CN110451806B - Uniform crystallization control method of glass ceramic - Google Patents
Uniform crystallization control method of glass ceramic Download PDFInfo
- Publication number
- CN110451806B CN110451806B CN201910821009.1A CN201910821009A CN110451806B CN 110451806 B CN110451806 B CN 110451806B CN 201910821009 A CN201910821009 A CN 201910821009A CN 110451806 B CN110451806 B CN 110451806B
- Authority
- CN
- China
- Prior art keywords
- glass ceramic
- parts
- stage
- temperature
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
Abstract
The invention relates to a uniform crystallization control method of glass ceramic, which comprises the following steps: high-purity zirconia with the grain diameter less than or equal to 100nm is added into the glass ceramic raw material. According to the uniform crystallization control method of the glass ceramic, the high-purity zirconia is adopted, the original particle size is controlled, the zirconia is easily dispersed in a glass melt, the glass is uniformly melted, and the overall performance of the material is improved through uniform crystallization; meanwhile, the original grain size of the high-purity zirconia is controlled, so that the size of the material crystal nucleus is controlled, and the material crystal nucleus can be uniformly nucleated in a controllable range.
Description
Technical Field
The invention relates to the technical field of glass ceramics, in particular to a uniform crystallization control method of glass ceramics.
Background
The glass ceramic is also called as microcrystalline glass, is a composite material which is prepared by high-temperature melting, molding and heat treatment and combines a crystal phase with glass, and has the advantages of high mechanical strength, adjustable thermal expansion performance, thermal shock resistance, chemical corrosion resistance, low dielectric loss and the like. Glass ceramics are widely used in the fields of mechanical manufacturing, optics, electronics and microelectronics, aerospace, chemistry, industry, biomedicine, architecture and the like.
The manufacturing process of the glass ceramic is complex and has high technical requirements. The research on the glass ceramic material avoids researching the control of the crystallization process of the glass ceramic material. The good crystallization method and the process can effectively improve the conversion efficiency of the crystal so as to enhance the mechanical property of the material and the overall uniformity of the material, and the most studied method at present is a heterogeneous nucleation method for controlling the crystallization of the material, namely adding a nucleating agent into the base glass. The commonly used nucleating agents comprise noble metal colloid nucleating agents (gold, silver, platinum, copper and the like), the nucleating agents are expensive, part of metal colloid ions are seriously colored, the final color of the material is greatly influenced and is difficult to control, and the nucleating agents are not suitable for large-batch industrial production. In order to control the cost and reduce the influence of the color of the colloid ions, the research on the crystal nucleating agent suitable for mass production has great practical significance.
The nucleating agent commonly used in industrial production is an oxide nucleating agent such as zirconia, which has the advantages of low price, wide application, basically no change of material color, skillful controllable method and high controllability, is extremely suitable for modern industrial production, and can basically replace a noble metal colloid nucleating agent. However, the zirconia has physical characteristics and related preparation processes, which cause difficulty in founding the basic glass and uneven texture, thus causing uneven crystallization and seriously affecting the overall performance of the glass ceramic.
Disclosure of Invention
The invention aims to provide a uniform crystallization control method of glass ceramic, which solves the problem of poor overall performance of the glass ceramic caused by nonuniform crystallization in the preparation process of the glass ceramic in the prior art.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for controlling uniform crystallization of glass ceramic, comprising: high-purity zirconia with the grain diameter less than or equal to 100nm is added into the glass ceramic raw material.
In the uniform crystallization control method of glass ceramics of the present invention, the average particle size of the high-purity zirconia is 40 to 60 nm; the purity of the high-purity zirconia is more than or equal to 99.9 percent.
In the uniform crystallization control method of the glass ceramic, the raw materials of the glass ceramic comprise the following components in parts by mass: 30-80 parts of SiO220-45 parts of Li2CO31-15 parts of alkali metal salt, 1-10 parts of Al (OH)3And 0-10 parts of rare earth oxide, and 1-10 parts of high-purity zirconia is added at the same time.
