CN112047638A - Glass and preparation method and application thereof - Google Patents
Glass and preparation method and application thereof Download PDFInfo
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- CN112047638A CN112047638A CN202010887293.5A CN202010887293A CN112047638A CN 112047638 A CN112047638 A CN 112047638A CN 202010887293 A CN202010887293 A CN 202010887293A CN 112047638 A CN112047638 A CN 112047638A
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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
- C03C12/00—Powdered glass; Bead compositions
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
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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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
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Abstract
The invention relates to the technical field of glass production, in particular to glass and a preparation method and application thereof. The glass comprises the following components in percentage by weight: 20-50% of CaO, 10-40% of MgO and SiO210％‑40％、B2O31％‑30％、ZrO20‑5％、Al2O30‑5％、La2O30 to 5 percent. The proportion of each component is adjusted, the proportion of a glass phase and a ceramic phase is adjusted, the thermal expansion coefficient of the glass is improved, the thermal expansion coefficient of the glass is determined to be 10.95-11.65 ppm/DEG C through experiments, the thermal expansion coefficient is larger, the thermal expansion coefficient is matched with the thermal expansion coefficient of stainless steel which is a common material of a connector of a solid oxide fuel cell, and the risk of cell leakage caused by mismatch of the thermal expansion coefficients of the glass and the ceramic phase can be reduced.
Description
Technical Field
The invention relates to the technical field of glass production, in particular to glass and a preparation method and application thereof.
Background
In the use process of a Solid Oxide Fuel Cell (SOFC), the cell operating temperature changes greatly, and the coefficient of thermal expansion of the conventional sealing glass is small, so that the coefficient of thermal expansion between the sealing glass and the cell connecting body is likely to be mismatched, and leakage is likely to occur. In the SOFC, a glaze glass layer is generally arranged between the sealing glass and the cell connector to protect the metal substrate of the connector, improve the oxidation resistance of the connector, and improve the bonding force between the sealing glass and the connector. Because the glaze layer glass and the sealing glass are different in types, a relatively obvious two-phase interface can be generated in the preparation process, so that the sealing strength is reduced, the permeation of different elements can be generated, and the stability of the sealing glass is reduced.
Japanese Kokai publication No. CN103987673B discloses that a sealing glass having a high expansion coefficient can be obtained by adjusting the type of crystallization to obtain 2 MgO. SiO2、BaO·2MgO·2SiO2And 2SiO21 or more kinds of crystals of 2 ZnO. BaO; the patent CN 102190440B of Schottky public corporation obtains sealing glass with high expansion coefficient by mixing the types of additives; SiO was prepared by Japanese Shanmura Nitri Kabushiki Kaisha patent CN101801873B2-B2O3-CaO-MgO-ZrO2Sealing glass of the system.
Although the formulations mentioned in the prior patents allow to obtain sealing glasses with high expansion coefficients, they still have the following drawbacks: (1) the type of crystallization cannot be controlled, although a plurality of crystal phases with high expansion coefficients can be obtained, the expansion coefficients of the crystal phases cannot be controlled within a narrow range, and the situation that the thermal expansion coefficients of the sealing glass, the connector and the glaze layer glass are not matched easily occurs; (2) the ratio of the glass phase and the ceramic phase cannot be controlled by the glass formula, the glass phase has the functions of reducing porosity and increasing toughness, but the expansion coefficient is low, the ceramic phase has high expansion coefficient but insufficient toughness, and if the ratio of the glass phase to the ceramic phase cannot be controlled well, the loss of one property occurs. If the proportion of the glass phase is too high, on one hand, the thermal expansion coefficient is reduced, the requirement of high expansion coefficient cannot be met, and the mismatch of the thermal expansion coefficients among the sealing glass, the connecting body and the glaze layer glass is caused, on the other hand, the glass phase is changed to the ceramic phase along with the operation of the galvanic pile in a large proportion, the change is accompanied with volume shrinkage, the shrinkage causes internal defects, the strength of the sealing glass is reduced, and the leakage is easily caused; compared with a glass phase, the ceramic phase has poor toughness and poor thermal shock resistance, the galvanic pile needs to operate at high temperature, and can generate large thermal shock when operating at low temperature to high temperature, and if the proportion of the ceramic phase is too high, the stress can not be quickly released, so that large compressive stress can be generated inside, the inside is cracked, and leakage occurs.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide glass and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: providing glass, wherein the glass comprises the following components in percentage by weight: 20-50% of CaO, 10-40% of MgO and SiO2 10％-40％、B2O31％-30％、ZrO2 0-5％、Al2O3 0-5％、La2O3 0-5％。
Na and K do not need to be added into the glass, and MgO and CaO are not easy to volatilize at high temperature, so that the instability of the performance of the glass caused by the volatilization of Na and K at high temperature can be avoided, the chemical stability of the glass is better, and the attenuation of the electrochemical performance of a battery caused by the instability of the performance of the glass is avoided; the glass of the invention does not need to be added with Ba element, thereby avoiding the condition of high temperatureBa in the glass reacts with Cr in the connector and the cover plate to generate BaCrO with very high thermal expansion coefficient4Resulting in leakage of the battery.
