High-performance microcrystalline glass and preparation method thereof

Abstract

The invention belongs to the technical field of glass ceramics, and particularly relates to high-performance glass ceramics and a preparation method thereof.The preparation method comprises the following steps that S101, all component raw materials for preparing the glass ceramics are evenly mixed, put into an alumina crucible and placed in a high-temperature furnace to be melted for 3-5 h at the temperature of 1550-1650 DEG C; s102, after melting is completed, the temperature is reduced to 1450-1550 DEG C, and a clarifying agent accounting for 0.1%-0.8% of the total mass of all the raw materials of the microcrystalline glass is scattered for clarification; s103, after the clarification is finished, taking out the crucible, rapidly pouring the crucible into deionized water for quenching, and then drying, grinding and sieving to obtain basic glass powder; s104, a mold is preheated to 550-580 DEG C, the basic glass powder is put into the mold to be pressed, then two times of nucleation and one time of crystallization are carried out, and the high-performance glass ceramic is obtained. The microcrystalline glass prepared by the invention has relatively high transmittance and optical performance.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of glass-ceramics, and particularly relates to a high-performance glass-ceramic and a preparation method thereof. BACKGROUND

[0002] Glass-ceramics is a new type of composite material which uniformly precipitates crystal phase in a glass matrix through a controlled crystallization process, and has the advantages of high chemical stability of glass and high mechanical strength and heat resistance of ceramics, and has irreplaceable value in the fields of aerospace, precision optics, semiconductor manufacturing and the like. In particular, high-strength and ultra-low thermal expansion coefficient glass-ceramics have become the core materials of high-precision instrument substrates, laser gyroscope cavities and extreme ultraviolet lithography machine optical systems.

[0003] The clarifying agent used in the preparation process of the glass-ceramic serves to improve the uniformity and transparency of the melt by promoting the coalescence, floating and escape of bubbles, so as to improve the optical performance and crystallization quality of the glass. Commonly used clarifying agents mainly include antimony trioxide and arsenic trioxide. Such clarifying agents have strong volatility and are easy to produce harmful gases in the high-temperature melting process, which not only causes environmental pollution, but also affects the stability of the glass composition. In view of the shortcomings of antimony trioxide, some non-toxic clarifying agents such as cerium dioxide and tin dioxide are used to improve the clarifying effect to some extent, but the high melt viscosity is high, the bubble floating rate is slow, and the bubbles are easy to be retained in the melt, resulting in the existence of small bubbles and stripe defects in the glass, thereby affecting the optical uniformity and transparency of the product. In addition, a single clarifying agent cannot meet the requirements of melt clarification and crystal nucleus regulation, and lacks effective nucleation promotion in the cooling and crystallization stage, which easily causes uneven crystal grain size distribution or incomplete crystallization, and affects the mechanical and optical properties of the material. Therefore, it is necessary to prepare a new clarifying agent to overcome the problems of single function, limited clarifying efficiency and insufficient crystallization regulation ability of the clarifying agent in the prior art. SUMMARY

[0004] In view of the problems existing in the prior art, the application provides a high-performance glass-ceramic and a preparation method thereof.

[0005] The technical solution of the application for solving the above technical problems is as follows: A preparation method of a high-performance glass-ceramic, comprising the following steps: S101, uniformly mixing each component raw material for preparing the glass-ceramic, loading into an alumina crucible, and placing in a high-temperature furnace to melt at 1550-1650 DEG C for 3-5 h; S102, after completing the melting, reducing the temperature to 1450-1550 DEG C, and scattering 0.1%-0.8% of a clarifying agent based on the total mass of each component raw material of the glass-ceramic to clarify; S103, after the clarification, the crucible is taken out and quickly poured into deionized water for rapid cooling, and then dried, ground and sieved to obtain a base glass powder; S104, the mold is preheated to 550-580℃, and the base glass powder is loaded into the mold for pressing, and then twice nucleation and once crystallization are performed to obtain the high-performance glass-ceramic; Further, the components of the glass-ceramic prepared in step S101 include SiO2: 38-48%, Al2O3: 20-25%, Na2O: 16-21%, Li2O: 1-4%, B2O3: 2-7%, ZrO2: 3-6%, TiO2: 0.1-1%, P2O5: 0.5-4%, MgO: 0.1-2%, SrO: 0.1-4%, Gd2O3: 0.5-5%, Y2O3: 0.1-1%, Yb2O3: 0.1-1%, Sm2O3: 0.1-1%, La2O3: 0.1-3%, Er2O3: 0.05-0.5%, Nd2O3: 0.05-1%, CeO2: 0.1-1% by weight percentage.

