CN111072292A - Glass strengthening process capable of shortening strengthening time - Google Patents
Glass strengthening process capable of shortening strengthening time Download PDFInfo
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- CN111072292A CN111072292A CN201911357047.2A CN201911357047A CN111072292A CN 111072292 A CN111072292 A CN 111072292A CN 201911357047 A CN201911357047 A CN 201911357047A CN 111072292 A CN111072292 A CN 111072292A
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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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- 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
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The invention relates to the technical field of glass cover plate strengthening, in particular to a glass strengthening process capable of shortening strengthening time, which comprises the following steps: (1) when the number of the furnaces is 0 to (15-18), putting the glass into the potassium nitrate molten salt, and strengthening for 4-5h at the temperature of 415-425 ℃; (2) when the number of the furnaces is (15-18) - (30-40), the glass is put into the potassium nitrate molten salt and strengthened for 8-11h at the temperature of 390-400 ℃. The invention can greatly shorten the strengthening time by properly increasing the strengthening temperature at the front furnace number, and can also obtain the required stress layer compression depth and stress layer compression depth by strengthening at the normal temperature at the rear furnace number, the service life of the furnace salt is not changed, and the processing period can be shortened and the processing efficiency can be improved under the condition of almost using electricity.
Description
Technical Field
The invention relates to the technical field of glass cover plate strengthening, in particular to a glass strengthening process capable of shortening strengthening time.
Background
In recent years, devices such as smartphones and tablet computers have become widespread, and a trend toward reduction in thickness and weight has been shown. One problem with thinning is that the strength of the glass decreases with decreasing thickness. In order to be able to meet the requirements of use, it is necessary for the display glass to have a high strength even at small thicknesses. To achieve this, the glass needs to be strengthened.
Currently, the composition of aluminosilicate glass used is high in the content of alkali metal oxide in order to ensure ion exchange capacity and in consideration of factors such as melting property, formability, resistance to devitrification of the glass. When the aluminosilicate glass is strengthened, a chemical toughening method is generally selected because the glass is thin and the physical toughening effect is not obvious. The chemical tempering method is usually low-temperature formingChemical tempering, a low temperature type ion exchange process, involves immersing the glass in a molten salt (usually KNO)3With NaNO3Mixed molten salt of (1), with KNO3Mainly), ion exchange is carried out for a period of time (usually 5-20h) at a certain temperature (usually 350-550 ℃).
Generally, increasing the chemical strengthening temperature and prolonging the chemical strengthening time can increase the stress layer depth of the glass, but too high a chemical strengthening temperature and too long a chemical strengthening time can cause the stress relaxation of the glass, and reduce the compressive stress and the bending strength of the glass surface, but increasing the strengthening temperature appropriately can shorten the strengthening time.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the invention aims to provide a glass strengthening process capable of shortening strengthening time, wherein the strengthening time can be greatly shortened by properly increasing the strengthening temperature in the front furnace number, the strengthening is performed at normal temperature in the rear furnace number, the required stress layer compression depth and stress layer compression depth can be obtained, the service life of furnace salt is not changed, and the processing period and the processing efficiency can be shortened under the condition of almost no more electric quantity.
The purpose of the invention is realized by the following technical scheme: a glass strengthening process capable of shortening strengthening time comprises the following steps:
(1) when the number of the furnaces is 0 to (15-18), putting the glass into the potassium nitrate molten salt, and strengthening for 4-5h at the temperature of 415-425 ℃;
(2) when the number of the furnaces is (15-18) - (30-40), the glass is put into the potassium nitrate molten salt and strengthened for 8-11h at the temperature of 390-400 ℃.
The invention can greatly shorten the strengthening time by properly increasing the strengthening temperature at the front furnace number, and can also obtain the required stress layer compression depth and stress layer compression depth by strengthening at the normal temperature at the rear furnace number, the service life of the furnace salt is not changed, and the processing period can be shortened and the processing efficiency can be improved under the condition of almost using electricity.
