CN110304840A - A kind of intensifying method and fortified compositions containing lithium glass - Google Patents
A kind of intensifying method and fortified compositions containing lithium glass Download PDFInfo
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- CN110304840A CN110304840A CN201810257945.XA CN201810257945A CN110304840A CN 110304840 A CN110304840 A CN 110304840A CN 201810257945 A CN201810257945 A CN 201810257945A CN 110304840 A CN110304840 A CN 110304840A
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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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Abstract
The present invention provides a kind of intensifying method containing lithium glass, including uses by KNO3And NaNO3The fused salt mixt processing of composition is described to contain lithium glass, and wherein KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, the method also includes the additive comprising sodium phosphate and special adsorbent is added in the fused salt mixt, the special adsorbent is selected from one of metasilicic acid, diatomite and aluminium oxide or a variety of, and it is 100:0.3~0.6:0.2~0.5 that the additive amount being added every time, which is the weight ratio of the fused salt mixt, sodium phosphate and special adsorbent,.Generation lithium phosphate is reacted with the lithium ion in fused salt mixt by adding sodium phosphate in the present invention, and the lithium phosphate of generation is wrapped up to by special adsorbent and deposited to reinforcing furnace bottom, so that the service life of fused salt mixt improves several times.The present invention correspondingly provides a kind of fortified compositions.The method of the invention successfully imports volume production, and glass reinforced production efficiency has obtained great promotion, and production cost is greatly reduced.
Description
Technical field
The present invention is specifically a kind of to contain for touched panel glass panel chemistry reinforcement process such as mobile phone, tablet computer, Mac
The intensifying method and fortified compositions of lithium glass.
Background technique
Containing lithium glass eventually for the equipment such as mobile phone, tablet computer, Mac glass panel when need to first pass through it is chemical strong
Change, chemically reinforced glass has that intensity is high, stress is uniform, stability is good, can cutting processing and not generate optical distortion etc. excellent
Performance is widely used in mobile phone screen, wrist-watch eyeglass, advanced optical camera lens etc..The Gorilla P series glass of Corning Incorporated's exploitation
With its excellent damage-retardation performance, antiscratching properties energy, it is widely used in Novel high-end mobile phone screen.
Such as the P series glass of Gorilla 5 and 6 of Corning Incorporated's exploitation belongs to high aluminosilicate lithium base glass, contains in glass
Some lithium ions and sodium ion, which need to replace from glass panel by chemical strengthening, to be come out.Existing chemical strengthening technique is adopted
With primary reinforcement technique, the ion exchange carried out simultaneously containing two kinds: one is the sodium ions in the lithium ion and fused salt in glass
Exchange, another kind is that the sodium ion in glass is exchanged with the potassium ion in fused salt.Thus the glass reinforced fused salt is all nitric acid
The fused salt mixt of sodium and potassium nitrate composition.Wherein the exchange process of sodium ion is very fast and general in the lithium ion and fused salt in glass
Exchange depth in glass is deeper, and in the sodium ion and fused salt in glass potassium ion exchange process because potassium ion volume compared with
Big and general only depth certain near glass surface exchanges.For example using KNO in the prior art3Content be 90~
98wt% and NaNO3The fused salt mixt that content is 2~10wt% strengthens when containing lithium glass, with the increasing of strengthened glass product quantity
Add, strengthens Li in the fused salt mixt in furnace+Concentration constantly rises, and ion-exchange capacity decline, the expansion of product is (because volume is larger
Sodium ion replacement glass in small volume lithium ion and volume biggish potassium ion replacement glass in small volume sodium
Ion, thus it is glass reinforced during product expand) do not reach requirement gradually, work as Li+Concentration rises to 220-280ppm, produces
Product expansion is reduced to original 80%, and corresponding stress value declines (the minimum stress required value LSL of <), fused salt end-of-life, by force
Furnace water (fused salt mixt) service life for changing furnace only has 4 furnaces.That is, in the prior art one furnace of every completion (such as every furnace strengthen
2280 sheet glass) product production after, can test product surface stress value and product size.If product surface stress value or product
Size exceeds defined critical field, i.e. the production of stopping table, clears up furnace water, cleans table, add new salt, secondary under investment
It produces.The technique is significant adverse to cost control.