In the glass, the addition of CaO improves the expansion coefficient of the devitrified ceramic phase, and is beneficial to being matched with a connector with higher expansion coefficient; MgO is formed into CaO-MgO-SiO2-B2O3The essential components of the crystal are beneficial to improving the heat-resistant stability of the glass; SiO 22The method is very important for the melting of the glass, and the addition of the method can reduce the melting temperature of the glass and is also beneficial to improving the porosity of the glass; b is2O3Is necessary for melting glass, and the addition of the glass can improve the fluidity of the glass during melting and improve the leveling property in the sealing process.
In the glass, the mass percent of CaO is 20-50%, the crystallization amount of the glass is low due to the excessively low addition amount of CaO, the glass phases are increased, the glass crystallization conversion can occur in the use process of a galvanic pile, so that the stability of the glass is poor, the crystallization temperature can be increased due to the excessively high addition amount of CaO, and other components can be damaged due to high-temperature crystallization;
the weight percentage of MgO is 10-40%, and CaO-MgO-SiO can not be precipitated when the addition amount of MgO is too low2-B2O3The crystal (b) has a low expansion coefficient, cannot be matched with a connector, an electrolyte, a cathode and an anode, and is added in an excessively high amount, so that the water resistance of the precipitated crystal is poor, and leakage occurs after long-term use;
SiO210 to 40 percent of SiO2The addition amount is too low, so that the melting temperature of the glass is increased, the melting is difficult, more air holes are formed in the glass in use, the sealing strength is reduced, and SiO2Too high an amount of addition makes crystallization difficult;
B2O31-30% by mass of B2O3Too low an amount of addition makes the glass insufficiently fluid at the time of sealing and difficult to compress, B2O3The addition amount is too high, a large amount of volatilization can occur when the galvanic pile is in operation, B2O3Belongs to a network former and is stableOne of the main components of the glass is determined, if excessive volatilization causes the network structure inside the glass to be damaged, so that defects appear inside the glass, and the defects can cause the leakage of the galvanic pile;
ZrO20-5% by mass of ZrO2Too high an amount of addition causes the glass to precipitate other crystalline phase substances such as CaZrO3，MgZrO3The sealing effect of the glass is deteriorated;
Al2O30-5% by mass of Al2O3Too high an amount of addition can cause the viscosity of the glass to be too high, resulting in poor leveling property;
La2O30-5% of La2O3Too high an amount of addition increases the devitrified phase, makes the glass brittle and deteriorates the impact resistance.
As a preferred embodiment of the glass of the present invention, the glass comprises the following components in percentage by weight: 30-40% of CaO, 20-30% of MgO and SiO 2 20％-30％、B2O3 10％-20％、ZrO2 0.5-2％、Al2O3 0.5-2％、La2O3 0.5-2％。
By optimizing the glass formulation, Ca can be generated in use2Si，Ca2MgO7Si2，CaSi2O5，Mg2B2O5，MgSiO3CaO-MgO-SiO of2-B2O3The crystallization phase has high expansion coefficient and stable expansion coefficient, and can meet the sealing requirement of glass.