Preferably, in the step (1), the glass is aluminosilicateThe salt glass comprises the following components in percentage by weight: SiO 22：55％-65％、Al2O3：13％-17％、Na2O：12％-16％、K2O：1％-3％、MgO：3％-5％、CaO：0.2％-2.0％、B2O3：0.2％-2.0％、P2O5:0.1％-0.5％、ZrO2：0.1％-0.5％、ZnO：0-2％、TiO2：0-2％、CeO2：0-0.5％、SnO2: 0 to 0.5 percent, and the sum of the weight percent of the components is 100 percent.
According to the invention, by adopting the aluminosilicate glass and strictly controlling the weight percentage of each component, the prepared aluminosilicate glass has high surface compressive stress and stress layer compression depth after being strengthened, and also has excellent mechanical properties, high surface hardness, toughness, scratch resistance and anti-falling performance.
Preferably, the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：58％-62％、Al2O3：14％-16％、Na2O：13％-15％、K2O：1.5％-2.5％、MgO：3.5％-4.5％、CaO：0.5-1.5％、B2O3：0.5％-1.5％、P2O5:0.1％-0.3％、ZrO2：0.2％-0.4％、ZnO：0.2％-0.8％、TiO2：0.2％-0.8％、CeO2：0.2％-0.4％、SnO2: 0.1 to 0.3 percent, and the sum of the weight percent of the components is 100 percent.
Preferably, the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：60％、Al2O3：15％、Na2O：14％、K2O：2％、MgO：4％、CaO：1％、B2O3：1％、P2O5:0.25％、ZrO2：0.25％、ZnO：1％、TiO2：1％、CeO2：0.25％、SnO2：0.25％。
The reason why the glass composition is limited to the above range is as follows:
silicon dioxide (SiO)2) Is the main component for forming the glass skeleton, and has the functions of raising the strain point, chemical stability and mechanical strength of glass and lowering the thermal expansion coefficient and density of glass. When the content is less than 50%, the chemical stability of the glass is poor, but when the content exceeds 68%, the high-temperature viscosity of the glass increases, so that the melting temperature of the glass becomes too high and the melting becomes difficult. To obtain a glass with a high Young's modulus suitable for rapid chemical strengthening, SiO2The content of (B) is limited to 55-65%, preferably 58-62%.
Alumina (Al)2O3) Is an intermediate oxide, improves the hardness and mechanical strength of the glass, improves the chemical stability of the glass and can accelerate the ion exchange of the glass surface. When the content is less than 10%, the ion exchange effect is not good, the chemical stability of the glass is not good, when Al is used2O3When the content exceeds 18%, the viscosity of the glass increases and the devitrification resistance becomes poor. Thus, Al2O3The content of (b) is limited to 13 to 17%, preferably 14 to 16%.
Sodium oxide (Na)2O) is an essential component for ion exchange, and also lowers the melting temperature of the glass, improves the tendency of the glass to devitrify, improves the melting property and the formability of the glass, and improves the devitrification resistance of the glass. Na (Na)2When the content of O is less than 11%, the ion exchange performance is poor and the strengthening effect is weak. When Na is present2When the content of O exceeds 18%, the thermal expansion coefficient of the glass becomes too large, and the chemical stability and thermal shock resistance are lowered. Thus, Na will be2The content of O is limited to 12-16%, preferably 13-15%.
Potassium oxide (K)2O) is capable of lowering the high-temperature viscosity of the glass to improve the meltability and formability of the glass, and is capable of reacting with Na+The ion exchange speed in the chemical strengthening is increased by interdiffusion during the ion exchange to obtain the required compressive stress and deepen the depth of the compressive stress layer, and the devitrification resistance of the glass can be improved. When K is2When the content of O exceeds 3%, the ion exchange rate is hindered, and the strengthening effect is impaired. When K is2The content of O is between 1 and 3 percent, which not only can improve the etching rate, but also can shorten the time of ion exchange treatment, so K2The content of O is limited to 1-3% is preferably 1.5-2.5%.