Patent application CN201710525829.7 be related to it is a kind of extend the glass reinforced method with fused salt service life, belong to
Glass working arts field.Wherein, in order to solve the problems, such as that existing service life is low, a kind of extension fused salt service life is provided
Glass reinforced method, this method includes that will be used to tempering fused salt and first pass through heat treatment in advance and make to reach molten condition form melting
Liquid；The tempering fused salt includes sodium nitrate and potassium nitrate, specifically KNO3Content is 35~45wt% and NaNO3Content be 55~
65wt%；Glass containing lithium ion to be fortified is put into molten liquid, then sodium phosphate is added into molten liquid and controls temperature and exists
Intensive treatment is carried out under conditions of 350 DEG C~400 DEG C；By after the glass of intensive treatment takes out cooling, passed through accordingly
Cross the glass after strengthening.The invention can be realized preferable strengthening effect and guarantee the service life of fused salt.And in the invention
Potassium titanium oxide phosphate and/or powdered graphite are further preferably added in strengthening fused salt.
But for certain containing KNO used in lithium glass3Content is 90~98wt% and NaNO3Content is 2~10wt%'s
For fused salt mixt, sodium phosphate processing fused salt mixt is individually added or using sodium phosphate and potassium titanium oxide phosphate and/or powdered graphite
Handling fused salt mixt all can not biggish raising fused salt service life.
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 KNO3Content is 90~98wt% and NaNO3Content is to add for the fused salt mixt of 2~10wt%
In addition stating for example, Na2CO3At least one additive when, the service life of fused salt mixt is not improved significantly, and is also possible to lead
Cause the product after strengthening unqualified.
It would therefore be highly desirable to KNO when developing a kind of reinforcing containing lithium glass3Content is 90~98wt% and NaNO3Content be 2~
The method that the fused salt mixt service life of 10wt% improves.
Summary of the invention
Therefore, the present invention provides a kind of intensifying method containing lithium glass, including uses by KNO3And NaNO3The mixing of composition
Fused salt processing is described to contain lithium glass, and wherein KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, the method
Further include in the fused salt mixt be added include sodium phosphate and special adsorbent additive, the special adsorbent be selected from
One of metasilicic acid, diatomite and aluminium oxide are a variety of, and the sodium phosphate dosage being added every time is the fused salt mixt and phosphorus
The weight ratio of sour sodium is 100:0.3~0.6, and the special adsorbent dosage being added every time is the fused salt mixt and special adsorbent
Weight ratio be 100:0.2~0.5.
In the present invention, " additive comprising sodium phosphate and special adsorbent is added ", which refers to, includes at least phosphoric acid in additive
Sodium and special adsorbent can also have in additive in other component or additive no longer comprising any other component.
In a specific embodiment, the reinforcing temperature containing lithium glass is 420~450 DEG C, and every furnace glass containing lithium
The enhanced time of glass is 3~5 hours, preferably 3.5~4.5 hours.
In a specific embodiment, for strengthening containing lithium glass and using containing in the fused salt mixt of a period of time
Have from containing the lithium ion in lithium glass, the addition is added in this fused salt mixt containing lithium using a period of time
Agent, and stand reaction 4 hours or more so that the additive 300 DEG C or more at a temperature of with the lithium ion in fused salt mixt
It reacts and takes reaction product and deposit to furnace bottom is strengthened, to purify the fused salt mixt and prolong its service life.
In a specific embodiment, after the additive being added in fused salt mixt containing lithium, it is small to stand reaction 4~20
When.
In a specific embodiment, after containing lithium glass using complete one to five furnace of fresh mix fused salt intensive treatment,
Preferably after complete three to four furnace of intensive treatment is containing lithium glass, then containing from the fused salt mixt for the lithium ion being precipitated in glass
The additive is added, allows fused salt to stand reaction at a temperature of reinforcing, so that additive brings the lithium ion in fused salt mixt into
Furnace bottom deposits to obtain regenerative mixed fused salt, is further continued for using one to five furnace of regenerative mixed fused salt intensive treatment containing lithium glass.
In a specific embodiment, the operation for additive being uniformly added into same a collection of fused salt mixt is the more of interval
Secondary, the regenerative mixed fused salt after additive is added every time and stands contains lithium glass, preferably three to four furnaces for handling one to five furnaces.
In a specific embodiment, the special adsorbent is metasilicic acid and/or aluminium oxide.
