CN105130211B - A kind of preparation method of hydrothermal chemistry strengthened glass - Google Patents
A kind of preparation method of hydrothermal chemistry strengthened glass Download PDFInfo
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- CN105130211B CN105130211B CN201510567353.4A CN201510567353A CN105130211B CN 105130211 B CN105130211 B CN 105130211B CN 201510567353 A CN201510567353 A CN 201510567353A CN 105130211 B CN105130211 B CN 105130211B
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Abstract
The invention discloses a kind of preparation method of hydrothermal chemistry strengthened glass, this method includes：Glassware is soaked in thermal and hydric environment of the high concentration containing potassium ion solution and carries out ion-exchange treatment, and the intermittent concentration polarization for applying ultrasonic wave elimination glass surface, so that obtained chemically reinforced glass.This method is by ion exchange by the small Li of the ionic radius of glass pane surface+And Na+Alkali metal ion is exchanged for the bigger K of ionic radius+, the glass after ion exchange is after the cleaning of deionized water, as strengthened glass.The concentration polarization of glass surface can be eliminated using ultrasonication, increases the diffusion motive force of interface ion.
Description
Technical field
The present invention relates to strengthened glass preparing technical field, and in particular to a kind of preparation side of hydrothermal chemistry strengthened glass
Method.
Background technology
It is to improve glassware intensity effective ways that compressive stress layers are formed on glass surface.It is generally strong using air cooling
Change method (physics tempering method), even if being heated to the glass surface quenching close to softening point；Or less than than glass transition point
At a temperature of, (it is typically K with the alkali metal ion of larger ionic radius+) exchange having compared with small ionic radii on glass surface
Alkali metal ion (is typically Li+Or Na+).Therefore, the surface treatment process of glass can cause the intensity of glassware to increase,
So as to which the thickness of glassware is thinned, lightweight purpose is reached.Comparatively speaking, air quenched reinforcement is applied to thin body glass system
Product can not then ensure the temperature difference between glass surface and inside, be difficult to form compressive stress layers, it is impossible to obtain expected intensity.It is molten
There is the Na in fused salt in salt ion commutation rule+The fused salt that concentration accumulation is caused changes frequent, and thin body soda-lime glass is difficult system
30 microns compressive stress layers and more than 200 MPas of surface compression stress.Although fuse salt has high-temperature stability, wide scope
Low-vapor pressure, low viscosity, good electric conductivity, higher Ion transfer and diffusion velocity, high thermal capacity dissolve various differences
The advantages of ability of material.But high consumption of the melting of inorganic salts dependent on heat energy, just occurs that viscosity increases less than melting temperature
Greatly, corresponding properties are deteriorated.In addition, immersion glassware needs to consume a large amount of inorganic salts and heat, the glass after processing
Product needs to clean desalination repeatedly.
Such as the patent No.：CN201180041099.4, application publication number：CN103068759A, discloses a kind of reinforcing alkalescence
The method of aluminium borosilicate glass.Smaller metal cation present in glass is exchanged by using larger metal cation, is formed
The compression layer of layer depth is extended to from glass surface.In the second step, the metal cation in glass by larger metal sun from
Son exchanges the second depth into glass, and second depth is less than the layer depth, and enhances the compression stress of compression layer.Can
By two step ion-exchanges formation compression layer and to replace cation with compared with macrocation.Additionally provide alkaline aluminoborosilicate
Glass, it has compression layer, and at least 3000gf crack indentation threshold.This method process is complex, and cost is higher.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of hydrothermal chemistry strengthened glass, ensured
Under conditions of glassware intensity, reduction melting and cleaning cost, so as to solve problem described above.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of preparation method of hydrothermal chemistry strengthened glass, this method includes：Glassware is soaked in high concentration containing potassium
Ion-exchange treatment is carried out in the thermal and hydric environment of solion, and the intermittent concentration polarization for applying ultrasonic wave elimination glass surface
Change, so that chemically reinforced glass is made.
This method is by ion exchange by the small Li of the ionic radius of glass pane surface+And Na+Alkali metal ion be exchanged for from
The bigger K of sub- radius+, the glass after ion exchange is after the cleaning of deionized water, as strengthened glass.
