CN117023979A - Alkaline aluminosilicate glass and preparation process and application thereof - Google Patents
Alkaline aluminosilicate glass and preparation process and application thereof Download PDFInfo
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- CN117023979A CN117023979A CN202310834448.2A CN202310834448A CN117023979A CN 117023979 A CN117023979 A CN 117023979A CN 202310834448 A CN202310834448 A CN 202310834448A CN 117023979 A CN117023979 A CN 117023979A
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- 239000005354 aluminosilicate glass Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 92
- 238000000034 method Methods 0.000 claims abstract description 23
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 12
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 6
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 6
- 238000005496 tempering Methods 0.000 claims description 112
- 239000005358 alkali aluminosilicate glass Substances 0.000 claims description 42
- 239000000126 substance Substances 0.000 claims description 38
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 22
- 239000005368 silicate glass Substances 0.000 claims description 16
- 239000000395 magnesium oxide Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical group [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 230000035939 shock Effects 0.000 abstract description 4
- 239000005357 flat glass Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 18
- 239000002994 raw material Substances 0.000 description 10
- 239000012634 fragment Substances 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000005341 toughened glass Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000003426 chemical strengthening reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006060 molten glass Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000005336 safety glass Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
- C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
- B60J1/00—Windows; Windscreens; Accessories therefor
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/012—Tempering or quenching glass products by heat treatment, e.g. for crystallisation; Heat treatment of glass products before tempering by cooling
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B27/00—Tempering or quenching glass products
- C03B27/04—Tempering or quenching glass products using gas
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses an alkaline aluminosilicate glass and a preparation process and application thereof, wherein the alkaline aluminosilicate glass comprises 58-65% by mass of SiO 2 13 to 15 percent of Al 2 O 3 12-15% of Na 2 O,0 to 6 percent of K 2 O,3 to 5 percent of alkaline earth metal and 0 to 1 percent of ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein the CS satisfies: CS is more than or equal to 700Mpa and less than or equal to 800Mpa; the depth of the compressive stress layer of the glass is DOL, wherein the DOL meets the following conditions: DOL is more than or equal to 30 mu m and less than or equal to 40 mu m; the glass has impact energy CT, whereinCT satisfies: CT is more than or equal to 0.8J. Has high depth of the compressive stress layer of the glass stress glass and excellent shock resistance. And when the car window made of the alkaline aluminosilicate glass is broken, the state meets the national safety requirements on car window glass.
Description
Technical Field
The invention relates to the field of glass products, in particular to alkaline aluminosilicate glass and a preparation process and application thereof.
Background
Alkali aluminosilicate glasses are particularly well suited for use in the prior art for making thinner glass articles. For example, treatment of alkali aluminosilicate glass with ion exchange (IX) technology can impart high levels of compressive stress to the glass, which is suitable for use in the manufacture of strong, lightweight automotive glazings. However, when the glass is broken, a large amount of long fragments appear, and the end part is in a blade shape, which cannot meet the requirements of national standards on the safety glass of automobiles.
This is because it is difficult to avoid the impact of the window against gravel, crushed stone and other various particulate objects during the running of the automobile. The microcracks generated on the surface of the glass by the impact of broken stone or fragments are about tens of micrometers, so that the scratch resistance of the window glass is weak, and the appearance and the service life of the window are directly influenced.
Thus, there is a need to enhance the scratch resistance and safety of alkali aluminosilicate glasses after breakage.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, an object of the present invention is to provide an alkali aluminosilicate glass which is high in scratch resistance and safety after breakage.
Another object of the present invention is to provide a method for preparing alkali aluminosilicate glass.
It is another object of the present invention to provide the use of an alkali aluminosilicate glass in automotive windows.
The alkaline aluminosilicate glass of the embodiment of the invention comprises 58-65% of SiO by mass 2 13 to 15 percent of Al 2 O 3 12-15% of Na 2 O,0 to 6 percent of K 2 O,3 to 5 percent of alkaline earth metal and 0 to 1 percent of ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein the CS satisfies: CS is more than or equal to 700Mpa and less than or equal to 800Mpa; the depth of the compressive stress layer of the glass is DOL, wherein the DOL meets the following conditions: DOL is more than or equal to 30 mu m and less than or equal to 40 mu m; the impact energy of the glass is CT, wherein the CT satisfies the following conditions: CT is more than or equal to 0.8J.
