A method for preparing lithium aluminosilicate glass with high elastic modulus

Abstract

The present invention relates to a method for preparing lithium aluminosilicate glass with high elastic modulus, wherein the mass percentage of each component of the lithium aluminosilicate glass is: 50-65% SiO 2 , 15~25% Al 2 O 3 , 2~8% MgO, 2~10% K 2 O, 3~15% Na 2 O, 0.1~1% CaO, 0.5~6% Li 2 O, 0.1~1.5% ZrO 2 , 0.1~1.5% TiO 2 , where RO (Li 2 O+Na 2 O+K 2 O) value is 10%~20%; RO 2 (ZrO 2 +TiO 2 ) value is 0.5%~2%, and the clarifier is 0.1~0.5%. After melting, homogenization, clarification, ultra-fine crystallization and forming annealing, the elastic modulus of lithium aluminum silicate glass can reach 86 GPa.

Description

Technical Field

[0001] The invention relates to the technical field of glass preparation, and in particular to lithium aluminosilicate glass with high elastic modulus and a preparation method thereof. Background Art

[0002] Glass materials are widely used, such as windshields and windows in aerospace, windows in high-speed trains, and cover glass for electronic display devices. With the rapid development of society, the performance requirements for glass materials are getting higher and higher. Not only do they require high elastic modulus, high transmittance, wear resistance, and scratch resistance, but they also require high strength and low density. Lithium aluminum silicon (LAS) glass contains Li + 、Na + and K + A variety of alkali metal ions can be used for secondary chemical strengthening to give the glass surface greater compressive stress, increasing the strength of the glass by nearly 20 times, and are gradually gaining attention in related fields.

[0003] At present, lithium aluminum silicate (LAS) glass is + With strong field strength, Ti 4+ and Zr 4+ It is a commonly used nucleating agent. These ions are easy to crystallize during the glass forming process, thus reducing the elastic modulus and impact resistance of the glass. Therefore, the influence of various glass components and heat treatment on the performance of lithium aluminum silicate (LAS) glass is studied, and different proportions of components are used, combined with ultra-microcrystallization treatment, to develop high elastic modulus lithium aluminum silicate glass. Summary of the invention

[0004] The purpose of the present invention is to solve the defect in the prior art that the glass is easily crystallized during the forming process, thereby reducing the elastic modulus, impact resistance and other properties of the glass, and to provide a method for preparing high elastic modulus lithium aluminum silicate glass.

[0005] The technical solution adopted by the present invention is as follows:

[0006] A method for preparing lithium aluminosilicate glass with high elastic modulus, characterized by comprising the following steps:

[0007] (a) Weigh the following batch materials according to the following mass percentages: 50-65% SiO2, 15-25% Al2O3, 2-8% MgO, 2-10% K2O, 3-15% Na2O, 0.1-1% CaO, 0.5-6% Li2O, 0.1-1.5% ZrO2, 0.1-1.5% TiO2, of which RO (Li2O+Na2O+K2O) value is 10%-20%; RO2 (ZrO2+TiO2) value is 0.5%-2%, and clarifier is 0.1-0.5%;

[0008] (b) The glass batch material (a) is melted, homogenized and clarified in a high temperature furnace; the temperature is lowered to 800°C-1100°C for ultrafine crystallization treatment for 1-5 min, during which crystal nuclei are formed and a small amount of microcrystals are precipitated; the glass batch material is then annealed at 500-650°C for 10-25 min and then cooled in the furnace.

[0009] On the basis of the above technical solutions, there are also the following further technical solutions:

[0010] In step (a), the clarifier is selected from one or more of sulfate, nitrate, fluoride and chloride;

[0011] The temperature of melting, homogenizing and clarifying in step (b) is 1550-1660°C;

[0012] The ultra-microcrystallization heat preservation treatment in step (b) is 800°C-1100°C, and the treatment time is 2-5 min. The annealing temperature in step (b) is 500-650°C, and the annealing time is 10-25 min, and then the alloy is cooled in the furnace.

[0013] In the above technical solution, compared with conventional lithium aluminum silicate glass, this invention adopts an optimized composition formula combined with microcrystallization and heat preservation treatment to improve the elastic modulus. In a short treatment process, new structural changes occur inside the glass, which ultimately leads to an increase in the elastic modulus.