[0006] Further, in step S103, drying is performed at 105℃, grinding is performed at a speed of 200-600 rpm for 10-30 min, and sieving is performed through a 200 mesh sieve.

[0007] Further, the pressing condition in step S104 is 15 MPa pressure forming.

[0008] Further, the twice nucleation condition in step S104 is that the first nucleation temperature is 500-560℃, and the holding time is 2-3 h; the second nucleation temperature is 600-640℃, and the holding time is 2-3 h; the once crystallization condition is that the crystallization temperature is 650-800℃, and the crystallization time is 1-2 h.

[0009] The clarifying agent comprises zirconium oxide, lithium nitrate, lanthanum nitrate hexahydrate and cerium nitrate hexahydrate; the preparation method of the clarifying agent comprises the following steps: S201, 40-70 parts of zirconium oxide are weighed according to weight parts, dried to obtain dried zirconium oxide; S202, the dried zirconium oxide is added to the reaction bottle, a mixed solution of anhydrous ethanol and deionized water is added to the reaction bottle according to a solid-liquid ratio of 1:10, then polyvinylpyrrolidone is added, and stirring and ultrasonic treatment are performed to obtain a zirconium oxide suspension, the mass ratio of the zirconium oxide to the polyvinylpyrrolidone being 100: (1-5); S203, 5-18 parts of lithium nitrate, 15-22 parts of lanthanum nitrate hexahydrate and 10-22 parts of cerium nitrate hexahydrate are weighed in a reaction container, deionized water and anhydrous ethanol are added according to the solid-liquid ratio of 1:2.5, stirring, adjusting the pH to 3.5-4.5, and preparing a shell precursor solution; S204, the shell precursor solution is added dropwise to the zirconia suspension, stirring at a speed of 300 rpm, the dropwise time is 45-60 min; after the dropwise addition is completed, continue to stir at a speed of 300 rpm for 1-2 h; then remove the solvent under reduced pressure, recover the solid and wash with deionized water, filter and dry to obtain a dry powder; S205, the dry powder is subjected to staged temperature calcination, anhydrous ethanol is added to the calcined product according to the solid-liquid ratio of 1:2.5, and ball milling is carried out to obtain the clarifier.

[0010] Further, in the mixed solution of anhydrous ethanol and deionized water in step S202, the volume ratio of anhydrous ethanol to deionized water is 1:(3-5).

[0011] Further, in step S205, the staged temperature calcination conditions are as follows: first, the temperature is raised to 200 DEG C and kept for 1-2 h, then the temperature is raised to 350-450 DEG C at a rate of 5 DEG C / min, and kept for 1-2 h; then the temperature is raised to 750-820 DEG C at a rate of 5 DEG C / min, and kept for 1-2 h.

[0012] Further, in step S205, the ball milling conditions are as follows: zirconia balls are used as the grinding medium, the rotation speed is 300 rpm, the ball-to-material ratio is 5:1, and the ball milling time is 4-5 h.

[0013] The present application provides a kind of microcrystalline glass prepared by the preparation method of high-performance microcrystalline glass.

[0014] Compared with the prior art, the beneficial effects of the present application are: the clarifier provided by the present application adopts a core-shell structure design, and through the synergistic effect of multiple components, the double regulation of the glass melt clarification process and crystallization behavior is realized; the cerium nitrate hexahydrate in the clarifier can release oxygen at high temperature, effectively remove the bubbles in the melt, and achieve sufficient clarification; the introduction of light rare earth element lanthanum can significantly reduce the high temperature viscosity of the melt, accelerate the bubble floating and escaping process, and make the clarification more thorough.