The glass of the invention does not contain any Li2O，Li2O is contained in the glass component at most 0.1%, which is an optional component. Certain Li in the glass2The O concentration helps to lower the melt viscosity of the glass and thus improves the melting effect, and a small amount of Li2O helps to improve the water resistance of the glass, but higher Li2O tends to inhibit Na + and K + exchange and the glass raw material cost greatly increases, so that Li-free is preferred in the present invention2O。
Magnesium oxide (MgO) is a glass network external body, and a certain amount of magnesium oxide (MgO) is introduced to promote the melting of glass and reduce the melting temperature of the glass. MgO also reduces the tendency and rate of crystallization and improves the chemical stability of the glass. If the MgO content is less than 2%, the effect of lowering the melting temperature of the glass is not significant; however, the content should not be too large, and if it exceeds 7%, the glass tends to be loose, the density decreases, the glass tends to be crystallized, and the coefficient of expansion becomes too high. Therefore, the content thereof is limited to 3% to 5%, preferably 3.5% to 4.5%.
Calcium oxide (CaO) is a component that lowers the high-temperature viscosity of glass, provides chemical stability, and promotes melting or formability of glass, and also has the effect of increasing the strain point or tensile elastic modulus of glass. When the CaO content exceeds 3%, the ion exchange property is deteriorated, the strengthening effect is weak, and the devitrification resistance of the glass is deteriorated, so that the CaO content is limited to 0.2% to 2.0%, preferably 0.5% to 1.5%.
Boron oxide (B)2O3) Mainly used for reducing the melting temperature of glass, has the effect second to alkali metal, can accelerate the melting and clarification of the glass, improve the luster of the glass, improve the chemical stability of the glass and also improve the mechanical property of the glass, but B2O3The content of more than 4 wt% inhibits the ion exchange depth of the glass, and therefore, the content thereof is limited to 0.2 to 2%, preferably 0.5 to 1.5%.
Phosphorus oxide (P)2O5) The method is used for accelerating the ion exchange speed of the glass and can also reduce the melting temperature of the glass. P2O5With [ PO ]4]The tetrahedra being interconnected to form a network, P2O5The network structure formed is layered and the layers are connected with each other by van der waals force, and if the content is more than 1%, the chemical stability of the glass is lowered and the thermal expansion coefficient is increased. Therefore, the content thereof is limited to 0.1% to 0.5%, preferably 0.1% to 0.3%.
Zirconium dioxide (ZrO)2) The ion exchange performance and the strain point of the aluminosilicate glass can be obviously improved, the strength of matrix glass can be improved, and the chemical stability, the thermal stability and the scratch resistance of the glass are improved, but when the content is higher than 1 percent, the melting temperature of the glass is increased, and infusible matters in the glass are increased, so that the content is limited to 0.1 to 0.5 percent, and the preferable content is 0.2 to 0.4 percent.
The alkaline earth metal oxide stabilizes the glass and prevents the generation of devitrification in the glass, but has the effect of inhibiting ion exchange. The glass composition of the present invention does not contain alkaline earth metals other than MgO and CaO, and ZnO and TiO which are advantageous for improving ion exchange are introduced2To improve the stability of the glass.
Zinc oxide (ZnO) is a fluxing component in glass and has the effect of improving the ion exchange properties of the glass, in particular the compressive stress of the glass. When the ZnO content is too high to exceed 3%, the glass tends to undergo phase separation, resulting in poor devitrification. Therefore, the content thereof is limited to 0 to 2%, preferably 0.5% to 1.5%.
Titanium oxide (TiO)2) Has the effects of improving the ion exchange performance of the glass and improving the mechanical strength of the glass substrate. When TiO is present2When the content exceeds 1%, the glass tends to have poor resistance to devitrification. Therefore, the content thereof is limited to 0 to 2%, preferably 0.5% to 1.5%.
