than make fused salt come into full contact with to react to be put into fused salt again with additive and to be fortified contain lithium
Whiteware glass.
6. intensifying method according to claim 5, which is characterized in that after the additive is added in fused salt, stand 3
It is put into the glass of whiteware containing lithium to be fortified after~40 hours in fused salt again.
7. intensifying method described according to claim 1~any one of 4, which is characterized in that add described in being added into fused salt
Agent and fused salt and additive is added to stand in reaction process, the temperature of fused salt is maintained at 420~450 DEG C.
8. a kind of fortified compositions of the glass of whiteware containing lithium, including by NaNO3The fused salt and additive of composition, feature exist
In the additive includes sodium carbonate and special adsorbent, and the special adsorbent is selected from metasilicic acid, diatomite and aluminium oxide
One of or it is a variety of, and in composition fused salt, sodium carbonate and special adsorbent weight ratio be 100:0.5~4:0.1~1.
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| CN201810257814.1A CN110304839A (en) | 2018-03-27 | 2018-03-27 | A kind of intensifying method and fortified compositions of the glass of whiteware containing lithium |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111116057A (en) * | 2019-12-31 | 2020-05-08 | 河南裕展精密科技有限公司 | Chemical strengthening additive and method for chemical strengthening using the same |
| CN112194386A (en) * | 2020-09-14 | 2021-01-08 | 深圳市辰美科技有限公司 | Process flow of 3D glass lens |
| WO2021113237A1 (en) * | 2019-12-02 | 2021-06-10 | Corning Incorporated | Methods to mitigate haze induced during ion exchange with carbonate salts |
| JP2021104915A (en) * | 2019-12-26 | 2021-07-26 | Ａｇｃ株式会社 | Method for producing chemically strengthened glass and lithium ion adsorbent |
| CN113233789A (en) * | 2021-06-30 | 2021-08-10 | 重庆鑫景特种玻璃有限公司 | Recycling method of reinforced microcrystalline glass |
| CN113845315A (en) * | 2021-10-21 | 2021-12-28 | 成都光明光电股份有限公司 | Ion exchange salt bath additive |
| CN115477480A (en) * | 2021-06-15 | 2022-12-16 | 常熟佳合显示科技有限公司 | Strengthening salt and strengthening method for microcrystalline glass |
| CN116023043A (en) * | 2022-12-27 | 2023-04-28 | 富联科技(兰考)有限公司 | Glass chemical strengthening additive and glass chemical strengthening method |
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| JPS61178004A (en) * | 1985-02-05 | 1986-08-09 | Nippon Sheet Glass Co Ltd | Treatment of molten salt |
| CN102951850A (en) * | 2012-11-23 | 2013-03-06 | 浙江大学 | Preparation method of chemical toughened glass product with wearing-resisting film |
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| JPS61178004A (en) * | 1985-02-05 | 1986-08-09 | Nippon Sheet Glass Co Ltd | Treatment of molten salt |
| CN102951850A (en) * | 2012-11-23 | 2013-03-06 | 浙江大学 | Preparation method of chemical toughened glass product with wearing-resisting film |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021113237A1 (en) * | 2019-12-02 | 2021-06-10 | Corning Incorporated | Methods to mitigate haze induced during ion exchange with carbonate salts |
| CN114787095A (en) * | 2019-12-02 | 2022-07-22 | 康宁股份有限公司 | Method for reducing haze caused during ion exchange using carbonate salts |
| JP2021104915A (en) * | 2019-12-26 | 2021-07-26 | Ａｇｃ株式会社 | Method for producing chemically strengthened glass and lithium ion adsorbent |
| JP7283380B2 (en) | 2019-12-26 | 2023-05-30 | Ａｇｃ株式会社 | Chemically strengthened glass manufacturing method and lithium ion adsorbent |
| CN111116057A (en) * | 2019-12-31 | 2020-05-08 | 河南裕展精密科技有限公司 | Chemical strengthening additive and method for chemical strengthening using the same |
| CN112194386A (en) * | 2020-09-14 | 2021-01-08 | 深圳市辰美科技有限公司 | Process flow of 3D glass lens |
| CN115477480A (en) * | 2021-06-15 | 2022-12-16 | 常熟佳合显示科技有限公司 | Strengthening salt and strengthening method for microcrystalline glass |
| CN113233789A (en) * | 2021-06-30 | 2021-08-10 | 重庆鑫景特种玻璃有限公司 | Recycling method of reinforced microcrystalline glass |
| CN113845315A (en) * | 2021-10-21 | 2021-12-28 | 成都光明光电股份有限公司 | Ion exchange salt bath additive |
| CN116023043A (en) * | 2022-12-27 | 2023-04-28 | 富联科技(兰考)有限公司 | Glass chemical strengthening additive and glass chemical strengthening method |
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