The present invention correspondingly provides a kind of fortified compositions containing lithium glass, including fused salt mixt and additive, described mixed
Fused salt is closed by KNO3And NaNO3Composition, and KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, the addition
Agent includes sodium phosphate and special adsorbent, the special adsorbent be selected from one of metasilicic acid, diatomite and aluminium oxide or
It is a variety of, and the weight ratio of fused salt mixt, sodium phosphate and special adsorbent is 100:0.3~0.6:0.2~0.5 in composition.
The present invention at least has the following beneficial effects:
1) generation lithium phosphate is reacted with the lithium ion in fused salt mixt by adding sodium phosphate in the present invention, and by special suction
The lithium phosphate of generation is wrapped up and is deposited to reinforcing furnace bottom by attached dose, so that the service life of fused salt mixt improves several times.
2) the method for the invention successfully imports volume production, and glass reinforced production efficiency has obtained great promotion, and raw
Cost is produced to be greatly reduced.
Detailed description of the invention
Every furnace fused salt mixt Fig. 1 is adds sodium phosphate and modified special adsorbent after four furnace glass of the every reinforcing of fused salt mixt when
The variation diagram of middle lithium concentration.
Every furnace enhanced products Fig. 2 is adds sodium phosphate and modified special adsorbent after four furnace glass of the every reinforcing of fused salt mixt when
Stress value (CS2 value) situation.
Specific embodiment
The present invention provides a kind of intensifying method containing lithium glass, including uses by KNO3And NaNO3At the fused salt mixt of composition
Reason is described to contain lithium glass, and wherein KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, the method also includes
The additive comprising sodium phosphate and special adsorbent is added in the fused salt mixt, the special adsorbent is selected from inclined silicon
One of acid, diatomite and aluminium oxide are a variety of, and the additive amount being added every time be the fused salt mixt, sodium phosphate and
The weight ratio of special adsorbent is 100:0.3~0.6:0.2~0.5.
In the present invention, KNO in the fused salt mixt3Content is specially 93.5wt% and the NaNO3Content is 6.5wt%.
Inventor is found through experiments that, is using KNO3Content is 90~98wt% and NaNO3Content is the fused salt mixt of 2~10wt%
Such as healthy and free from worry Gorilla 6 serial when containing lithium glass is handled, if added in the fused salt mixt according to the scheme in background technique
A certain amount of sodium phosphate clean when, or addition sodium phosphate and graphite (or active carbon) jointly clean when, react the phosphoric acid of generation
Lithium can all be strengthened in furnace at cotton-shaped swim in, and influence the stress distribution to be processed containing in lithium glass in the present invention.Because of the present invention
Middle corning glass, which needs to orient after strengthening, is supplied to display panel of the Apple Inc. as products such as mobile phone or IPAD, and Apple Inc.
Force request highest is answered to the strengthened glass panel.It is reacted by adding sodium phosphate with the lithium ion in fused salt mixt in the present invention
Lithium phosphate is generated, and the lithium phosphate of generation is wrapped up to by special adsorbent and deposited to reinforcing furnace bottom, so that fused salt mixt
Service life improves several times.Therefore, it is the reinforcing of the product containing lithium glass of adaptation high stress standard, needs in the present invention using sodium phosphate
It is cleaned in time in conjunction with lithium phosphate can be made all to deposit to furnace bottom to fused salt mixt with special adsorbent.
In addition, inventor can not use other salt such as sodium carbonate to replace the sodium phosphate through overtesting discovery, using
When sodium carbonate cooperates as the component of additive and the special adsorbent, glass product stress abnormality after reinforcing, glass
Stress value is low, each point stress data disorder observed, Stress non-homogeneity between the divided glass of same furnace, widely different.Therefore,
The sodium phosphate in the present invention cannot be replaced using sodium carbonate or other salt.
In a specific embodiment, the reinforcing temperature containing lithium glass is 420~450 DEG C, and every furnace glass containing lithium
The enhanced time of glass is 3~5 hours, preferably 3.5~4.5 hours.When reinforcing temperature is too low, the enhanced time needed is too long；By force
Change temperature it is too high when, sodium nitrate and potassium nitrate are easily decomposed to nitrite and unfavorable to strengthening.Enhanced time is too short to be easy to lead
Cause glass reinforced depth 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 slightly different, such as thicker glass uses longer enhanced time.
In a specific embodiment, for strengthening containing lithium glass and using containing in the fused salt mixt of a period of time
Have from containing the lithium ion in lithium glass, the addition is added in this fused salt mixt containing lithium using a period of time
Agent, and stand reaction 4 hours or more so that the additive 300 DEG C or more at a temperature of with the lithium ion in fused salt mixt
It reacts and takes reaction product and deposit to furnace bottom is strengthened, to purify the fused salt mixt and prolong its service life.