[0015] The mutual cooperation between the components in the clarifying agent optimizes the thermodynamic and kinetic conditions of the melt, not only inhibits the bubble regeneration, but also provides a favorable environment for the subsequent crystal nucleus formation and grain uniform growth; in addition, the element composition in the clarifying agent is derived from the composition of the glass-ceramic system itself, effectively avoiding the introduction of exogenous impurities, ensuring the chemical compatibility and structural stability of the melt reaction process. The clarifying agent prepared in the application reduces the bubble density in the melt by the synergistic clarification mechanism, and the internal structure of the glass is more dense and uniform, and the prepared glass-ceramics has higher transmittance and more excellent optical performance. BRIEF DESCRIPTION OF DRAWINGS

[0016] Fig. 1 Process flow chart for the glass-ceramics prepared in the application; Fig. 2 Process flow chart for the clarifying agent prepared in the application. DETAILED DESCRIPTION

[0017] The principles and characteristics of the application are described below in conjunction with the drawings, and the examples are only used to explain the application and not to limit the scope of the application.

[0018] Referring to the drawings Figs. 1-2 The application provides: Example 1 1. Preparation of clarifying agent S201, weigh 70 g of zirconium oxide and place it in a drying oven at 120℃ for 2h, then transfer it to a desiccator and cool it to room temperature to obtain dried zirconium oxide; S202, add 525 mL of anhydrous ethanol and 175 mL of deionized water to a reaction bottle, then add 3.5 g of polyvinylpyrrolidone, stir at a speed of 80 rpm to dissolve it, then add the dried zirconium oxide to the reaction bottle and stir at a speed of 80 rpm to dissolve it, then ultrasonic at a power of 300 w for 15 min to obtain a zirconium oxide suspension; S203, add 75 mL of deionized water to a 500 mL beaker, then add 5 g of lithium nitrate, 15 g of lanthanum nitrate hexahydrate and 10 g of cerium nitrate hexahydrate, heat to 40℃ and stir at a speed of 80 rpm to dissolve it, then slowly add 75 mL of anhydrous ethanol solution, and adjust the pH of the solution to 3.5 with appropriate amount of acetic acid to obtain a shell precursor solution; S204. The shell precursor solution was slowly added dropwise to the zirconium oxide suspension through a titration funnel while stirring at 300 rpm for 60 min. After the addition was completed, stirring was continued at 300 rpm for 2 h. Then, the solvent was removed by vacuum concentration in a rotary evaporator at 180 rpm and 60 °C. The solid was recovered, washed with deionized water, filtered, and dried in an 80 °C drying oven to constant weight to obtain a dry powder. S205. The above-mentioned dried powder is placed in a porcelain boat and heated in a muffle furnace by a programmed temperature increase. First, it is heated to 200℃ and held for 2 hours. Then, the temperature is increased to 450℃ at 5℃ / min and held for 2 hours. The temperature is then increased to 820℃ at 5℃ / min and held for 2 hours. After that, it is cooled to room temperature to obtain the calcined product. The calcined product is added to anhydrous ethanol at a solid-liquid ratio of 1:2.5 and placed in a planetary ball mill. Zirconia balls are used as the grinding medium. The milling speed is 300 rpm and the ball-to-material ratio is 5:1. The milling is carried out for 5 hours to obtain a slurry. The slurry is then dried in an oven at 80℃ for 12 hours. After drying, the slurry is pulverized and passed through a 100-mesh sieve to obtain a clarifying agent.