Component Al2O3The adhesion between the glass and the connector is improved, and the binding force between the glass and the base material is improved; la2O3The method is used for adjusting the proportion between the crystallization phase and the glass phase, and can improve the stability of the glass ceramics; the glass system belongs to alkali metal glass system, SiO2The network connection structure of the glass is [ SiO ]4]Silicon-oxygen tetrahedron as principal component (also [ BO ]3]Boron oxygen trigones), degree of network connectivity (mainly [ SiO ]4]Silicon oxygen fourHas a large influence on devitrification of glass, and the addition of alkali metal promotes such structural destruction to cause crystallization, and La is added2O3The oxide serving as the network external plasma can reconnect the network connector, so that the crystallization amount is reduced, and the adjustment effect is achieved; ZrO (ZrO)2The crystallization can be easily caused, the moisture resistance of the glass can be improved, and the sealing strength of the cured glass can be improved.
The invention provides a preparation method of the glass, which comprises the following steps: the components are uniformly mixed, heated and melted, and subjected to water quenching after heat preservation until the components are clear and have no bubbles, and the components are obtained after crushing and grinding.
As a preferred embodiment of the preparation method of the invention, the temperature of the heating and melting is 1000-1600 ℃.
As a preferred embodiment of the preparation method of the present invention, the time for the heat-retention is 0.5 to 4 hours.
The invention provides application of the glass in preparing sealing glass or glaze layer glass.
The invention provides application of the glass in preparing a solid oxide fuel cell.
The invention also provides a solid oxide fuel cell, which contains the glass.
The invention has the beneficial effects that:
(1) the glass does not introduce volatile alkali metal elements (Na and K) and Ba which can react with Cr in stainless steel, so that the chemical stability and the structural stability of the glass are ensured, and simultaneously, the reduction of glass phase content caused by crystallization can be reduced or avoided in the process of operating solid oxide fuel;
(2) the proportion of each component is adjusted, the proportion of a glass phase and a ceramic phase is also adjusted, the thermal expansion coefficient of the glass is improved, the thermal expansion coefficient of the glass is determined to be 10.95-11.65 ppm/DEG C through experiments, the thermal expansion coefficient is larger, the thermal expansion coefficient is matched with the thermal expansion coefficient of stainless steel which is a common material of a connector of a solid oxide fuel cell, and the risk of cell fever and leakage caused by mismatch of the thermal expansion coefficients of the glass and the ceramic phase can be reduced;
(3) the glass has a wider sintering window, can be used as sealing glass and glaze layer glass on a connector, ensures that crystal phases and contents precipitated by high-temperature firing of the glaze layer glass and low-temperature firing of the sealing glass are basically consistent, does not generate an obvious two-phase interface, improves the sealing strength, does not generate permeation of different elements, and improves the stability of the sealing glass.
Drawings
FIG. 1 is a graph showing the crystal form precipitation and the strength change of the glass of the present invention before and after operation.
FIG. 2 is a graph showing the change in porosity after 6h and 5318h of run of the glass of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples. This should not be understood as limiting the scope of the above-described subject matter of the present invention to the following examples. All the technologies realized based on the above contents of the present invention belong to the scope of the present invention.
Example 1
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 40%, MgO 20%, SiO 2 20％、B2O3 10％、ZrO2 3％、Al2O3 5％、La2O3 2％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1250 ℃, and then heat-preserved for 0.5 hour to ensure complete clarification and no air bubbles, and then directly quenched by water, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 1 μm).
When the glass of the present embodiment is used as a sealing glass: and (3) performing heat treatment on the glass powder for 1 hour at the high temperature of 700 ℃ during sealing to crystallize the glass powder.