According to some embodiments of the invention, the alkaline earth metal oxide is magnesium oxide.
According to a second aspect of the present invention, there is provided a process for preparing an alkali aluminosilicate glass according to the above-mentioned first aspect of the present invention, comprising subjecting an alkali aluminosilicate glass sample to a physical tempering treatment at a temperature of 620 to 780 ℃ for 180 to 300s and a chemical tempering treatment; and/or the temperature of the chemical tempering treatment is 400-450 ℃ and the time is 120-300 min.
According to some embodiments of the invention, the silicate glass sample piece has a thickness of 1.1mm or more.
According to some embodiments of the invention, a tempering salt is added in the step of chemically tempering, preferably potassium nitrate.
According to some embodiments of the invention, the method comprises the steps of: step one, cleaning and preheating an alkaline aluminosilicate glass sample; step two, carrying out physical tempering treatment on the silicate glass sample piece treated in the step one, and then cooling the silicate glass sample piece treated in the step three, and carrying out secondary cleaning and preheating on the silicate glass sample piece treated in the step two; and fourthly, performing chemical tempering treatment on the silicate glass sample piece obtained in the third step to form a silicate glass product.
According to some embodiments of the invention, in the first step, the preheating is performed at 600-720 ℃ for 120-180 s.
According to some embodiments of the invention, the cooling pressure is 8000-12000 Pa, and the cooling time is 30-60 s; and/or the preheating temperature is 350-380 ℃, and the preheating time is 30-60 min.
According to an embodiment of a third aspect of the present invention, the present invention provides an application of the alkali aluminosilicate glass according to the embodiment of the first aspect or the glass prepared by the preparation process according to the embodiment of the second aspect, and the glass is applied to an automobile window.
Advantageous effects
The alkali aluminosilicate glass according to the embodiment of the invention has higher depth of the compressive stress layer of the glass stress glass and excellent shock resistance. Specifically, the CS satisfies: CS is more than or equal to 700Mpa and less than or equal to 800Mpa; the DOL satisfies: DOL is more than or equal to 30 mu m and less than or equal to 40 mu m; the CT satisfies the following conditions: CT > 0.8J. And when the car window made of the alkaline aluminosilicate glass is broken, the state meets the national safety requirements on car window glass.
In addition, the alkaline earth metal content in the glass of the specific embodiment of the invention is w in terms of mass percent of alkaline earth metal oxide, wherein w satisfies the following conditions: w is less than or equal to 5 percent. Alkali aluminosilicate glass has high stress because alkali aluminosilicate glass can be treated with ion exchange (IX) technology to produce high levels of compressive stress in the treated glass, up to about 1000Mpa at the surface, and has high strength, and is very suitable for use in the manufacture of strong, lightweight automotive glazings. The strength of the glass treated by the method generally depends on CS, DOL, CT values, the larger the CS, the deeper the DOL, the smaller the CT and the higher the theoretical strength value of the glass, but with the increase of the CS value of the glass, the reinforced glass shows a strip shape and an acute angle shape after receiving ball impact, so that the glass does not meet the national standard for automobile glass. Therefore, it is necessary to control the alkaline earth metal content of the alkali aluminosilicate glass of the present invention. When the content of alkaline earth metal in the glass is reduced, the ion exchange rate is reduced, CS or DOL is reduced, and when the MgO content is between 3 and 5 percent, the alkaline aluminosilicate glass has higher shock resistance and can improve the state of fragments of the glass after strengthening. The alkali aluminosilicate glass is subjected to a reduction treatment of CS and DOL after chemical strengthening, but the extent of the reduction must not be too great, otherwise the ball drop impact strength of the final glass will be affected.