In a specific embodiment, after the additive being added in fused salt mixt containing lithium, it is small to stand reaction 4~20
When.
In a specific embodiment, after containing lithium glass using complete one to five furnace of fresh mix fused salt intensive treatment,
Preferably after complete three to four furnace of intensive treatment is containing lithium glass, then containing from the fused salt mixt for the lithium ion being precipitated in glass
The additive is added, allows fused salt to stand reaction at a temperature of reinforcing, so that additive brings the lithium ion in fused salt mixt into
Furnace bottom deposits to obtain regenerative mixed fused salt, is further continued for using one to five furnace of regenerative mixed fused salt intensive treatment containing lithium glass.
In the present invention, if not yet added described in addition for strengthening in any fused salt mixt containing lithium glass in fresh
Add agent, then special adsorbent can lithium ion total number in glass be discharged into fused salt mixt before just partly or entirely sink
For product to furnace bottom is strengthened, this will affect the additive that is added in the present invention to the uniform adsorption and band of the lithium ion in fused salt mixt
It falls.Therefore, the additive is uniformly added into the fused salt mixt in the present invention preferably in use for some time.
In a specific embodiment, the operation for additive being uniformly added into same a collection of fused salt mixt is the more of interval
Secondary, the regenerative mixed fused salt after additive is added every time and stands contains lithium glass, preferably three to four furnaces for handling one to five furnaces.
In a specific embodiment, the special adsorbent is metasilicic acid and/or aluminium oxide.
In the present invention, the special adsorbent plays the lithium phosphate for reacting sodium phosphate with lithium ion and generating and wraps up and drive
Its effect for depositing to furnace bottom.Graphite and active carbon drive lithium phosphate to deposit to furnace bottom because can not be successfully, thus make in the present invention
It cannot get good fused salt mixt cleaning effect when being combined as additive with graphite or active carbon and sodium phosphate.The present invention
In, especially preferred special adsorbent is metasilicic acid and/or aluminium oxide, because diatomite carries the speed that lithium phosphate deposits to furnace bottom
It is relatively slow, thus the present invention strengthens four furnaces containing after lithium glass in the fused salt mixt, uses diatomite as the component of additive
One of regenerative mixed fused salt when, needing to spend can make the lithium phosphate generated all deposit to furnace bottom for 12 hours or so；And make
When with metasilicic acid and/or aluminium oxide, probably standing 6 hours may make the lithium phosphate of generation all smoothly to deposit to furnace bottom.This
In invention, one layer of white powdery solids particle is formed in bottom of pond after lithium phosphate traction is deposited to bottom of pond by special adsorbent.
After additive is added three times into reinforcing furnace, the height probably in the bottom 1/4 for strengthening furnace can be deposited with white solid particle.
If the lower part or bottom of reinforcing furnace are provided with to be fortified containing lithium glass at this time, it is not up to standard to will lead to product reinforcing.It at this time can be with
This batch of fused salt mixt is no longer regenerated and is discarded, or is not provided with appointing by the lower part for strengthening furnace and bottom empty avoiding after regenerating again
What non-strengthened glass so may make the fused salt mixt to can continue to using a period of time.
Every furnace fused salt mixt Fig. 1 is adds sodium phosphate and modified special adsorbent after four furnace glass of the every reinforcing of fused salt mixt when
The variation diagram of middle lithium concentration.Fig. 2 is modified to add sodium phosphate and special adsorbent after four furnace glass of the every reinforcing of fused salt mixt
When every furnace enhanced products stress value (CS2 value) situation.From Fig. 1 and Fig. 2 as it can be seen that the additive is not added into reinforcing furnace
When, the lithium concentration strengthened in furnace in fused salt mixt is higher and higher, and the stress value for strengthening products obtained therefrom is lower and lower.The 4th
After furnace and the 5th furnace start before i.e. between the 4th furnace and 5 furnaces and between the 8th furnace and 9 furnaces and in the 12nd furnace and 13 furnaces
Between be separately added into the additive and stand after reaction regenerates the fused salt mixt in 6 hours, the entire life of the fused salt mixt prolongs
Long 4 times to the former service life.