When the glass of the present example is used as an enamel layer glass: when the glass powder is used as a glaze layer, the glass powder is subjected to heat treatment at the high temperature of 800 ℃ for 3 hours to crystallize the glass powder.
Example 2
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 30%, MgO 25%, SiO2 25％、B2O3 15％、ZrO2 1.5％、Al2O3 1.5％、La2O3 2％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1000 ℃, and then heat-preserved for 1.0 hour, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 30 μm).
When the glass of the present embodiment is used as a sealing glass: and (3) performing high-temperature heat treatment on the glass powder at 800 ℃ for 10 hours during sealing to crystallize the glass.
When the glass of the present example is used as an enamel layer glass: when the glass powder is used as a glaze layer, the glass powder is thermally treated at 870 ℃ for 15 hours to crystallize.
Example 3
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 50%, MgO 10%, SiO 2 20％、B2O3 10％、ZrO2 5％、Al2O3 5％、La2O3 0％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1300 ℃, and then heat-preserved for 2.0 hours, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 10 μm).
Example 4
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: 20% of CaO, 35% of MgO and SiO2 10％、B2O3 30％、ZrO2 0％、Al2O3 0％、La2O3 5％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1350 ℃, and then heat-preserved for 1.5 hours, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 50 μm).
Example 5
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 30%, MgO 27%, SiO 2 20％、B2O3 20％、ZrO2 1％、Al2O3 1％、La2O3 1％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1350 ℃, and then heat-preserved for 1.5 hours, after the complete clarification and no air bubbles are ensured, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 15 μm).
Example 6
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 32%, MgO 25%, SiO2 25％、B2O3 12％、ZrO2 2％、Al2O3 2％、La2O3 2％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1400 ℃, and then heat-preserved for 3.0 hours, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 18 μm).
Example 7
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 22%, MgO 40%, SiO2 28％、B2O3 1％、ZrO2 3％、Al2O3 3％、La2O3 3％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1500 ℃, and then heat-preserved for 3.5 hours, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 20 μm).
Example 8
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 26%, MgO 21%, SiO2 40％、B2O3 10％、ZrO2 1％、Al2O3 1％、La2O3 1％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1400 ℃, and then heat-preserved for 3.0 hours, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 8 μm).
Example 9
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 40%, MgO 20%, SiO228％、B2O3 10％、ZrO2 0.5％、Al2O3 0.5％、La2O3 1％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1450 ℃, and then heat-preserved for 1.0 hour, after ensuring complete clarification and no air bubbles, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 5 μm).
Example 10
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 30%, MgO 30%, SiO2 28％、B2O3 10％、ZrO2 1％、Al2O3 0.5％、La2O3 0.5％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1150 ℃, and then heat-preserved for 1.3 hours, and after completely clarifying and bubble-free, the glass is directly water-quenched, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 15 μm).
Example 11
The glass provided by the embodiment of the invention comprises the following components in percentage by weight: CaO 30%, MgO 27%, SiO 2 30％、B2O3 10％、ZrO2 1％、Al2O3 1％、La2O3 1％。
The preparation method of the glass of the embodiment specifically comprises the following steps:
the components of the glass of the embodiment are uniformly mixed, heated and melted at 1150 ℃, and then kept warm for 2 hours, after ensuring complete clarification and no air bubbles, the glass is directly quenched by water, crushed and ground to obtain the glass (also called glass powder, the granularity of the glass powder is controlled at 15 μm).
Test example 1 glass Performance data testing
The sealing glasses prepared in examples 1 to 11 were subjected to a Coefficient of Thermal Expansion (CTE) test after glass devitrification, specifically including the following steps:
0.1 to 3g of sealing glass was weighed, pressed into a block, calcined at 650 to 900 ℃ for 1 to 60 minutes, the sintered body obtained by sintering the glass powder was cut into about 5X 7.5mm, polished on the upper and lower surfaces, and heated from room temperature to 900 ℃ at a rate of 10 ℃/min using a TMA thermomechanical tester, and the thermal expansion coefficients (. alpha.1) based on the two points of 25 ℃ and 850 ℃ and (. alpha.2) based on the two points of 30 ℃ and 650 ℃ were calculated from the thermal expansion curves obtained therefrom, and the data are shown in Table 1.