In the method for controlling uniform crystallization of a glass ceramic of the present invention, the high-purity zirconia, SiO2、Li2CO3Alkali metal salt, Al (OH)3And the rare earth oxide comprises the following components in parts by weight: 1-5 parts of high-purity zirconia and 48-60 parts of SiO228-32 parts of Li2CO34.8-8 parts ofAlkali metal salt of (2-5 parts of Al (OH)3And 0-10 parts of rare earth oxide.
In the method for controlling uniform crystallization of a glass ceramic according to the present invention, the method for controlling uniform crystallization of a glass ceramic further comprises: uniformly mixing a glass ceramic raw material and high-purity zirconia, settling and drying the mixture until the mixture is hardened and agglomerated, carrying out boiling melting on the dried material, placing the liquid material subjected to boiling melting in a forming die to form a sample block, and then carrying out heat treatment on the sample block to carry out nucleation and crystallization.
In the uniform crystallization control method of glass ceramic of the present invention, the heat treatment of the sample block to cause nucleation specifically comprises:
a1, nucleation stage: preserving the heat for 5-15min at the temperature of 450-;
a2, crystallization stage: heating to 600-700 ℃, and preserving the heat for 15-60min at 600-700 ℃;
a3, complete crystallization stage: heating to 820 and 880 ℃, and preserving the temperature for 10-30min at 820 and 880 ℃.
In the uniform crystallization control method of the glass ceramic, the temperature rise rate is controlled to be 50-90 ℃/min in the steps A2 and A3.
In the uniform crystallization control method of glass ceramic of the present invention, the process of boiling and melting the dried material specifically comprises:
b1, first stage: putting the settled and dried material into a melting device with the temperature of 1200-1250 ℃;
b2, second stage: heating to 1300 ℃ and 1400 ℃, and preserving the heat for 2-4h at 1300 ℃ and 1400 ℃;
b3, third stage: heating to 1500-;
b4, cooling from 1500-1600 ℃ of the third stage to 1300-1400 ℃ of the second stage; the second and third stages are repeated.
In the uniform crystallization control method of the glass ceramic, in the step B2, the temperature rise rate is controlled at 10-20 ℃/min; in the step B3, the temperature rising rate is controlled to be 20-40 ℃/min; in the step B4, the temperature reduction rate from the third stage to the second stage is controlled at 25-35 ℃/min.
In the uniform crystallization control method of the glass ceramic, the glass ceramic raw material and the high-purity zirconia are uniformly mixed by using a ball mill, and the drying temperature is controlled to be 90-100 ℃ when the glass ceramic raw material and the high-purity zirconia are settled and dried after being uniformly mixed.
The implementation of the uniform crystallization control method of the glass ceramic has the following beneficial effects: according to the uniform crystallization control method of the glass ceramic, the high-purity zirconia is adopted, the original particle size is controlled, the zirconia is easily dispersed in a glass melt, the glass is uniformly melted, and the overall performance of the material is improved through uniform crystallization; meanwhile, the original grain size of the high-purity zirconia is controlled, so that the size of the material crystal nucleus is controlled, and the material crystal nucleus can be uniformly nucleated in a controllable range.
Detailed Description
The method for controlling uniform devitrification of a glass ceramic according to the present invention will be further described with reference to the following examples:
nucleation of zirconia by precipitation of zirconium-oxygen-rich crystals from the parent phase to induce nucleation in LiO-Al2O3-SiO2In the glass ceramic system, zirconia is mainly induced to form a beta-quartz solid solution as a main crystal phase, and cubic ZrO with fine particles as a secondary crystal phase2And (3) a solid. The invention provides a uniform crystallization control method of glass ceramic by using zirconium oxide as a nucleating agent.