Cerium oxide (CeO)2) And tin oxide (SnO)2) Are added as fining agents to the glass composition of the present invention, usually in the amount of 0.1% to 1.0%, to eliminate bubbles in the molten glass when CeO is present2And SnO2When the mass percent of the raw materials is 0.1-0.5%, the effect of completely removing bubbles can be achieved while saving raw materials. The glass of the present invention is an aluminosilicate glass system because the components thereof containThe present invention utilizes a clarifying agent cerium oxide (CeO) to make it difficult to melt and clarify molten glass by increasing the viscosity and surface tension of molten glass due to a large amount of alumina2) And tin oxide (SnO)2) To achieve the clarification effect of the glass.
In addition, the aluminosilicate glass of the present invention also satisfies the following requirements:
preferably, the components satisfy the following formula: 70% < SiO2+Al2O3Is < 78%. The mechanical strength and ion exchange effect of the glass can be improved.
Preferably, the components satisfy the following formula: 14% < Na2O+K2O is less than 18 percent. The ion exchange rate in chemical strengthening can be increased to achieve the desired surface compressive stress and stress layer compression depth.
Preferably, the components satisfy the following formula: k is more than 0.12O/Na2O＜0.2。K2When the O content is too high, the ion exchange rate is hindered, and the strengthening effect is affected, so that the K is controlled2O and Na2The proportion of O can obtain higher surface compressive stress and stress layer compression depth.
Preferably, the components satisfy the following formula: 4 percent to less than MgO plus CaO to less than 6 percent. Although the alkaline earth metal oxide stabilizes the glass and prevents the generation of devitrification in the glass, it has the effect of inhibiting ion exchange, so that the amount of MgO + CaO used is controlled to 4% to 6%.
Preferably, the components satisfy the following formula: 0.5% < ZrO2+ZnO+TiO2Is less than 2.0 percent. Can improve the chemical stability, thermal stability and scratch resistance of the glass.
Preferably, the components satisfy the following formula: 0.5% < CeO2+SnO2Is less than 1.0 percent. The effect of completely removing bubbles can be achieved while saving raw materials.
The invention has the beneficial effects that: the invention can greatly shorten the strengthening time by properly increasing the strengthening temperature at the front furnace number, and can also obtain the required stress layer compression depth and stress layer compression depth by strengthening at the normal temperature at the rear furnace number, the service life of the furnace salt is not changed, and the processing period can be shortened and the processing efficiency can be improved under the condition of almost using electricity.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
A glass strengthening process capable of shortening strengthening time comprises the following steps:
(1) when the number of furnaces is 0-15, putting the glass into the potassium nitrate molten salt, and strengthening for 5 hours at the temperature of 415 ℃;
(2) when the number of furnaces is 15-30-furnaces, putting the glass into the potassium nitrate molten salt, and strengthening for 11 hours at the temperature of 390 ℃.
In the step (1), the glass is aluminosilicate glass, and the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：58％、Al2O3：16％、Na2O：15％、K2O：2.5％、MgO：4.5％、CaO：0.5％、B2O3：0.5％、P2O5:0.1％、ZrO2：0.2％、ZnO：0.5％、TiO2：1.5％、CeO2：0.4％、SnO2：0.3％。
Example 2
A glass strengthening process capable of shortening strengthening time comprises the following steps:
(1) when the number of furnaces is 0-16, putting the glass into the potassium nitrate molten salt, and strengthening for 4.5 hours at the temperature of 420 ℃;
(2) when the number of furnaces is 16-35, putting the glass into the potassium nitrate molten salt, and strengthening for 9 hours at the temperature of 395 ℃.
In the step (1), the glass is aluminosilicate glass, and the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：60％、Al2O3：15％、Na2O：14％、K2O：2％、MgO：4％、CaO：1％、B2O3：1％、P2O5:0.25％、ZrO2：0.25％、ZnO：1％、TiO2：1％、CeO2：0.25％、SnO2：0.25％。
Example 3
A glass strengthening process capable of shortening strengthening time comprises the following steps:
(1) when the number of furnaces is 0-18, putting the glass into the potassium nitrate molten salt, and strengthening for 4 hours at the temperature of 425 ℃;
(2) when the number of furnaces is 18-40, putting the glass into the potassium nitrate molten salt, and strengthening for 8 hours at the temperature of 400 ℃.