TSP (the i.e. Na added in the present invention3PO4) with fused salt in Li+Reaction, by chemically reacting Li+Displacement, and
Table bottom is deposited in by substance is replaced by special adsorbent.It is solidifying to be also known as silicic acid, silica gel or silicic acid for metasilicic acid in the present invention
Glue.Additive formulations and ratio are fused salt: TSP (Na3PO4): metasilicic acid (H2SiO3)=1:0.4wt%:0.5wt%.Reaction
Principle: Li++(PO4)3-→Li3PO4.Because of Li3PO4Density ratio fused salt is low, at cotton-shaped suspended state in fused salt, adds metasilicic acid
(H2SiO3) etc. special adsorbents can play the role of adsorption and sedimentation, while in adsorbable fused salt mixt the impurity of itself and addition TSP
When the impurity brought into.From Fig. 1 and Fig. 2 as it can be seen that importing this additive (special absorption of TSP+ after four furnace glass of every reinforcing in the present invention
Agent), it adds 3 times, the furnace water service life is promoted to 16 furnaces, raising efficiency 300% by 4 original furnaces.
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 containing lithium glass, including use by KNO3And NaNO3The fused salt mixt of composition handles the glass containing lithium
Glass, and wherein KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, and the method also includes molten in the mixing
The additive comprising sodium phosphate and special adsorbent is added in salt, the special adsorbent is selected from metasilicic acid, diatomite and oxygen
Change one of aluminium or a variety of, and it is 100 that the sodium phosphate dosage being added every time, which is the weight ratio of the fused salt mixt and sodium phosphate:
0.3~0.6, the special adsorbent dosage being added every time is that the weight ratio of the fused salt mixt and special adsorbent is 100:0.2
~0.5.
2. intensifying method according to claim 1, which is characterized in that the reinforcing temperature containing lithium glass is 420~450
DEG C, and enhanced time of every furnace containing lithium glass is 3~5 hours, preferably 3.5~4.5 hours.
3. intensifying method according to claim 1, which is characterized in that when for strengthening containing lithium glass and used one section
Between fused salt mixt in containing from containing the lithium ion in lithium glass, in the fused salt mixt containing lithium that this has used a period of time
It is middle that the additive is added, and stand reaction 4 hours or more so that the additive 300 DEG C or more at a temperature of with mix
Lithium ion in fused salt, which reacts and takes reaction product, to be deposited to furnace bottom is strengthened, so that purifying the fused salt mixt and extending it makes
Use the service life.
4. intensifying method according to claim 3, which is characterized in that the additive is added in fused salt mixt containing lithium
Afterwards, reaction 4~20 hours are stood.
5. intensifying method according to claim 3, which is characterized in that arrived using fresh mix fused salt intensive treatment complete one
After five furnaces contain lithium glass, preferably after complete three to four furnace of intensive treatment is containing lithium glass, then containing the lithium being precipitated from glass
The additive is added in the fused salt mixt of ion, fused salt is allowed to stand reaction at a temperature of reinforcing, so that additive is molten by mixing
Lithium ion in salt brings furnace bottom into and deposits to obtain regenerative mixed fused salt, is further continued for arriving using the regenerative mixed fused salt intensive treatment one
Five furnaces contain lithium glass.
6. intensifying method according to claim 5, which is characterized in that be uniformly added into additive into same a collection of fused salt mixt
Operation be interval it is multiple, every time be added additive and stand after regenerative mixed fused salt for handle one to five furnace glass containing lithium
Glass, preferably three to four furnaces.
7. intensifying method according to claim 1, which is characterized in that the special adsorbent is metasilicic acid and/or oxidation
Aluminium.
8. a kind of fortified compositions containing lithium glass, including fused salt mixt and additive, the fused salt mixt is by KNO3And NaNO3
Composition, and KNO3Content is 90~98wt% and NaNO3Content is 2~10wt%, and the additive includes sodium phosphate and special suction
Attached dose, the special adsorbent be mixed selected from one of metasilicic acid, diatomite and aluminium oxide or a variety of, and in composition it is molten
The weight ratio of salt, sodium phosphate and special adsorbent is 100:0.3~0.6:0.2~0.5.
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| CN110981219A (en) * | 2019-12-11 | 2020-04-10 | 深圳市力沣实业有限公司 | Salt bath impurity ion purification method |
| 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 |
| CN112079559A (en) * | 2020-09-25 | 2020-12-15 | 光华科学技术研究院(广东)有限公司 | Method for controlling lithium ion concentration in molten salt and molten salt treating agent |
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