The uniform crystallization control method of the glass ceramic comprises the following steps:
s1, selecting high-purity zirconia, wherein the overall particle size requirement of the high-purity zirconia is less than or equal to 100nm, the average particle size is 40-60nm, the particle sizes are preferably dispersed in the range so as to form an interlocking structure, the purity of the high-purity zirconia is preferably more than or equal to 99.9%, more preferably more than or equal to 99.99%, and no other auxiliary agent is added;
s2, mixing the raw materials of the glass ceramic and the high-purity zirconia according to the mass part ratio, and performing ball milling and uniform mixing by using a ball mill, wherein the rotating speed of the ball mill is 300-;
the glass ceramic comprises the following raw materials in parts by mass: 30-80 parts of SiO220-45 parts of Li2CO31-15 parts of alkali metal salt, 1-10 parts of Al (OH)3And 0-10 parts of rare earth oxide, and 1-10 parts of high-purity zirconia is added at the same time; preferably, the high-purity zirconia, SiO2、Li2CO3Alkali metal salt, Al (OH)3And the rare earth oxide comprises the following components in parts by weight: 1-5 parts of high-purity zirconia and 48-60 parts of SiO228-32 parts of Li2CO34.8-8 parts of alkali metal salt, 2-5 parts of Al (OH)3And 0-10 parts of rare earth oxide; wherein the alkali metal salt is a salt corresponding to metal oxides of IA group and IIA group in the chemical element table, preferably, the alkali metal salt is at least one selected from potassium carbonate, sodium sulfate, magnesium carbonate and strontium carbonate; the rare earth oxide is preferably selected from at least one of cerium oxide, bismuth oxide and yttrium oxide, and is used for improving the aesthetic degree of the material, such as color and corresponding saturation;
s3, settling and drying the uniformly mixed materials, wherein the temperature during settling and drying is 90-100 ℃, and the settling and drying time is 5-10 hours until the materials are hardened and agglomerated;
s4, boiling and melting the dried material, wherein the process specifically comprises the following steps:
s41, a first stage: putting the settled and dried materials into a melting appliance with the temperature of 1200-1250 ℃, namely preheating the melting appliance to 1200-1250 ℃ in advance, and putting the settled and dried materials into the melting appliance, wherein the melting appliance can be various heat-resistant appliances including but not limited to a crucible, a smelting kiln, a smelting furnace and the like;
s42, a second stage: heating to 1300 ℃ and 1400 ℃, and preserving the heat for 2-4h at 1300 ℃ and 1400 ℃; the heating rate is controlled at 10-20 ℃/min;
s43, third stage: heating to 1500-; the temperature rising rate is controlled to be 20-40 ℃/min;
s44, cooling from 1600 ℃ at the third stage to 1400 ℃ at the second stage, wherein the cooling rate is controlled to be 25-35 ℃/min, preferably 30 ℃/min; the second stage is repeated to preserve heat for 2-4h at 1300-1400 ℃ and the third stage is heated to 1500-1600 ℃ and preserved heat for 2-6h at 1500-1600 ℃;
s5, placing the liquid material subjected to boiling melting into a forming die for forming to obtain a sample block; wherein, the forming die is preheated for about 30min at 500 ℃ before use;
s6, carrying out heat treatment on the sample block to crystallize the nucleation, wherein the process specifically comprises the following steps:
s61, nucleation stage: preserving the heat for 5-15min at the temperature of 450-; wherein the molded sample block is subjected to heat treatment before being completely cooled, and the temperature of the sample block is about 450 ℃;
s62, crystallization stage: heating to 600-700 ℃, controlling the heating rate at 50-90 ℃/min, and keeping the temperature at 600-700 ℃ for 15-60 min;
s63, complete crystallization stage: the temperature is increased to 820 ℃ at 880 ℃, the temperature increase rate is controlled to be 50-90 ℃/min, and the temperature is kept at 820 ℃ at 880 ℃ for 10-30 min.