In the step (1), the glass is aluminosilicate glass, and the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：62％、Al2O3：14％、Na2O：13％、K2O：1.5％、MgO：3.5％、CaO：1.5％、B2O3：1.5％、P2O5:0.3％、ZrO2：0.4％、ZnO：1.5％、TiO2：0.5％、CeO2：0.2％、SnO2：0.1％。
The invention can greatly shorten the strengthening time by properly increasing the strengthening temperature at the front furnace number, and can also obtain the required stress layer compression depth and stress layer compression depth by strengthening at the normal temperature at the rear furnace number, the service life of the furnace salt is not changed, and the processing period can be shortened and the processing efficiency can be improved under the condition of almost using electricity.
The glass surface compressive stress strengthened by the glass strengthening process can reach 750-800MPa, the compression depth of the stress layer can reach 45-50 mu m, and the glass has excellent mechanical property, higher surface hardness, toughness, scratch resistance and anti-falling performance.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A glass strengthening process capable of shortening strengthening time is characterized in that: the method comprises the following steps:
(1) when the number of the furnaces is 0 to (15-18), putting the glass into the potassium nitrate molten salt, and strengthening for 4-5h at the temperature of 415-425 ℃;
(2) when the number of the furnaces is (15-18) - (30-40), the glass is put into the potassium nitrate molten salt and strengthened for 8-11h at the temperature of 390-400 ℃.
2. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: in the step (1), the glass is aluminosilicate glass, and the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：55％-65％、Al2O3：13％-17％、Na2O：12％-16％、K2O：1％-3％、MgO：3％-5％、CaO：0.2％-2.0％、B2O3：0.2％-2.0％、P2O5:0.1％-0.5％、ZrO2：0.1％-0.5％、ZnO：0-2％、TiO2：0-2％、CeO2：0-0.5％、SnO2: 0 to 0.5 percent, and the sum of the weight percent of the components is 100 percent.
3. The glass strengthening process capable of shortening the strengthening time according to claim 2, wherein: the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：58％-62％、Al2O3：14％-16％、Na2O：13％-15％、K2O：1.5％-2.5％、MgO：3.5％-4.5％、CaO：0.5-1.5％、B2O3：0.5％-1.5％、P2O5:0.1％-0.3％、ZrO2：0.2％-0.4％、ZnO：0.2％-0.8％、TiO2：0.2％-0.8％、CeO2：0.2％-0.4％、SnO2: 0.1 to 0.3 percent, and the sum of the weight percent of the components is 100 percent.
4. The process of claim 2, wherein the strengthening time is reducedThe method comprises the following steps: the aluminosilicate glass comprises the following components in percentage by weight: SiO 22：60％、Al2O3：15％、Na2O：14％、K2O：2％、MgO：4％、CaO：1％、B2O3：1％、P2O5:0.25％、ZrO2：0.25％、ZnO：1％、TiO2：1％、CeO2：0.25％、SnO2：0.25％。
5. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: 70% < SiO2+Al2O3＜78％。
6. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: 14% < Na2O+K2O＜18％。
7. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: k is more than 0.12O/Na2O＜0.2。
8. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: 4 percent to less than MgO plus CaO to less than 6 percent.
9. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: 0.5% < ZrO2+ZnO+TiO2＜2.0％。
10. The glass strengthening process capable of shortening the strengthening time according to claim 1, wherein: the components satisfy the following formula: 0.5% < CeO2+SnO2＜1.0％。
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| CN116354601A (en) * | 2023-04-14 | 2023-06-30 | 清远南玻节能新材料有限公司 | Aluminosilicate glass and method for producing same |
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