The preparation process of the alkaline aluminosilicate glass comprises the steps of carrying out physical tempering treatment and chemical tempering treatment on the alkaline aluminosilicate glass sample piece, and realizing the reinforced preparation of silicate glass by the synergistic effect of the physical tempering treatment and the chemical tempering treatment. Specifically, the thickness of the alkali aluminosilicate glass sample used in the present invention is 1.1mm or more. In combination with specific experiments, it was found that when the thickness of the alkali aluminosilicate glass sample is less than 1.1mm, the strengthening efficiency is very low, the breaking rate is as high as more than 50%, and the deformation of the glass is serious, which is not suitable for physical strengthening. In the case of glass with a thickness of more than 1.1mm, the glass sample of the alkali aluminosilicate glass sample has a small breaking rate and is deformed within a proper range. Further, the alkaline aluminosilicate glass sample piece treatment of the invention comprises the steps of preheating the alkaline aluminosilicate glass sample piece, physical tempering treatment and chemical tempering treatment, and specifically comprises the following steps: the step of preheating the alkali aluminosilicate glass sample piece comprises the step of placing the alkali aluminosilicate glass sample piece in a preheating area in a physical tempering furnace for preheating, wherein the preheating time is 120s-180s by setting the preheating temperature of the glass to be 600-720 ℃. So that the glass reaches a semi-plastic state before entering the tempering temperature, and the stress of the glass is eliminated. And (3) physically tempering the preheated silicate glass sample. The temperature and time of physical tempering and tempering wind pressure play an important role in forming the tempering degree and surface stress of the glass, and the glass needs to be determined according to different physical and chemical properties and thickness of the glass. When the thickness of the alkaline aluminosilicate glass sample piece is smaller than 1.1mm, conveying the preheated glass sample piece to a physical tempering area in a physical tempering furnace through a conveying track, wherein the tempering temperature is 650-780 ℃, and the heat preservation time is 90-120 seconds. And cooling the silicate glass sample by adopting a cooling fan, wherein the pressure of the cooling fan is 10000-30000 Pa, the time is 30-60 seconds, and the air temperature is lower than 35 ℃ during quenching. The stress of the glass sample piece after the physical tempering is between 120 and 300Mpa, and the physical tempered glass particles can be kept when the glass is broken after the physical tempering, so that the obtuse angle strip shape can be generated when the aluminosilicate glass product is damaged by impact after being tempered, and the glass can meet the related safety standard. Before chemical tempering is carried out on the aluminosilicate glass piece, the secondary preheating temperature is 350-380 ℃, the preheating time is 30-60 min, and under the temperature and time, the thermal uniformity of the physically tempered glass is good, and the stress non-uniformity caused during chemical tempering can be avoided. The chemical tempering temperature of the aluminosilicate glass piece is 400-450 ℃, and the chemical tempering time is 120-00 min. The chemical tempering time and the chemical tempering temperature are not suitable to be overlong, otherwise, the compressive stress CS of the aluminosilicate glass is excessively large, the physical tempering effect is eliminated, the strip obtuse angle form is easy to appear when the glass is broken, whether the compressive stress CS of the aluminosilicate glass is excessively large after the chemical tempering is judged whether the surface compressive stress CS is more than 700Mpa and less than 850Mpa, when the compressive stress of the chemical tempering is more than 850Mpa, the state situation of fragments is changed, and when the compressive stress CS is less than 700Mpa, the impact resistance of the aluminosilicate glass cannot meet the standard requirement, so that the compressive stress of the aluminosilicate glass is between 700 and 850 Mpa.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a schematic view showing a state after glass breakage according to an embodiment of the present invention;
fig. 2 is a schematic view of a state after breaking a conventional high alumina glass.
Detailed Description
The alkali aluminosilicate glass of the present invention and the process for producing the same will be specifically described with reference to the following examples.
Example 1
An alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 60.65% SiO 2 14.41% of Al 2 O 3 13.38% Na 2 O,5.86% K 2 O,4.95% MgO,0.81% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=780 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=40 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=1.1j.
The preparation process comprises the following steps:
step one: washing the alkaline aluminosilicate glass sample piece with deionized water to remove glass fragments and impurities on the surface of the sample piece, wherein the thickness of the sample piece is 1.1mm; and then placing the cleaned sample into a conveying roller, and entering a physical tempering furnace for preheating, wherein the preheating is performed from room temperature (25 ℃) to 680 ℃, and the preheating time is 180 seconds.
Step two: and (3) physically tempering the aluminosilicate glass sample piece preheated in the step one, wherein the specific steps are as follows: and conveying the preheated glass into a physical tempering area through a conveying belt, wherein the physical tempering temperature is 620 ℃, and the tempering time is 300s. The cold area is reinforced by air cooling, the pressure of a fan is 12000pa, the time is 40s, and the air cooling temperature is 32 ℃.