Through accurate multistage temperature treatment, crystal nuclei with different particle sizes and lengths grow in a certain uniform range, so that a perfect interlocking structure is formed, and the properties of the glass ceramic, such as breaking strength, toughness and the like, are enhanced.
The following is a detailed description of specific examples.
Example 1
3kg of SiO22kg of Li2CO30.1kg of magnesium carbonate, 0.1kg of Al (OH)30.1kg of zirconia is added into a ball mill, the rotating speed of the ball mill is 500r/min, and the running time is 4 hours; after being uniformly mixed, the mixture is settled and dried for 5 hours, the drying temperature is 90 ℃, and the agglomeration is approximately hardened; then boiling and melting are carried out, the settled and dried material is put into a melting device with the temperature of 1200-1250 ℃, the temperature is raised to 1300-; cooling from 1500-1600 ℃ to 1300-1400 ℃, controlling the cooling rate at 25 ℃/min, repeating the second stage of heat preservation at 1300-1400 ℃ for 2h and the third stage of heat preservation at 1500-1600 ℃, and preserving heat at 1500-1600 ℃ for 2 h; (ii) a Then the liquid material after boiling and melting is placed at 500 DEG CPreheating the sample in a forming die for about 30min to obtain a sample block; then carrying out heat treatment on the sample block to cause nucleation and crystallization, and carrying out heat preservation for 5min at the temperature of 450-550 ℃; heating to 600 ℃ and 700 ℃, controlling the heating rate at 50 ℃/min, and keeping the temperature at 600 ℃ and 700 ℃ for 15 min; the temperature is increased to 820 ℃ and 880 ℃, the temperature rising rate is controlled at 50 ℃/min, and the temperature is preserved for 10min at 820 ℃ and 880 ℃. Referring to table 1, the difference in purity and particle size of zirconia causes the difference in performance, and the use of high-purity nano-grade zirconia (the overall particle size is required to be less than or equal to 100nm, and the average particle size is 40-60nm) has excellent performance in all aspects of glass ceramics.
Table 1:
example 2
4.8kg of SiO22.8kg of Li2CO30.48kg of potassium carbonate, 0.2kg of Al (OH)30.3kg of cerium oxide and 0.1kg of zirconium oxide are added into a ball mill, the rotating speed of the ball mill is 400r/min, and the running time is 1 h; after being uniformly mixed, the mixture is settled and dried for 8 hours at the drying temperature of 95 ℃, and is approximately hardened and agglomerated; then boiling and melting, putting the settled and dried material into a melting device with the temperature of 1200-1250 ℃, heating to 1300-; cooling from 1500-1600 ℃ to 1300-1400 ℃, controlling the cooling rate at 30 ℃/min, repeating the second stage of heat preservation at 1300-1400 ℃ for 3h and the third stage of heat preservation at 1500-1600 ℃, and preserving heat at 1500-1600 ℃ for 4 h; then placing the liquid material after boiling and melting in a forming die for preheating for about 30min at 500 ℃ to form a sample block; then carrying out heat treatment on the sample block to cause nucleation and crystallization, and carrying out heat preservation for 10min at the temperature of 450-550 ℃; the temperature is raised to 600 ℃ and 700 ℃, and the temperature raising rate is controlled to 70Keeping the temperature at 600-700 ℃ for 40 min; the temperature is increased to 820-. Referring to Table 2, the difference in purity and particle size of zirconia leads to performance difference, and the use of high-purity nano-grade zirconia (the overall particle size is required to be less than or equal to 100nm, and the average particle size is 40-60nm) has excellent performance in all aspects of glass ceramics.