TABLE 1 coefficient of thermal expansion of sealing glass
| Examples | 25℃-850℃(CTE ppm/℃) | 30℃-650℃(CTE ppm/℃) |
| Example 1 | 10.89 | 10.77 |
| Example 2 | 10.58 | 10.25 |
| Example 3 | 11.44 | 11.12 |
| Example 4 | 11.77 | 11.42 |
| Example 5 | 11.66 | 11.35 |
| Example 6 | 11.85 | 11.64 |
| Example 7 | 11.88 | 11.73 |
| Example 8 | 10.53 | 10.42 |
| Example 9 | 11.12 | 11.01 |
| Example 10 | 11.52 | 11.32 |
| Example 11 | 11.65 | 11.43 |
As can be seen from table 1: the sealing glass prepared by the invention has the thermal expansion coefficient of 10.95-11.65 ppm/DEG C, and the thermal expansion coefficient is larger; the thermal expansion coefficient of the stainless steel which is a common material of the connector of the solid oxide fuel cell is 10.88-11.45 ppm/DEG C, and the thermal expansion coefficient is matched with that of the connector, so that the risk of the cell fever and leakage caused by the mismatch of the thermal expansion coefficients of the two can be reduced.
Test example 2 test of operation of sealing glass
The sealing glass prepared by the invention operates for 5000 hours at the temperature of 850 ℃, and the thermal expansion coefficient is 10.95-11.65 ppm/DEG C and is not changed, which shows that the sealing glass prepared by the invention has stable thermal expansion coefficient when operating at high temperature for a long time.
And the crystal phase and the porosity of the sealing glass in the glass do not change after the glass runs at high temperature for a long time, as shown in figure 1, the crystal form and the strength precipitated before and after the glass runs do not change, as shown in figure 2, the porosity is kept at 11.52 percent from the original 11.5 percent after the glass runs for 5318 hours, and the porosity is basically unchanged, so that the stable and reliable running of the battery is ensured.
The sealing glass and the glaze layer glass can adopt the same glass type, so that the compatibility is increased, and the complex reaction between different glasses is avoided.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The glass is characterized by comprising the following components in percentage by weight: 20-50% of CaO, 10-40% of MgO and SiO2 10％-40％、B2O3 1％-30％、ZrO2 0-5％、Al2O30-5％、La2O3 0-5％。
2. The glass according to claim 1, comprising the following components in percentage by weight: 30-40% of CaO, 20-30% of MgO and SiO2 20％-30％、B2O3 10％-20％、ZrO2 0.5-2％、Al2O3 0.5-2％、La2O3 0.5-2％。
3. A method for producing a glass according to any one of claims 1-2, characterized in that the method comprises the steps of: the components are uniformly mixed, heated and melted, and subjected to water quenching after heat preservation until the components are clear and have no bubbles, and the components are obtained after crushing and grinding.
4. The method as claimed in claim 3, wherein the temperature for melting by heating is 1000-1600 ℃.
5. The method of claim 3, wherein the incubation time is 0.5 to 4 hours.
6. Use of a glass according to any of claims 1-2 for the production of sealing glass or glazing.
7. Use of a glass according to any one of claims 1 to 2 in the manufacture of a solid oxide fuel cell.
8. A solid oxide fuel cell comprising the glass of any one of claims 1-2.
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| CN116119934A (en) * | 2023-02-22 | 2023-05-16 | 江苏虹普电子材料科技有限公司 | NTC thermistor coated glass powder and preparation method thereof |
| CN116813202A (en) * | 2023-06-16 | 2023-09-29 | 潮州三环（集团）股份有限公司 | Microcrystalline glass material and preparation method and application thereof |
| CN116813202B (en) * | 2023-06-16 | 2024-03-19 | 潮州三环（集团）股份有限公司 | Microcrystalline glass material and preparation method and application thereof |
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