Step three: and (3) carrying out secondary cleaning and preheating on the sample piece treated in the step (II), wherein the specific steps are as follows: and (3) cleaning the sample piece subjected to the physical tempering in the step two by deionized water, and then sending the sample piece into a tempering furnace for preheating at the preheating temperature of 360 ℃ for 30min.
And fourthly, performing chemical tempering treatment on the silicate glass sample piece obtained in the third step to form a silicate glass product, wherein the chemical tempering temperature is 420 ℃, the tempering molten salt is pure potassium nitrate, the tempering time is 210min, and the sample is naturally cooled in a furnace, annealed to below 100 ℃ and taken out, and is cleaned and dried after being cooled to room temperature. An alkali aluminosilicate glass having a number of 1 was obtained.
Example 2
Example 2 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 60.82% SiO 2 13.58% of Al 2 O 3 14.65% Na 2 O,5.95% K 2 O,4.13% MgO,0.87% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=752 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=36 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=0.8j. An alkali aluminosilicate glass having a number of 2 was obtained.
Example 3
Example 3 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 61.35% SiO 2 14.58% of Al 2 O 3 14.55% Na 2 O,5.12% K 2 O,3.58% MgO,0.82% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=775 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=38 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=0.9J. An alkaline aluminosilicate glass having a number of 3 was obtained.
Example 4
Example 4 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 61.33% SiO 2 14.25% of Al 2 O 3 14.28% Na 2 O,5.12% K 2 O,3.58% MgO,0.82% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=775 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=38 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=0.9J. An alkali aluminosilicate glass having a number of 4 was obtained.
Example 5
Example 5 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 58% SiO 2 15% of Al 2 O 3 15% Na 2 O,6% K 2 O,5% MgO,1% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=785 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=42 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=1.2j. An alkali aluminosilicate glass having a number of 5 was obtained.
In addition, in the preparation process, the physical tempering temperature is 630 ℃, and the tempering time is 280s; the chemical tempering temperature is 430 ℃ and the tempering time is 200min.
Example 6
Example 6 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 65% SiO 2 13% Al 2 O 3 14.05% Na 2 O,3.95% K 2 O,4% MgO; and, the compressive stress of the glass is CS, wherein CS satisfies: cs=775 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=38 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=1.2j. An alkali aluminosilicate glass having a number of 6 was obtained.
In addition, in the preparation process, the physical tempering temperature is 650 ℃, and the tempering time is 280s; the chemical tempering temperature is 420 ℃, and the tempering time is 220min.
Example 7
Example 7 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 61% SiO 2 14% Al 2 O 3 15% Na 2 O,6% K 2 O，3％MgO of (2), zrO 1% 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=781 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=39 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=1.1j. An alkaline aluminosilicate glass having a number of 7 was obtained.
In addition, in the preparation process, the physical tempering temperature is 660 ℃, and the tempering time is 280s; the chemical tempering temperature is 420 ℃, and the tempering time is 250min.
Example 8
Example 8 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 64.53% SiO 2 13.97% of Al 2 O 3 12% Na 2 O,3.5% K 2 O,5% MgO,1% ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=775 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=41 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=0.9J. An alkali aluminosilicate glass having a number of 8 was obtained.
In addition, in the preparation process, the physical tempering temperature is 670 ℃, and the tempering time is 280s; the chemical tempering temperature is 430 ℃ and the tempering time is 190min.
Example 9
Example 9 is substantially the same as example 1, except that,
cs=765 mpa, dol=39 μm, ct=1.1j. An alkaline aluminosilicate glass having a number of 9 was obtained.
In the preparation process, the physical tempering temperature is 620 ℃, and the tempering time is 300s; the chemical tempering temperature is 430 ℃ and the tempering time is 180min.
Example 10
Example 10 is substantially the same as example 1, except that,
cs=765 mpa, dol=39 μm, ct=1.1j. An alkali aluminosilicate glass having a number of 10 was obtained.
In the preparation process, the physical tempering temperature is 620 ℃, and the tempering time is 300s; the chemical tempering temperature is 430 ℃ and the tempering time is 180min.