Table 2:
example 3
6kg of SiO23.2kg of Li2CO30.8kg of potassium carbonate, 0.5kg of Al (OH)30.5kg of cerium oxide and 0.5kg of zirconium oxide are added into a ball mill, the rotating speed of the ball mill is 400r/min, and the running time is 3 hours; after being uniformly mixed, the mixture is settled and dried for 8 hours at the drying temperature of 95 ℃, and is approximately hardened and agglomerated; then boiling and melting, putting the settled and dried material into a melting device with the temperature of 1200-1250 ℃, heating to 1300-; cooling from 1500-1600 ℃ to 1300-1400 ℃, controlling the cooling rate at 30 ℃/min, repeating the second stage of heat preservation at 1300-1400 ℃ for 3h and the third stage of heat preservation at 1500-1600 ℃, and preserving heat at 1500-1600 ℃ for 4 h; then placing the liquid material after boiling and melting in a forming die for preheating for about 30min at 500 ℃ to form a sample block; then carrying out heat treatment on the sample block to cause nucleation and crystallization, and carrying out heat preservation for 10min at the temperature of 450-550 ℃; heating to 600 ℃ and 700 ℃, controlling the heating rate at 70 ℃/min, and preserving the heat for 40min at 600 ℃ and 700 ℃; the temperature is increased to 820-. Referring to Table 3, the difference in purity and particle size of the zirconia leads to performanceThe difference is that high-purity nano-grade zirconia (the overall requirement of the grain diameter is less than or equal to 100nm, the average grain diameter is 40-60nm) is adopted, and the glass ceramic has excellent performance in all aspects.
Table 3:
example 4
8kg of SiO24.5kg of Li2CO38kg of potassium carbonate, 1.5kg of Al (OH)31kg of bismuth oxide and 1kg of zirconium oxide are added into a ball mill, the rotating speed of the ball mill is 500r/min, and the running time is 5 hours; after being uniformly mixed, the mixture is settled and dried for 10 hours at the drying temperature of 100 ℃, and is approximately hardened and agglomerated; then boiling and melting are carried out, the settled and dried material is put into a melting device with the temperature of 1200-1250 ℃, the temperature is raised to 1300-; cooling from 1500-1600 ℃ to 1300-1400 ℃, controlling the cooling rate at 35 ℃/min, repeating the second stage of heat preservation for 4h at 1300-1400 ℃ and the third stage of heat preservation for 1500-1600 ℃, and preserving heat for 6h at 1500-1600 ℃; then placing the liquid material after boiling and melting in a forming die for preheating for about 30min at 500 ℃ to form a sample block; then carrying out heat treatment on the sample block to carry out nucleation and crystallization, and carrying out heat preservation for 15min at the temperature of 450-550 ℃; heating to 600 ℃ and 700 ℃, controlling the heating rate at 90 ℃/min, and keeping the temperature at 600 ℃ and 700 ℃ for 60 min; the temperature is increased to 820 ℃ and 880 ℃, the temperature rising rate is controlled at 90 ℃/min, and the temperature is kept for 30min at 820 ℃ and 880 ℃. Referring to Table 4, the difference in purity and particle size of zirconia causes the difference in performance, and the use of high-purity nano-grade zirconia (the overall particle size is required to be less than or equal to 100nm, and the average particle size is 40-60nm) provides excellent performance in all aspects of glass ceramics.
Table 4:
it will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings, and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (9)
1. A method for controlling uniform crystallization of glass ceramic, comprising: adding high-purity zirconia with the grain diameter less than or equal to 100nm into a glass ceramic raw material;
the uniform crystallization control method of the glass ceramic further comprises the following steps: uniformly mixing the glass ceramic raw material and the high-purity zirconia, settling and drying the mixture until the mixture is hardened and agglomerated, carrying out boiling melting on the dried material, placing the liquid material subjected to boiling melting in a forming die to form a sample block, and then carrying out heat treatment on the sample block to carry out nucleation and crystallization;
the temperature of the sedimentation drying is 90-100 ℃, and the time of the sedimentation drying is 5-10 h.
2. The method for controlling uniform crystallization of a glass ceramic according to claim 1, wherein the high-purity zirconia has an average particle diameter of 40 to 60 nm; the purity of the high-purity zirconia is more than or equal to 99.9 percent.