[0019] 2. Preparation method of glass-ceramics S101. Mix all the raw materials for preparing the microcrystalline glass, place them in an alumina crucible, and melt them at 1650℃ for 5 h in a high-temperature furnace. The compounds for preparing the microcrystalline glass include, by weight percentage: SiO2: 48%, Al2O3: 21%, Na2O: 17%, Li2O: 2%, B2O3: 2%, ZrO2: 3%, TiO2: 0.1%, P2O5: 1%, MgO: 0.1%, SrO: 0.1%, Gd2O3: 5%, Y2O3: 0.1%, Yb2O3: 0.1%, Sm2O3: 0.1%, La2O3: 0.2%, Er2O3: 0.05%, Nd2O3: 0.05%, CeO2: 0.1%. S102. After melting is complete, reduce the temperature to 1550℃ and stir gently with a preheated quartz rod. During stirring, slowly and evenly sprinkle in 0.1% of the total mass of each component of the microcrystalline glass raw material as a clarifying agent, and evenly sprinkle it into the melt for clarification. S103. After clarification, carefully remove the crucible and quickly pour the molten glass into a large amount of cooled deionized water for rapid cooling to obtain the base glass. Place the obtained base glass in a 105°C oven to dry. After drying, grind the base glass at 600 rpm for 10 min using a high-speed disperser and pass it through a 200-mesh sieve to obtain base glass powder. S104, preheat the mold to 580℃, load the base glass powder into the mold, and press form at a pressure of 15 MPa to obtain a glass blank, and then sequentially perform twice nucleation and once crystallization on the glass blank: the first nucleation temperature is 560℃, and the holding time is 3 h; then heat to 640℃ at a rate of 10℃ / min for the second nucleation, and the holding time is 3 h; then heat to 800℃ at the same rate for crystallization, and the crystallization time is 2 h; after the completion of crystallization, cool to room temperature in the furnace to obtain the glass-ceramic.

[0020] Example 2 1. Preparation of clarifying agent S201, weigh 49 g of zirconium oxide and dry in a drying oven at 120℃ for 2 h, then transfer to a desiccator and cool to room temperature to obtain dried zirconium oxide; S202, add 392 mL of anhydrous ethanol and 98 mL of deionized water to a reaction bottle, then add 1.47 g of polyvinylpyrrolidone, stir at a speed of 80 rpm to dissolve, then add the dried zirconium oxide to the reaction bottle, and stir at a speed of 80 rpm to dissolve, then ultrasonic at 300 w for 12 min to obtain a zirconium oxide suspension; S203, add 127.5 mL of deionized water to a 500 mL beaker, then add 9 g of lithium nitrate, 22 g of lanthanum nitrate hexahydrate, and 20 g of cerium nitrate hexahydrate to the beaker, heat to 40℃ and stir at a speed of 80 rpm to dissolve, then slowly add 127.5 mL of anhydrous ethanol solution, and add an appropriate amount of acetic acid to adjust the pH of the solution to 4.0 to obtain a shell precursor solution; S204, slowly add the shell precursor solution to the zirconium oxide suspension through a buret, stirring at a speed of 300 rpm while adding, and the dropwise addition time is 50 min; continue stirring at a speed of 300 rpm for 1.5 h after the dropwise addition is completed; then concentrate and remove the solvent under reduced pressure in a rotary evaporator at a speed of 180 rpm and a temperature of 60℃, recover the solid and wash with deionized water, suction filter, and dry in a 80℃ drying oven to constant weight to obtain a dry powder; S205, place the above dry powder in a porcelain boat, and program the temperature in a muffle furnace: first heat to 200℃ and hold for 1.5 h, then heat to 400℃ at a rate of 5℃ / min and hold for 1.5 h; continue to heat to 800℃ at a rate of 5℃ / min and hold for 1.5 h, then cool to room temperature to obtain the calcined product; add the calcined product to anhydrous ethanol at a solid-liquid ratio of 1:2.5, place in a planetary ball mill, use zirconium oxide balls as grinding medium, rotate at a speed of 300 rpm, ball-to-material ratio of 5:1, and ball mill for 4.5 h to obtain a slurry, dry in a 80℃ oven for 12 h, crush after drying to pass through a 100 mesh sieve to obtain the clarifying agent.