Example 11
Example 11 is substantially the same as example 1, except that,
cs=761 mpa, dol=36 μm, ct=1.0j. An alkali aluminosilicate glass having a number of 11 was obtained.
In the preparation process, the physical tempering temperature is 610 ℃ and the tempering time is 380s; the chemical tempering temperature is 420 ℃, and the tempering time is 210min.
Example 12
Example 12 is substantially the same as example 1, except that,
cs=750 mpa, dol=35 μm, ct=0.8j. An alkali aluminosilicate glass having a number of 12 was obtained.
In the preparation process, the physical tempering temperature is 610 ℃ and the tempering time is 380s; the chemical tempering temperature is 430 ℃ and the tempering time is 180min.
Example 13
Example 13 is substantially the same as example 1, except that,
cs=761 mpa, dol=38 μm, ct=0.85J. An alkali aluminosilicate glass having a number of 13 was obtained.
In the preparation process, the physical tempering temperature is 610 ℃ and the tempering time is 380s; the chemical tempering temperature is 410 ℃ and the tempering time is 300min.
Example 14
Example 14 is substantially the same as example 1, except that,
cs=785 mpa, dol=37 μm, ct=1.0j. An alkali aluminosilicate glass having a number of 14 was obtained.
In the preparation process, the physical tempering temperature is 680 ℃, and the tempering time is 180s; the chemical tempering temperature is 420 ℃, and the tempering time is 210min.
Example 15
Example 15 is substantially the same as example 1, except that,
cs=778 mpa, dol=36 μm, ct=1.1j. An alkali aluminosilicate glass having a number of 15 was obtained.
In the preparation process, the physical tempering temperature is 680 ℃, and the tempering time is 180s; the chemical tempering temperature is 430 ℃ and the tempering time is 180min.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that,
cs=890mpa, dol=42 μm, ct=1.1j. An alkali aluminosilicate glass numbered 16 was obtained.
In the preparation process, the step of physical tempering is omitted; the chemical tempering temperature is 420 ℃, and the tempering time is 300min.
Comparative example 2
Comparative example 2 is substantially the same as example 1, except that,
cs=140 mpa, dol is undetectable, ct=0.3J. An alkaline aluminosilicate glass having a number of 17 was obtained.
In the preparation process, the step of chemical tempering is omitted; the physical tempering temperature is 620 ℃, and the tempering time is 180s.
Comparative example 3
Comparative example 3 is substantially the same as example 1, except that,
cs=780 mpa, dol=38 mpa, ct=0.9J. An alkali aluminosilicate glass having a number of 18 was obtained.
In the preparation process, the physical tempering temperature is 620 ℃, and the tempering time is 300s; the chemical tempering temperature is 450 ℃, and the tempering time is 300min.
Comparative example 4
Comparative example 4 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 62.52% SiO 2 15.17% of Al 2 O 3 14.1% Na 2 O,5.83% K 2 O, mgO in 1.62% and ZrO in 0.78% 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=776 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=35 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=0.7j. The base number 19 is obtainedAn alumino silicate glass.
Comparative example 5
Comparative example 5 is substantially the same as example 1, except that,
an alkaline aluminosilicate glass comprises the following raw materials in percentage by mass: 60.53% SiO 2 13.41% of Al 2 O 3 12.41% Na 2 O,5.34% K 2 O, mgO in 7.55% and ZrO in 0.76% 2 The method comprises the steps of carrying out a first treatment on the surface of the And, the compressive stress of the glass is CS, wherein CS satisfies: cs=835 Mpa; the depth of the compressive stress layer of the glass is DOL, wherein DOL meets the following conditions: dol=45 μm; the impact energy of the glass is CT, wherein CT satisfies the following conditions: ct=1.1j. An alkali aluminosilicate glass numbered 20 was obtained.
In addition, the alkaline aluminosilicate glass sample element can be prepared by the following method:
the ingredients may be mixed in the proportions described in table 1, the mixed ingredients may be placed in a sealed bag, mixed uniformly in the sealed bag, then poured into a platinum crucible, melted at 1550-1650 ℃, the molten glass is poured into a metal mold, the glass together with the metal mold is placed into an annealing furnace for annealing and cooling, and the glass sheet is processed into an 145mm x73mm x1.1mm and 300mm x1.1mm alkaline aluminosilicate glass sample.