3. The method for controlling uniform crystallization of glass ceramic according to claim 1, wherein the raw materials of the glass ceramic comprise the following components in parts by mass: 30-80 parts of SiO220-45 parts of Li2CO31-15 parts of alkali metal salt, 1-10 parts of Al (OH)3And 0-10 parts of rare earth oxide, and 1-10 parts of high-purity zirconia is added at the same time.
4. The method for controlling uniform crystallization of a glass ceramic according to claim 3, wherein the high purity zirconia, SiO2、Li2CO3Alkali metal salt, Al (OH)3And the rare earth oxide comprises the following components in parts by weight: 1-5 parts of high-purity zirconia and 48-60 parts of SiO228-32 parts of Li2CO34.8-8 parts of alkali metal salt, 2-5 parts of Al (OH)3And 0-10 parts of rare earth oxide.
5. The method for controlling uniform crystallization of a glass ceramic according to claim 1, wherein the step of heat-treating the sample block to cause nucleation specifically comprises:
a1, nucleation stage: preserving the heat for 5-15min at the temperature of 450-;
a2, crystallization stage: heating to 600-700 ℃, and preserving the heat for 15-60min at 600-700 ℃;
a3, complete crystallization stage: heating to 820 and 880 ℃, and preserving the temperature for 10-30min at 820 and 880 ℃.
6. The method for controlling uniform devitrification of glass-ceramics according to claim 5, wherein the temperature rise rate is controlled to 50 to 90 ℃/min in the steps of A2 and A3.
7. The method for controlling uniform crystallization of glass ceramic according to claim 1, wherein the process of boiling and melting the dried material specifically comprises:
b1, first stage: putting the settled and dried material into a melting device with the temperature of 1200-1250 ℃;
b2, second stage: heating to 1300 ℃ and 1400 ℃, and preserving the heat for 2-4h at 1300 ℃ and 1400 ℃;
b3, third stage: heating to 1500-;
b4, cooling from 1500-1600 ℃ of the third stage to 1300-1400 ℃ of the second stage; the second and third stages are repeated.
8. The method for controlling uniform crystallization of a glass ceramic according to claim 7, wherein in the step B2, the temperature rise rate is controlled to 10 to 20 ℃/min; in the step B3, the temperature rising rate is controlled to be 20-40 ℃/min; in the step B4, the temperature reduction rate from the third stage to the second stage is controlled at 25-35 ℃/min.
9. The method for controlling uniform crystallization of a glass ceramic according to claim 1, wherein the glass ceramic raw material and the high-purity zirconia are uniformly mixed by a ball mill, and the drying temperature at the time of sedimentation drying after uniform mixing is controlled to 90 to 100 ℃.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910821009.1A CN110451806B (en) | 2019-08-30 | 2019-08-30 | Uniform crystallization control method of glass ceramic |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910821009.1A CN110451806B (en) | 2019-08-30 | 2019-08-30 | Uniform crystallization control method of glass ceramic |
Publications (2)
Publication Number | Publication Date |
---|---|
CN110451806A CN110451806A (en) | 2019-11-15 |
CN110451806B true CN110451806B (en) | 2022-03-08 |
Family
ID=68490427
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910821009.1A Active CN110451806B (en) | 2019-08-30 | 2019-08-30 | Uniform crystallization control method of glass ceramic |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110451806B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112876214B (en) * | 2021-01-22 | 2022-07-19 | 北京科技大学 | Microcrystalline foamed ceramic and preparation method and application thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1383201A (en) * | 1971-02-19 | 1975-02-05 | Pilkington Brothers Ltd | Glass ceramic material |
CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
CN106277800A (en) * | 2016-08-26 | 2017-01-04 | 湖北戈碧迦光电科技股份有限公司 | Li2o Al2o3siO2the preparation method and application of system glass ceramics |