Contain potassium ion solution as chemical enhanced, as long as can be by the Li of surface layer of glass2O or Na2O and K2O carries out ion
Exchange is not particularly limited, the soluble potassium salt such as potassium chloride, potassium sulfate, potassium carbonate, saleratus, potassium nitrate, such as will
Glass-impregnated is to potassium nitrate (KNO3) method in solution, it is also possible to a variety of sylvite compound uses.
In addition, in potassium salt soln, K in cation+Molar concentration is at least 34molL-1.Containing Na in potassium solution+Mole
Percentage is 4~6%, and rich natrium potassium salt solution is carried out into sodium potassium separation with 732 type strong acidic ion resins, potassium salt soln is realized
Low sodium processing.
Condition for forming the chemical enhanced layer with desired bearing stress on glass：According to the surface of glass
The difference of compression thickness, hydrothermal temperature conditions are preferably 200~240 DEG C, water heating kettle compactedness 60~80%, and solvent is pure
Water, the time of hydro-thermal reinforcing is preferably 6~18h, ultrasonic time 10~20min, ultrasonic 1~2h of interval time.
The applicable glass basis of this method is the soda-lime glass product of all kinds of types, the table of the glass after hydrothermal chemistry reinforcing
The depth of face pressure stressor layers is preferably 24 μm~50 μm, and surface compression stress is preferably 250~500MPa.
The beneficial effects of the invention are as follows：
1st, ultrasonication can eliminate the concentration polarization of glass surface, the diffusion of increase interface sodium ion and potassium ion
Motive force；
2nd, in the thermal and hydric environment of HTHP, the solubility of sylvite is greatly improved, and ionic activity is high, and heat diffusivity can be good,
Be conducive to glass to carry out ion exchange with solution, realize that surface chemistry is strengthened；
3rd, sylvite consumption is small, and solution viscosity is small, it is easy to separated with glass, glass surface sylvite less residue, is easy to follow-up
Cleaning；
4th, low-temperature operation, can select labile sylvite, add the washability of sylvite species, and thermal energy consumption is big
Big reduction, it also avoid corrosion of the high-temperature molten salt to wall；
5th, the thermal and hydric environment of closing can provide safe operating environment, it is to avoid fused salt decomposes produce poisonous under high temperature
Injury of the gas to operator；
6th, potassium salt soln can be realized by ion exchange and regenerated, and realize that sylvite is purified, it is not necessary to which the sylvite more renewed is molten
Liquid, substantially increases the utilization rate of sylvite, falls below sylvite consumption cost.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1
Glass basis selects soda-lime glass Bottle ＆ Can, and sylvite selects K in potassium nitrate and potassium chloride, solution+Molar concentration is
35mol·L-1；Hydrothermal temperature conditions are 210 DEG C, compactedness 80%, and solvent is pure water, and the time of hydro-thermal reinforcing is preferably 18h,
Ultrasonic time 12min, ultrasonic interval time 2h.Na in solution+Molar percentage is 4%, by Klorvess Liquid with 732 type strong acid
Property resin cation carry out sodium potassium separation, realize the processing of Klorvess Liquid low sodium.The surface of glass after hydrothermal chemistry reinforcing
The depth of compressive stress layer is 27 μm, and surface compression stress is 258MPa.
Embodiment 2
Glass basis selects soda-lime glass Bottle ＆ Can, and sylvite selects K in potassium nitrate and potassium sulfate, solution+Molar concentration is
52mol·L-1；Hydrothermal temperature conditions are 220 DEG C, compactedness 70%, and solvent is pure water, and the time of hydro-thermal reinforcing is preferably 14h,
Ultrasonic time 16min, ultrasonic interval time 1.5h.Na in solution+Molar percentage is 5%, and Klorvess Liquid is strong with 732 types
Acidic cationic resin carries out sodium potassium separation, realizes the low sodium processing of Klorvess Liquid.The table of glass after hydrothermal chemistry reinforcing
The depth of face pressure stressor layers is 34 μm, and surface compression stress is 387MPa.
Embodiment 3
Glass basis selects soda-lime glass Bottle ＆ Can, and sylvite selects K in potassium carbonate, potassium nitrate and potassium sulfate, solution+It is mole dense
Spend for 74molL-1；Hydrothermal temperature conditions are 240 DEG C, compactedness 65%, and solvent is pure water, and the time of hydro-thermal reinforcing is preferably
12h, ultrasonic time 20min, ultrasonic interval time 1h.Na in solution+Molar percentage is 5%, by 732 types of Klorvess Liquid
Strong acidic ion resin carries out sodium potassium separation, realizes the low sodium processing of Klorvess Liquid.Glass after hydrothermal chemistry reinforcing
The depth of bearing stress layer is 46 μm, and surface compression stress is 492MPa.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (2)
1. a kind of preparation method of hydrothermal chemistry strengthened glass, it is characterized in that this method includes：Glassware is soaked in highly concentrated
Degree carries out ion-exchange treatment in the thermal and hydric environment containing potassium ion solution, and the intermittent ultrasonic wave that applies eliminates the dense of glass surface
Difference polarization, so that chemically reinforced glass is made；
The high concentration selects a kind of or several in potassium chloride, potassium sulfate, potassium carbonate, saleratus, nitrate containing potassium ion solution
Plant the solution being made；
The high concentration contains in potassium ion solution, K in cation+Molar concentration is at least 34molL-1；
The high concentration contains Na in potassium ion solution+Molar percentage is 4~6%；
Above-mentioned hydrothermal temperature conditions are 200~240 DEG C, the compactedness 60~80% of glass, and solvent is pure water, hydrothermal exchange processing
Time be 6~18h, ultrasonic time 10~20min, ultrasonic 1~2h of interval time.
2. a kind of preparation method of hydrothermal chemistry strengthened glass according to claim 1, it is characterized in that, by above-mentioned high concentration
Sodium potassium separation is carried out with strong acidic ion resin containing potassium ion solution, the low sodium processing of potassium salt soln is realized.
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| CN105130211B true CN105130211B (en) | 2017-09-22 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108101361B (en) | 2016-12-30 | 2021-07-06 | 东旭光电科技股份有限公司 | Silicate product and reinforcing method thereof |
| JP2019006615A (en) * | 2017-06-21 | 2019-01-17 | Ａｇｃ株式会社 | Manufacturing method of chemically strengthened glass |
| CN108675652B (en) * | 2018-06-05 | 2021-07-16 | 吴江金刚玻璃科技有限公司 | Ultrathin chemically strengthened glass and preparation method thereof |
| CN112919827B (en) * | 2021-02-06 | 2021-11-19 | 安徽科技学院 | Tempering process for reducing glass self-explosion rate |
| CN114477791B (en) * | 2022-02-21 | 2024-07-05 | 湖南工学院 | Method for improving light transmittance by embedding alkali metal ions into surface of reconstructed photovoltaic glass |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815860A (en) * | 2011-06-10 | 2012-12-12 | 肖特玻璃科技(苏州)有限公司 | Method for producing tempered glass with plurality of surface stress layers and tempered glass product |
| CN103332869A (en) * | 2013-06-04 | 2013-10-02 | 中南大学 | Method for preparing multifunctional composite ZnO/In coating glass |
| CN104129906A (en) * | 2014-07-31 | 2014-11-05 | 湖南丹化农资有限公司 | Additive-containing single-crystal-state potassium nitrate glass-reinforcing molten salt and glass reinforcing technology |
| CN104736495A (en) * | 2013-07-19 | 2015-06-24 | 旭硝子株式会社 | Method for manufacturing chemically reinforced glass |
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- 2015-09-08 CN CN201510567353.4A patent/CN105130211B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815860A (en) * | 2011-06-10 | 2012-12-12 | 肖特玻璃科技(苏州)有限公司 | Method for producing tempered glass with plurality of surface stress layers and tempered glass product |
| CN103332869A (en) * | 2013-06-04 | 2013-10-02 | 中南大学 | Method for preparing multifunctional composite ZnO/In coating glass |
| CN104736495A (en) * | 2013-07-19 | 2015-06-24 | 旭硝子株式会社 | Method for manufacturing chemically reinforced glass |
| CN104129906A (en) * | 2014-07-31 | 2014-11-05 | 湖南丹化农资有限公司 | Additive-containing single-crystal-state potassium nitrate glass-reinforcing molten salt and glass reinforcing technology |
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Denomination of invention: A preparation method of hydrothermal chemically strengthened glass Effective date of registration: 20211213 Granted publication date: 20170922 Pledgee: Anhui Fengyang Rural Commercial Bank Co.,Ltd. Pledgor: ANHUI FENGYANG HUAIHE GLASS Co.,Ltd. Registration number: Y2021980014800 |
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