[0021] 2. The method for preparing the glass-ceramics S101, mixing and uniformly blending each component raw material for preparing the glass-ceramics, loading into an alumina crucible, and placing in a high-temperature furnace to melt at 1600°C for 4 h, wherein the compounds for preparing the glass-ceramics include SiO2: 38%, Al2O3: 20%, Na2O: 16%, Li2O: 1%, B2O3: 7%, ZrO2: 6%, TiO2: 0.2%, P2O5: 0.5%, MgO: 2%, SrO: 0.5%, Gd2O3: 1.3%, Y2O3: 0.5%, Yb2O3: 1%, Sm2O3: 1%, La2O3: 3%, Er2O3: 0.5%, Nd2O3: 0.5%, and CeO2: 1% by weight percentage; S102, after the melting is completed, reducing the temperature to 1500°C, gently stirring with a preheated quartz rod, and slowly and uniformly sprinkling 0.5% of a clarifying agent with respect to the total mass of each component raw material for preparing the glass-ceramics in the melting process to uniformly sprinkle into the melt for clarification; S103, after the clarification is completed, carefully taking out the crucible, rapidly pouring the molten glass into a large amount of cooled deionized water for rapid cooling to obtain a base glass; drying the obtained base glass in a 105°C oven, grinding the dried base glass by a high-speed dispersion machine at a speed of 400 rpm for 20 min, and passing through a 200-mesh sieve to obtain a base glass powder; S104, preheating a mold to 560°C, loading the base glass powder into the mold, and pressing and forming into a glass blank at a pressure of 15 MPa, and then sequentially performing nucleation twice and crystallization once on the glass blank: the first nucleation temperature is 520°C, and the nucleation is maintained for 2.5 h; then the temperature is increased to 620°C at a rate of 10°C / min for the second nucleation, and the nucleation is maintained for 2.5 h; and then the temperature is increased to 700°C at the same rate for crystallization, and the crystallization time is 1.5 h, and after the crystallization is completed, the furnace is cooled to room temperature to obtain the glass-ceramics.

[0022] Example 3 1. Preparation of the clarifying agent S201, weighing 40 g of zirconium oxide, drying in a 120°C drying box for 2 h, then transferring to a desiccator to cool to room temperature to obtain dried zirconium oxide; S202, adding 333 mL of anhydrous ethanol and 67 mL of deionized water into a reaction bottle, then adding 0.4 g of polyvinylpyrrolidone, stirring at a speed of 80 rpm to dissolve, then adding the dried zirconium oxide into the reaction bottle, and stirring at a speed of 80 rpm to dissolve, and then ultrasonicating at a power of 300 w for 10 min to obtain a zirconium oxide suspension; S203, add 150 mL of deionized water in a 500 mL beaker, add 18 g of lithium nitrate, 20 g of lanthanum nitrate hexahydrate and 22 g of cerium nitrate hexahydrate to it, heat to 40℃ and stir at a speed of 80 rpm to dissolve, then slowly add 150 mL of anhydrous ethanol solution, and adjust the pH of the solution to 4.5 with appropriate amount of acetic acid to obtain a shell precursor solution; S204, slowly add the shell precursor solution to the zirconium oxide suspension through a burette, stirring at a speed of 300 rpm while adding, the dropping time is 45 min; continue stirring at a speed of 300 rpm for 1 h after the addition is completed; then concentrate and remove the solvent in a rotary evaporator at a speed of 180 rpm and a temperature of 60℃ under reduced pressure, recover the solid and wash it with deionized water, filter and dry in a 80℃ drying oven until constant weight to obtain a dry powder; S205, place the above dry powder in a porcelain boat and program the temperature in a muffle furnace, first heat to 200℃ and keep for 1 h, then heat to 350℃ at a rate of 5℃ / min and keep for 1 h; continue to heat to 750℃ at a rate of 5℃ / min and keep for 1 h, then cool to room temperature to obtain the calcined product; add the calcined product to anhydrous ethanol at a solid-liquid ratio of 1:2.5, place it in a planetary ball mill, use zirconia balls as grinding medium, rotate at a speed of 300 rpm, ball-to-material ratio is 5:1, ball mill for 4 h, obtain a slurry, dry in a 80℃ oven for 12 h, crush through a 100 mesh sieve after drying to obtain a clarifying agent.

[0023] 2. Method for preparing microcrystalline glass S101, mix the raw materials for preparing microcrystalline glass, load into an alumina crucible and place in a high-temperature furnace, melt at 1550℃ for 3 h, wherein the compounds for preparing microcrystalline glass include SiO2: 39%, Al2O3: 25%, Na2O: 21%, Li2O: 1.5%, B2O3: 2.2%, ZrO2: 2%, TiO2: 1%, P2O5: 4%, MgO: 0.1%, SrO: 0.5%, Gd2O3: 0.5%, Y2O3: 1%, Yb2O3: 0.5%, Sm2O3: 1%, La2O3: 0.1%, Er2O3: 0.25%, Nd2O3: 0.25%, CeO2: 0.1% by weight percentage; S102, after the melting is completed, reduce the temperature to 1450℃, gently stir with a preheated quartz rod, slowly and evenly sprinkle 0.8% of the clarifying agent with respect to the total mass of the raw materials for preparing microcrystalline glass into the melt to clarify; S103, After the clarification is completed, the crucible is carefully removed, and the molten glass is quickly poured into a large amount of cooled deionized water for rapid cooling to obtain a base glass; the obtained base glass is placed in a 105°C oven for drying, and the dried base glass is ground by a high-speed dispersion machine at a speed of 200 rpm for 30 min, and then passed through a 200-mesh sieve to obtain a base glass powder; S104, The mold is preheated to 550°C, the base glass powder is loaded into the mold, and is pressed into a glass blank at a pressure of 15 MPa, and then the glass blank is sequentially subjected to two nucleation and one crystallization treatments: the first nucleation temperature is 500°C, and the holding time is 2 h; then the temperature is increased to 600°C at a rate of 10°C / min for the second nucleation, and the holding time is 2 h; and then the temperature is increased to 650°C at the same rate for crystallization, and the crystallization time is 1 h, and after the crystallization is completed, the furnace is cooled to room temperature to obtain a glass-ceramic.

[0024] Comparative Example 1 The difference from Example 1 is that the preparation process of the fining agent does not contain lithium nitrate, and the rest is the same.

[0025] Comparative Example 2 The difference from Example 1 is that the preparation process of the fining agent does not contain lanthanum nitrate hexahydrate, and the rest is the same.

[0026] Comparative Example 3 The difference from Example 1 is that the preparation process of the fining agent does not contain cerium nitrate hexahydrate, and the rest is the same.

[0027] Comparative Example 4 The difference from Example 1 is that an equal amount of antimony trioxide is used to replace the fining agent prepared in Example 1, and the rest of the conditions remain unchanged.

[0028] Performance Test The glass-ceramics prepared in the examples and comparative examples are respectively subjected to performance tests, including bubble density and transmittance.

[0029] Table 1 Performance test results of the glass-ceramics prepared in the examples and comparative examples

[0030] The results are shown in Table 1, the bubble density of the glass-ceramics prepared in Examples 1-3 is significantly lower than that of each of the comparative examples, which shows that the clarifying agent prepared in the present application has a significant effect on promoting the bubble floating and discharging; secondly, the transmittance of the glass-ceramics prepared in Examples 1-3 is significantly higher than that of each of the comparative examples, the reason for the increase of the transmittance is the reduction of scattering caused by the reduction of the bubble density, the components of the clarifying agent improve the uniformity of the glass network structure, so that the light propagation is more smooth. In contrast, the comparative examples have a higher bubble content, and there may be some residual reducing impurities, which leads to a decrease in light transmission performance.