[0014] Advantages of the invention:

[0015] The method for preparing lithium aluminum silicate glass with high elastic modulus provided by the present invention can prepare lithium aluminum silicate glass with high elastic modulus, and secondary strengthening can be performed according to needs to further improve its performance. It can be applied to but not limited to windshields and window glass in aerospace, window glass in high-speed railways, and cover glass of electronic display equipment. Specific implementation plan

[0016] Example 1

[0017] A method for preparing high elastic modulus lithium aluminosilicate glass comprises the following steps:

[0018] (a) Weigh the following raw materials according to the following mass percentages:

[0019] SiO2: 55%,

[0020] Al2O3: 20%,

[0021] MgO: 8 %,

[0022] K2O: 6 %,

[0023] Na2O: 9%,

[0024] CaO: 0.1~1%,

[0025] Li2O: 0.5 %,

[0026] ZrO2: 1 %,

[0027] TiO2: 0.4 %,

[0028] Clarifying agent is ammonium sulfate: 0.1%

[0029] (b) The glass batch raw materials of (a) are melted, homogenized and clarified in a high temperature furnace at 1600°C; ultrafine crystallization treatment is carried out at 800°C for 5 min, and then annealed at 550°C for 25 min, and then cooled in the furnace.

[0030] The lithium aluminosilicate glass obtained through the above steps was subjected to Young's modulus test on an MK7 Young's modulus tester produced by Gridosonic in Belgium. The results were obtained after repeated testing for multiple times, and the elastic modulus was 86 GPa.

[0031] Embodiment 2:

[0032] A method for preparing high elastic modulus lithium aluminosilicate glass comprises the following steps:

[0033] (a) Weigh the following raw materials according to the following mass percentages:

[0034] SiO2: 50%,

[0035] Al2O3: 22.3 %,

[0036] MgO: 6 %,

[0037] K2O: 2 %,

[0038] Na2O: 14 %,

[0039] CaO: 0.5%,

[0040] Li2O: 4 %,

[0041] ZrO2: 0.6 %,

[0042] TiO2: 0.6 %,

[0043] Clarifying agent is sodium sulfate and sodium nitrate added in equal amounts: 0.5%

[0044] (b) The glass batch material of (a) is melted, homogenized and clarified in a high temperature furnace at 1550°C; subjected to ultrafine crystallization treatment at 950°C for 3 min, and then annealed at 650°C for 10 min, and then cooled in the furnace.

[0045] The lithium aluminum silicate glass obtained through the above steps was tested for Young's modulus on the MK7 Young's modulus tester produced by Gridosonic in Belgium. The results were obtained by repeated testing, and the elastic modulus was 86 GPa.

[0046] Embodiment 3:

[0047] A method for preparing high elastic modulus lithium aluminosilicate glass comprises the following steps:

[0048] (a) Weigh the following raw materials according to the following mass percentages:

[0049] SiO2: 63%,

[0050] Al2O3: 15 %,

[0051] MgO: 2 %,

[0052] K2O: 10%,

[0053] Na2O: 3 %,

[0054] CaO: 1 %,

[0055] Li2O: 5 %,

[0056] ZrO2: 0.9 %,

[0057] TiO2: 0.1 %,

[0058] Clarifying agent is sodium chloride: 0.3%

[0059] (b) The glass batch raw materials of (a) are melted, homogenized and clarified in a high-temperature furnace at 1660°C; ultrafine crystallization treatment is carried out at 1100°C for 2 min, and then annealed at 600°C for 15 min, and then cooled in the furnace.

[0060] The lithium aluminosilicate glass obtained through the above steps was subjected to Young's modulus test on an MK7 Young's modulus tester produced by Gridosonic in Belgium. The results were obtained by repeated testing many times, and the elastic modulus was 88 GPa.

Claims

1. A method for preparing lithium aluminosilicate glass with high elastic modulus, characterized in that The following steps are involved: (a) Weigh the following raw materials according to the following mass percentages: SiO2: 50%, Al2O3: 22.3 %, MgO: 6 %, K2O: 2 %, Na2O: 14 %, CaO: 0.5%, Li2O: 4 %, ZrO2: 0.6 %, TiO2: 0.6 %, The clarifier is sodium sulfate and sodium nitrate added in equal amounts: 0.5%, (b) The glass batch material (a) is fed into a high temperature furnace for melting, homogenization and clarification at 1550°C; ultrafine crystallization treatment is carried out at 950°C for 3 min, and then annealing is carried out at 650°C for 10 min, and then cooled in the furnace.

2. A method for preparing lithium aluminosilicate glass with high elastic modulus, characterized in that The following steps are involved: (a) Weigh the following raw materials according to the following mass percentages: SiO2: 63%, Al2O3: 15 %, MgO: 2 %, K2O: 10%, Na2O: 3 %, CaO: 1 %, Li2O: 5 %, ZrO2: 0.9 %, TiO2: 0.1 %, Clarifying agent is sodium chloride: 0.3%, (b) The glass batch material (a) is fed into a high temperature furnace for melting, homogenization and clarification at 1660°C; ultrafine crystallization treatment is performed at 1100°C for 2 min, and then annealing is performed at 600°C for 15 min, and then cooled in the furnace.