Performance testing
CS, DOL, 4PB, ball drop tests were performed on the alkali aluminosilicate glasses of examples 1-15 and comparative examples 1-5, wherein ball drop test conditions were: 132g steel ball, 15cm base height, 5cm gradient, 3 times/height, until crushing. See table 1 for various examples, comparative examples and test results thereof.
TABLE 1 examples and Performance test results
As can be seen from the combination of examples, comparative examples and Table 1, the glasses of examples 1 to 15, which were prepared by adopting the technical scheme of the present invention, have impact resistance and glass breakage conditions which meet the safety standards of automobile glass. Comparative example 1, compared with example 1 of the present invention, has only chemical tempering, no physical tempering, and has high impact resistance, but the glass is in a strip shape in a broken state, and does not have safety performance; comparative example 2 compared with example 1 of the present invention, only physical tempering without chemical tempering, the glass surface CS was shallower and the impact resistance was lower; comparative example 3 shows a broken state in a bar shape and has low safety performance, although it is physically and chemically tempered, compared with example 1 of the present invention. The lower magnesium oxide content of comparative example 4 and the lower magnesium oxide content of comparative example 5 resulted in lower safety performance of the glass.
According to the alkali aluminosilicate glass strengthening method, through two steps of strengthening, namely physical tempering and chemical tempering, glass particles produced by the method form an obtuse angle and cannot stab people when the glass is broken by heavy impact, higher shock resistance is maintained, and the national requirements on safety of automobile glass are met. The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, the technical proposal of the invention can be changed in a plurality of ways, including the combination of the technical characteristics in any other suitable way, and the simple changes and the combination should be regarded as the disclosure of the invention and all the changes and the combinations are all included in the protection scope of the invention
In the description of the present specification, reference to the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. An alkaline aluminosilicate glass is characterized by comprising 58-65% by mass of SiO 2 13 to 15 percent of Al 2 O 3 12-15% of Na 2 O,0 to 6 percent of K 2 O,3 to 5 percent of alkaline earth metal and 0 to 1 percent of ZrO 2 The method comprises the steps of carrying out a first treatment on the surface of the And, in addition, the processing unit,
the compressive stress of the glass is CS, wherein CS satisfies: CS is more than or equal to 700Mpa and less than or equal to 800Mpa;
the depth of the compressive stress layer of the glass is DOL, wherein the DOL meets the following conditions: DOL is more than or equal to 30 mu m and less than or equal to 40 mu m;
the impact energy of the glass is CT, wherein the CT satisfies the following conditions: CT is more than or equal to 0.8J.
2. The alkali aluminosilicate glass of claim 1, wherein the alkaline earth oxide is magnesium oxide.
3. A process for producing an alkali aluminosilicate glass according to claim 1 or 2, comprising subjecting an alkali aluminosilicate glass sample to a physical tempering treatment and a chemical tempering treatment to obtain the alkali aluminosilicate glass,
the temperature of the physical tempering treatment is 620-780 ℃ and the time is 180-300 s; and/or
The temperature of the chemical tempering treatment is 400-450 ℃ and the time is 120-300 min.
4. The process of claim 3, wherein the silicate glass sample has a thickness of 1.1mm or more.
5. A process according to claim 3, wherein a tempering salt is added during the step of chemical tempering, preferably potassium nitrate.
6. The preparation process according to any one of claims 3 to 5, characterized by comprising the steps of:
step one, cleaning and preheating an alkaline aluminosilicate glass sample;
step two, the silicate glass sample piece treated in the step one is subjected to physical tempering treatment and then cooled;
step three, carrying out secondary cleaning and preheating on the silicate glass sample piece treated in the step two;
and fourthly, performing chemical tempering treatment on the silicate glass sample piece obtained in the third step to form a silicate glass product.
7. The process according to claim 6, wherein in the first step, the preheating is performed at 600 to 720 ℃ for 120 to 180 seconds.
8. The preparation process according to claim 6, wherein the cooling pressure is 8000-12000 pa for 30-60 s; and/or
The preheating temperature is 350-380 ℃, and the preheating time is 30-60 min.
9. Use of an alkali aluminosilicate glass according to claim 1 or 2 or a glass prepared according to the preparation process of any one of claims 3-8, characterized in that the glass is applied to automotive windows.
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