[0031] The above description is merely preferred embodiments of the present application, but not to limit the present application, any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing high-performance glass-ceramics, characterized in that, Includes the following steps: S101. Mix the raw materials of each component for preparing microcrystalline glass, put them into an alumina crucible, place them in a high-temperature furnace, and melt them at 1550-1650℃ for 3-5 hours. S102. After melting is complete, reduce the temperature to 1450-1550℃ and add 0.1%-0.8% of clarifying agent by weight of the total raw materials of the microcrystalline glass components for clarification. S103. After clarification, remove the crucible and quickly pour it into deionized water for rapid cooling. Then, dry, grind and sieve to obtain basic glass powder. S104. Preheat the mold to 550-580℃, and put the basic glass powder into the mold for pressing. Then, perform two nucleation processes and one crystallization process to obtain the high-performance microcrystalline glass. The clarifying agent comprises zirconium oxide, lithium nitrate, lanthanum nitrate hexahydrate, and cerium nitrate hexahydrate; The method for preparing the clarifying agent includes the following steps: S201. Weigh 40-70 parts of zirconium oxide according to the weight ratio, dry it, and obtain dried zirconium oxide; S202. Add dried zirconium oxide to the reaction flask, add a mixed solution of anhydrous ethanol and deionized water to the reaction flask at a solid-liquid ratio of 1:10, then add polyvinylpyrrolidone, stir and sonicate to obtain a zirconium oxide suspension, wherein the mass ratio of zirconium oxide to polyvinylpyrrolidone is 100:(1-5). S203. Weigh 5-18 parts by weight of lithium nitrate, 15-22 parts by weight of lanthanum nitrate hexahydrate and 10-22 parts by weight of cerium nitrate hexahydrate into a reaction vessel. Add deionized water and anhydrous ethanol respectively according to a solid-liquid ratio of 1:2.

5. Stir and adjust the pH to 3.5-4.5 to obtain a shell precursor solution. S204. The shell precursor solution is added dropwise to the zirconium oxide suspension while stirring at 300 rpm for 45-60 min. After the addition is complete, stirring at 300 rpm is continued for 1-2 h. Then, the solvent is removed by vacuum concentration, the solid is recovered and washed with deionized water, filtered, and dried to obtain a dry powder. S205. The dried powder is calcined in stages by heating, and anhydrous ethanol is added to the calcined product at a solid-liquid ratio of 1:2.

5. The product is then ball-milled to obtain the clarifying agent.

2. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, The raw materials used in step S101 to prepare the microcrystalline glass include, by weight percentage: SiO2: 38-48%, Al2O3: 20-25%, Na2O: 16-21%, Li2O: 1-4%, B2O3: 2-7%, ZrO2: 3-6%, TiO2: 0.1-1%, P2O5: 0.5-4%, MgO: 0.1-2%, SrO: 0.1-4%, Gd2O3: 0.5-5%, Y2O3: 0.1-1%, Yb2O3: 0.1-1%, Sm2O3: 0.1-1%, La2O3: 0.1-3%, Er2O3: 0.05-0.5%, Nd2O3: 0.05-1%, CeO2: 0.1-1%.

3. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, In step S103, the product is dried at 105°C, ground at 200-600 rpm for 10-30 min, and then passed through a 200-mesh sieve.

4. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, The pressing condition in step S104 is 15 MPa pressure molding.

5. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, The nucleation conditions in step S104 are as follows: the first nucleation temperature is 500-560℃, and the holding time is 2-3 h; the second nucleation temperature is 600-640℃, and the holding time is 2-3 h; the crystallization conditions are as follows: the crystallization temperature is 650-800℃, and the crystallization time is 1-2 h.

6. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, In step S202, the volume ratio of anhydrous ethanol to deionized water in the mixed solution is 1:(3-5).

7. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, The segmented heating and calcination conditions in step S205 are as follows: first, the temperature is raised to 200℃ and held for 1-2 hours; then, the temperature is raised to 350-450℃ at a rate of 5℃ / min and held for 1-2 hours; then, the temperature is raised to 750-820℃ at a rate of 5℃ / min and held for 1-2 hours.

8. The method for preparing a high-performance microcrystalline glass according to claim 1, characterized in that, In step S205, the ball milling conditions are as follows: zirconium oxide balls are used as the grinding medium, the rotation speed is 300 rpm, the ball-to-material ratio is 5:1, and the ball milling time is 4-5 h.

9. A high-performance microcrystalline glass, characterized in that, The high-performance microcrystalline glass is prepared according to the preparation method described in any one of claims 1-8.

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