CN106927819A (en) * | 2017-03-14 | 2017-07-07 | 南京云启金锐新材料有限公司 | Hot pressed sintering high-purity zirconia composite ceramics and preparation method thereof |
CN107056071A (en) * | 2017-04-25 | 2017-08-18 | 福州大学 | ZrO2, HfO2The gear division devitrified glass being co-doped with |
CN108840569A (en) * | 2018-06-29 | 2018-11-20 | 安徽新瑞重工股份有限公司 | A kind of novel nucleated glass and preparation method thereof |
-
2019
- 2019-08-30 CN CN201910821009.1A patent/CN110451806B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1383201A (en) * | 1971-02-19 | 1975-02-05 | Pilkington Brothers Ltd | Glass ceramic material |
CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
CN106277800A (en) * | 2016-08-26 | 2017-01-04 | 湖北戈碧迦光电科技股份有限公司 | Li2o Al2o3siO2the preparation method and application of system glass ceramics |
CN106927819A (en) * | 2017-03-14 | 2017-07-07 | 南京云启金锐新材料有限公司 | Hot pressed sintering high-purity zirconia composite ceramics and preparation method thereof |
CN107056071A (en) * | 2017-04-25 | 2017-08-18 | 福州大学 | ZrO2, HfO2The gear division devitrified glass being co-doped with |
CN108840569A (en) * | 2018-06-29 | 2018-11-20 | 安徽新瑞重工股份有限公司 | A kind of novel nucleated glass and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN110451806A (en) | 2019-11-15 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN111072276B (en) | Lithium-aluminum-silicon microcrystalline glass containing composite clarifying agent and preparation method thereof | |
CN112552032B (en) | Synthetic beta-spodumene solid solution, microcrystalline glass manufactured by using same and manufacturing method thereof | |
CN110156333A (en) | The preparation method of the devitrified glass of crystal ordering growth | |
CN110451806B (en) | Uniform crystallization control method of glass ceramic | |
CN103420614B (en) | A kind of preparation method of thick film dielectric glass powder | |
CN104108882A (en) | Float microcrystalline glass and preparation method thereof | |
CN108083641B (en) | Preparation method of microcrystalline glass with high mechanical property | |
CN108675640A (en) | A kind of intensity can improve the preparation method of devitrified glass | |
CN103771711B (en) | Devitrified glass of high quality factor and preparation method thereof | |
CN111170642A (en) | High-strength high-toughness low-expansion lithium-aluminum-silicon transparent glass ceramic and preparation method thereof | |
CN110937805B (en) | Photoetching lithium-aluminum-silicon glass material and preparation method and application thereof | |
CN104478219A (en) | Nano-scale spinel glass ceramic and preparation method thereof | |
CN109608046B (en) | Boron-containing niobate-based energy storage glass ceramic with compact glass structure and preparation method thereof | |
CN108752017B (en) | Fused zirconia corundum brick and preparation method thereof | |
CN116395971A (en) | Microcrystalline glass and preparation method and application thereof | |
CN113955943B (en) | Complex phase glass ceramics and preparation method thereof | |
CN115784605A (en) | Tantalate additive for aluminum-silicon glass and preparation method and application thereof | |
US3982918A (en) | Process for preparing a copper containing sealing glass | |
CN111471332B (en) | Magnetic microcrystalline glass coating and preparation method thereof | |
CN115304259A (en) | Low-expansion magnesium-aluminum-silicon cordierite microcrystalline glass and preparation method thereof | |
CN105110646B (en) | A kind of devitrified glass containing pyroxferroite crystalline phase and preparation method thereof | |
CN110803868A (en) | Diopside reinforced mica-based machinable glass ceramic and preparation method thereof | |
CN105330161B (en) | TiO2Saturating infrared aluminate glass ceramics of doping and preparation method thereof | |
CN112521012B (en) | Heat-resistant high-hardness high-light-transmittance glass ceramic and preparation method thereof | |
CN111333330A (en) | Glass powder for sealing nickel-based superalloy and preparation and use methods thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |