CN107311438A - A kind of preparation technology of high-strength refractory Cs-K glass - Google Patents

A kind of preparation technology of high-strength refractory Cs-K glass Download PDF

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Publication number
CN107311438A
CN107311438A CN201710521873.0A CN201710521873A CN107311438A CN 107311438 A CN107311438 A CN 107311438A CN 201710521873 A CN201710521873 A CN 201710521873A CN 107311438 A CN107311438 A CN 107311438A
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glass
fused salt
cesium
potassium
preparation technology
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武娟
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Hefei Yutai Glass Products Co Ltd
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Hefei Yutai Glass Products Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B27/00Tempering or quenching glass products
    • C03B27/02Tempering or quenching glass products using liquid
    • C03B27/03Tempering or quenching glass products using liquid the liquid being a molten metal or a molten salt
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B27/00Tempering or quenching glass products
    • C03B27/012Tempering or quenching glass products by heat treatment, e.g. for crystallisation; Heat treatment of glass products before tempering by cooling
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B27/00Tempering or quenching glass products
    • C03B27/04Tempering or quenching glass products using gas
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C21/00Treatment of glass, not in the form of fibres or filaments, by diffusing ions or metals in the surface
    • C03C21/001Treatment 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
    • C03C21/002Treatment 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a kind of preparation technology of high-strength refractory Cs-K glass, it is characterised in that comprises the following steps:It is prepared by fused salt:Sylvite and cesium salt are mixed, is put into fused salt groove, adds additive, required fused salt is made;Chemical tempering:Monolithic glass is put into fused salt groove, ion exchange is carried out, realizes chemical tempering;It is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, after the completion of heating, glass enters the quick chilling of cooling section;Air-cooled shaping:Glass after will be physical toughened, which takes out and sends into air grid, carries out air-cooled shaping, and finally cooling obtains high-strength refractory Cs-K glass.Flame resistant glass produced by the present invention not only has preferable fire protecting performance, while having higher intensity and shock resistance.

Description

A kind of preparation technology of high-strength refractory Cs-K glass
Technical field
The present invention relates to a kind of processing technology of glass, more particularly, to a kind of system of high-strength refractory Cs-K glass Standby technique.
Background technology
At present, flame resistant glass common on domestic and international market is mostly interlayer composite fireproof glass and wired flame resistant glass, The refractory adhesive added in the former reforms into milky under ultraviolet irradiation and produces bubble quickly, has a strong impact on glass Translucency, service life is shorter, and using manual operations and control, production efficiency underground, product quality is difficult to ensure that, it is impossible to entered Row large-scale industrial production, and not only light transmittance is not good enough and heat can not be prevented to radiate for wired flame resistant glass, also there is peace The problems such as pretending to be stupid heavy, limits the use as building exterior wall glass.In addition, also a kind of single-sheet fire-resistant glass, using spray Coating carries out tempering to common float glass.
And the making of existing single-sheet fire-resistant glass, original is typically just used as using the material such as ordinary plate glass or safety glass Piece, on the basis of these semifinished sheets, is polished, cleans and technological process and the method processing such as fire prevention processing, full The performance requirement of sufficient flame resistant glass.The performance indications that the quality of its flame resistant glass is up to state standards, are mainly manifested in size inclined In terms of difference, presentation quality, fire resistance, flexibility, light transmittance.The preparation method of existing flame resistant glass mainly exists glass Heat, then cooled down in the presence of high-pressure blast air-flow, the preparation method has many drawbacks under hot environment, mainly Intensity is not high, shock resistance and heat resistant fire-proof poor performance, significantly limit it and uses scope, therefore is badly in need of a kind of the anti-of high intensity Flint glass.
The content of the invention
The purpose of the present invention is that there is provided a kind of preparation of high-strength refractory Cs-K glass for problem of the prior art Technique, equipment goes out high intensity, shock resistance and the good flame resistant glass of heat resistant fire-proof performance.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of preparation technology of high-strength refractory Cs-K glass, it is characterised in that comprise the following steps:
(1)It is prepared by fused salt:Sylvite and cesium salt are mixed, are put into fused salt groove, fused salt groove is heated to 400-500 DEG C, 6- is incubated 8h, is then reduced to 300-350 DEG C by fused salt groove again, adds additive, and stirring makes additive be sufficiently mixed with sylvite, cesium salt, Then 400-500 DEG C is increased the temperature to, continues to stir, required fused salt is made;
(2)Chemical tempering:Monolithic glass is put into fused salt groove, ion exchange, glass are carried out under 400-500 DEG C of temperature conditionss Sodium ion in glass causes vibration due to heating, thus complete in the less sodium ion of radius in surface layer of glass and fused salt radius compared with The exchange of big potassium ion or cesium ion, realizes chemical tempering, is exchanged by sodium ion with the potassium ion or cesium ion in fused salt Quantity increase, the compression of surface layer of glass is with enhancing;
(3)It is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, heating room temperature is set It is scheduled between 580-630 DEG C, the heat time, after the completion of heating, it is fast that glass enters cooling section by every millimeter of heating 35-45s of glass Fast chilling;
(4)Air-cooled shaping:Glass after will be physical toughened take out and with 350-450mm/s speed feeding air grid carry out it is air-cooled into Type, finally cooling obtains high-strength refractory Cs-K glass.
It is preferred that, the sylvite is more than one or both of potassium chloride, potassium nitrate, potassium sulfate and potassium phosphate.
It is preferred that, the cesium salt is cesium nitrate or cesium carbonate.
It is preferred that, the sylvite percentage by weight is the 48% of fused salt.
It is preferred that, the cesium salt percentage by weight is the 47% of fused salt.
It is preferred that, the additive includes the first additive and Second addition, wherein the first additive is aluminum oxide, oxygen Change more than one or both of magnesium, zinc oxide, boron oxide and zirconium dioxide, Second addition be potassium phosphate, potassium metapbosphate, It is more than one or both of potassium pyrophosphate and aluminum sodium phosphate.
It is preferred that, the first additive addition is the 2-4% of fused salt weight, and the Second addition addition is molten The 1-3% of salt weight.
It is preferred that, the blast of glass edge is 650-670KPa in the air-cooled shaping, and the blast in centre is 610- 630KPa。
It is preferred that, the adjustment height of the air grid is between 30-80mm.
The present invention compared with prior art, with following beneficial effect:
(1)The flame resistant glasses made from step such as the present invention is prepared by fused salt, chemical tempering, physical toughened and air-cooled shaping are not only With preferable fire protecting performance, while there is higher intensity and shock resistance, it is of the invention in the case of same thickness Obtained strength of glass is 8-14 times of float glass, is 4-6 times of safety glass;
(2)Ion-exchange treatment, the sodium ion of glass surface are carried out in fused salt of the invention by the way that glass to be immersed to 400-500 DEG C With the potassium ion in fused salt, cesium ion fast exchange, and by adding the first additive and Second addition in fused salt, enter one Step accelerate ion-exchange speed, because potassium ion and cesium ion radius ratio sodium ion radius are much larger, the extruding of big ion and Glass surface produces compression, makes glass-faced construction finer and close, due to caesium, the melange effect of potassium ion, glass surface shape Into big many of the compression that exchanges than single ionic of compression, question response reaches again to enter glass after predetermined balanced degree The physical toughened processing of row, is first heated at 580-630 DEG C, most glass surface is produced powerful compression through air-cooled shaping afterwards, So as to greatly improve the intensity of glass;
(3)Glass machinability is good made from preparation technology of the present invention, can be processed into fireproof hollow glass, interlayer fire prevention glass Glass, plated film flame resistant glass, arc flame resistant glass etc., application field are wide, can be used as indoor fire safety cut-off and passageway for fire apparatus etc..
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in the embodiment of the present invention Technical scheme is clearly and completely described, it is clear that described embodiment is a part of embodiment of the invention, rather than entirely The embodiment in portion.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made The every other embodiment obtained, belongs to the scope of protection of the invention.
Embodiment 1
A kind of preparation technology of high-strength refractory Cs-K glass, comprises the following steps:
(1)It is prepared by fused salt:Sylvite and cesium salt are mixed, are put into fused salt groove, fused salt groove is heated to 450 DEG C, 7h is incubated, then Fused salt groove is reduced to 320 DEG C again, additive is added, stirring makes additive be sufficiently mixed with sylvite, cesium salt, then raises temperature To 450 DEG C, continue to stir, required fused salt is made;
(2)Chemical tempering:Monolithic glass is put into fused salt groove, carried out under 450 DEG C of temperature conditionss in ion exchange, glass Sodium ion vibration is caused due to heating so that it is larger to complete radius in the less sodium ion of radius in surface layer of glass and fused salt The exchange of potassium ion or cesium ion, realizes chemical tempering, and quantity is exchanged with the potassium ion or cesium ion in fused salt by sodium ion Increase, the compression of surface layer of glass is with enhancing;
(3)It is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, heating room temperature is set It is scheduled between 600 DEG C, the heat time, after the completion of heating, glass entered the quick chilling of cooling section by every millimeter of heating 40s of glass;
(4)Air-cooled shaping:Glass after will be physical toughened takes out and carries out air-cooled shaping with 400mm/s speed feeding air grid, Finally cooling obtains high-strength refractory Cs-K glass.
Wherein, the sylvite is more than one or both of potassium chloride, potassium nitrate, potassium sulfate and potassium phosphate.
Wherein, the cesium salt is cesium nitrate or cesium carbonate.
Wherein, the sylvite percentage by weight is the 48% of fused salt.
Wherein, the cesium salt percentage by weight is the 47% of fused salt.
Wherein, the additive includes the first additive and Second addition, wherein the first additive is aluminum oxide, oxidation More than one or both of magnesium, zinc oxide, boron oxide and zirconium dioxide, Second addition is potassium phosphate, potassium metapbosphate, Jiao It is more than one or both of potassium phosphate and aluminum sodium phosphate.
Wherein, the first additive addition is the 3% of fused salt weight, and the Second addition addition is fused salt weight The 2% of amount.
Wherein, the blast of glass edge is 660KPa in the air-cooled shaping, and the blast in centre is 620KPa.
Wherein, the adjustment height of the air grid is between 50mm.
Embodiment 2
A kind of preparation technology of high-strength refractory Cs-K glass, comprises the following steps:
(1)It is prepared by fused salt:Sylvite and cesium salt are mixed, are put into fused salt groove, fused salt groove is heated to 400 DEG C, 6h is incubated, then Fused salt groove is reduced to 300 DEG C again, additive is added, stirring makes additive be sufficiently mixed with sylvite, cesium salt, then raises temperature To 400 DEG C, continue to stir, required fused salt is made;
(2)Chemical tempering:Monolithic glass is put into fused salt groove, carried out under 400 DEG C of temperature conditionss in ion exchange, glass Sodium ion vibration is caused due to heating so that it is larger to complete radius in the less sodium ion of radius in surface layer of glass and fused salt The exchange of potassium ion or cesium ion, realizes chemical tempering, and quantity is exchanged with the potassium ion or cesium ion in fused salt by sodium ion Increase, the compression of surface layer of glass is with enhancing;
(3)It is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, heating room temperature is set It is scheduled between 580 DEG C, the heat time, after the completion of heating, glass entered the quick chilling of cooling section by every millimeter of heating 35s of glass;
(4)Air-cooled shaping:Glass after will be physical toughened takes out and carries out air-cooled shaping with 350mm/s speed feeding air grid, Finally cooling obtains high-strength refractory Cs-K glass.
Wherein, the sylvite is more than one or both of potassium chloride, potassium nitrate, potassium sulfate and potassium phosphate.
Wherein, the cesium salt is cesium nitrate or cesium carbonate.
Wherein, the sylvite percentage by weight is the 48% of fused salt.
Wherein, the cesium salt percentage by weight is the 47% of fused salt.
Wherein, the additive includes the first additive and Second addition, wherein the first additive is aluminum oxide, oxidation More than one or both of magnesium, zinc oxide, boron oxide and zirconium dioxide, Second addition is potassium phosphate, potassium metapbosphate, Jiao It is more than one or both of potassium phosphate and aluminum sodium phosphate.
Wherein, the first additive addition is the 2% of fused salt weight, and the Second addition addition is fused salt weight The 1% of amount.
Wherein, the blast of glass edge is 650KPa in the air-cooled shaping, and the blast in centre is 610KPa.
Wherein, the adjustment height of the air grid is between 30mm.
Embodiment 3
A kind of preparation technology of high-strength refractory Cs-K glass, comprises the following steps:
(1)It is prepared by fused salt:Sylvite and cesium salt are mixed, are put into fused salt groove, fused salt groove is heated to 500 DEG C, 8h is incubated, then Fused salt groove is reduced to 350 DEG C again, additive is added, stirring makes additive be sufficiently mixed with sylvite, cesium salt, then raises temperature To 500 DEG C, continue to stir, required fused salt is made;
(2)Chemical tempering:Monolithic glass is put into fused salt groove, carried out under 500 DEG C of temperature conditionss in ion exchange, glass Sodium ion vibration is caused due to heating so that it is larger to complete radius in the less sodium ion of radius in surface layer of glass and fused salt The exchange of potassium ion or cesium ion, realizes chemical tempering, and quantity is exchanged with the potassium ion or cesium ion in fused salt by sodium ion Increase, the compression of surface layer of glass is with enhancing;
(3)It is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, heating room temperature is set It is scheduled between 630 DEG C, the heat time, after the completion of heating, glass entered the quick chilling of cooling section by every millimeter of heating 45s of glass;
(4)Air-cooled shaping:Glass after will be physical toughened takes out and carries out air-cooled shaping with 450mm/s speed feeding air grid, Finally cooling obtains high-strength refractory Cs-K glass.
Wherein, the sylvite is more than one or both of potassium chloride, potassium nitrate, potassium sulfate and potassium phosphate.
Wherein, the cesium salt is cesium nitrate or cesium carbonate.
Wherein, the sylvite percentage by weight is the 48% of fused salt.
Wherein, the cesium salt percentage by weight is the 47% of fused salt.
Wherein, the additive includes the first additive and Second addition, wherein the first additive is aluminum oxide, oxidation More than one or both of magnesium, zinc oxide, boron oxide and zirconium dioxide, Second addition is potassium phosphate, potassium metapbosphate, Jiao It is more than one or both of potassium phosphate and aluminum sodium phosphate.
Wherein, the first additive addition is the 3% of fused salt weight, and the Second addition addition is fused salt weight The 2% of amount.
Wherein, the blast of glass edge is 670KPa in the air-cooled shaping, and the blast in centre is 630KPa.
Wherein, the adjustment height of the air grid is between 80mm.
Service check is carried out to flame resistant glass prepared by above-mentioned 3 embodiments, wherein reference examples 1 are to use Authorization Notice No. The flame resistant glass made from the preparation method described in CN104291688B;Reference examples 2 be use Authorization Notice No. for Flame resistant glass made from preparation method described in CN102503178B;And according to《GB15763.1 safety glasses for building》Regulation Testing standard carry out performance test, test result is as shown in table 1:
Table 1
From table 1 it follows that flame resistant glass prepared by the present invention is compared with reference examples, its rupture strength, compression strength, anti-impact Hit intensity, stress value and fire integrity time are better than existing flame resistant glass, illustrate the high intensity list prepared by the present invention The features such as piece caesium potassium flame resistant glass has high intensity, shock resistance and good heat resistant fire-proof performance, and technique is simple, is adapted to big rule Mould is produced.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.

Claims (8)

1. a kind of preparation technology of high-strength refractory Cs-K glass, it is characterised in that comprise the following steps:
(1) prepared by fused salt:Sylvite and cesium salt are mixed, are put into fused salt groove, fused salt groove is heated to 400-500 DEG C, 6- is incubated 8h, is then reduced to 300-350 DEG C by fused salt groove again, adds additive, and stirring makes additive be sufficiently mixed with sylvite, cesium salt, Then 400-500 DEG C is increased the temperature to, continues to stir, required fused salt is made;
(2) chemical tempering:Monolithic glass is put into fused salt groove, ion exchange, glass are carried out under 400-500 DEG C of temperature conditionss Sodium ion in glass causes vibration due to heating, thus complete in the less sodium ion of radius in surface layer of glass and fused salt radius compared with The exchange of big potassium ion or cesium ion, realizes chemical tempering, is exchanged by sodium ion with the potassium ion or cesium ion in fused salt Quantity increase, the compression of surface layer of glass is with enhancing;
(3) it is physical toughened:Glass after fused salt soaks is sent into special annealing furnace to be heated, heating room temperature is set It is scheduled between 580-630 DEG C, the heat time, after the completion of heating, it is fast that glass enters cooling section by every millimeter of heating 35-45s of glass Fast chilling;
(4) air-cooled shaping:Glass after will be physical toughened take out and with 350-450mm/s speed feeding air grid carry out it is air-cooled into Type, finally cooling obtains high-strength refractory Cs-K glass.
2. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the sylvite More than one or both of potassium chloride, potassium nitrate, potassium sulfate and potassium phosphate.
3. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the cesium salt For cesium nitrate or cesium carbonate.
4. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the sylvite Percentage by weight is the 48% of fused salt.
5. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the cesium salt Percentage by weight is the 47% of fused salt.
6. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the addition Agent includes the first additive and Second addition, wherein the first additive is aluminum oxide, magnesia, zinc oxide, boron oxide and two More than one or both of zirconium oxide, Second addition is in potassium phosphate, potassium metapbosphate, potassium pyrophosphate and aluminum sodium phosphate It is one or more kinds of.
7. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that described first Additive addition is the 2-4% of fused salt weight, and the Second addition addition is the 1-3% of fused salt weight.
8. the preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that described air-cooled The blast of glass edge is 650-670KPa in shaping, and the blast in centre is 610-630KPa.
The preparation technology of high-strength refractory Cs-K glass according to claim 1, it is characterised in that the air grid Adjustment height is between 30-80mm.
CN201710521873.0A 2017-06-30 2017-06-30 A kind of preparation technology of high-strength refractory Cs-K glass Withdrawn CN107311438A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108002713A (en) * 2017-12-19 2018-05-08 常熟市沪联印染有限公司 The preparation method of chemically toughened glass fabric lining
CN108439775A (en) * 2018-04-04 2018-08-24 合肥钢骨玻璃制品有限公司 A kind of preparation process of composite fireproof glass
CN109052992A (en) * 2018-09-25 2018-12-21 北京京北华燕玻璃有限公司 A kind of single-sheet fire-resistant glass and preparation method thereof
CN111499192A (en) * 2020-04-24 2020-08-07 中国建筑材料科学研究总院有限公司 Aluminosilicate glass and preparation method and application thereof
CN112374768A (en) * 2020-11-12 2021-02-19 江苏长欣车辆装备有限公司 Toughened glass with excellent crushing state
CN114315170A (en) * 2020-10-10 2022-04-12 科立视材料科技有限公司 Antibacterial impact-resistant safety glass and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101219854A (en) * 2007-01-08 2008-07-16 宋丽 Process for manufacturing single-slice fireproof glass and the single-slice fireproof glass
CN101805117A (en) * 2010-03-19 2010-08-18 司志伟 Preparation method of novel ultra-high strength single-sheet fire-resistant glass

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101219854A (en) * 2007-01-08 2008-07-16 宋丽 Process for manufacturing single-slice fireproof glass and the single-slice fireproof glass
CN101805117A (en) * 2010-03-19 2010-08-18 司志伟 Preparation method of novel ultra-high strength single-sheet fire-resistant glass

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108002713A (en) * 2017-12-19 2018-05-08 常熟市沪联印染有限公司 The preparation method of chemically toughened glass fabric lining
CN108439775A (en) * 2018-04-04 2018-08-24 合肥钢骨玻璃制品有限公司 A kind of preparation process of composite fireproof glass
CN109052992A (en) * 2018-09-25 2018-12-21 北京京北华燕玻璃有限公司 A kind of single-sheet fire-resistant glass and preparation method thereof
CN109052992B (en) * 2018-09-25 2021-03-16 北京京北华燕玻璃有限公司 Single-piece fireproof glass and preparation method thereof
CN111499192A (en) * 2020-04-24 2020-08-07 中国建筑材料科学研究总院有限公司 Aluminosilicate glass and preparation method and application thereof
CN111499192B (en) * 2020-04-24 2022-07-12 中国建筑材料科学研究总院有限公司 Aluminosilicate glass and preparation method and application thereof
CN114315170A (en) * 2020-10-10 2022-04-12 科立视材料科技有限公司 Antibacterial impact-resistant safety glass and preparation method thereof
CN112374768A (en) * 2020-11-12 2021-02-19 江苏长欣车辆装备有限公司 Toughened glass with excellent crushing state

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