CN114671613B - Glass ceramic material and preparation method and application thereof - Google Patents
Glass ceramic material and preparation method and application thereof Download PDFInfo
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- CN114671613B CN114671613B CN202210230140.2A CN202210230140A CN114671613B CN 114671613 B CN114671613 B CN 114671613B CN 202210230140 A CN202210230140 A CN 202210230140A CN 114671613 B CN114671613 B CN 114671613B
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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
- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
-
- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/129—Ceramic dielectrics containing a glassy phase, e.g. glass ceramic
Abstract
The invention discloses a glass ceramic material and a preparation method and application thereof. The composition of the glass ceramic material of the invention comprises TiO 2 、SiO 2 、Al 2 O 3 、B 2 O 3 、BaCO 3 、SrO、Bi 2 O 3 And Cs 2 O, its preparation method includes the following steps: 1) Mixing the raw materials in proportion, grinding, and smelting to obtain glass liquid; 2) And injecting the glass liquid into a mould, cooling and crystallizing, and then annealing to obtain the glass ceramic material. The glass ceramic material has large dielectric constant and small dielectric loss at the frequency of 10 KHz-10 MHz, and has low sintering temperature and crystallization temperature, low cost, no lead and no pollution, and is beneficial to industrialization and miniaturization of the capacitor.
Description
Technical Field
The invention relates to the technical field of capacitors, in particular to a glass ceramic material and a preparation method and application thereof.
Background
In recent years, 5G communication technology has been rapidly developed, miniaturization and high capacity of electronic devices have become a necessary trend, and development of capacitors with high energy storage density and low loss has been one of the keys. The dielectric constant of conventional ceramic capacitors is large (> 1000) but the dielectric loss is also large, while the dielectric loss of conventional glass capacitors is small but the dielectric constant is also small (< 10). Therefore, existing ceramic capacitors and glass capacitors are not capable of meeting the increasing demands, and new capacitor materials are required to be developed.
CN 109942195A discloses a glass ceramic with high dielectric constant and low dielectric loss, and the glass ceramic with large dielectric constant (400-1200) and low dielectric loss (0.0007-0.0042) is obtained by adding PbO, but the toxicity and pollution of Pb are stronger, so that the glass ceramic does not conform to the development concept of green environmental protection.
CN 109704584A discloses a kind of composition containing SrNb 6 O 16 Phase titanate and niobate compounded glass ceramic with low dielectric loss through adding CeO 2 Promote crystallization process and further obtain glass with large dielectric constant (38-42) and low dielectric loss (0.25-1.23)Ceramic, but the forming temperature is very high due to the too low content of alkaline earth metal oxide and alkali metal oxide in the glass ceramic>1400 ℃, the energy consumption is large, the dielectric loss is 0.25 at the minimum, and the dielectric loss is still too large to meet the increasing demands.
Therefore, the development of a glass ceramic material with large dielectric constant and small dielectric loss has very important significance.
Disclosure of Invention
The invention aims to provide a glass ceramic material, and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
a glass ceramic material, which comprises the following components in percentage by mass:
TiO 2 ：3.0％～6.5％；
SiO 2 ：0％～10.3％；
Al 2 O 3 ：0％～2.0％；
B 2 O 3 ：2.9％～38.8％；
BaCO 3 ：6.3％～13.0％；
SrO：0.8％～1.7％；
Bi 2 O 3 ：38.2％～78.7％；
Cs 2 O：0％～3.6％。
preferably, a glass ceramic material comprises the following components in percentage by mass:
TiO 2 ：3.0％～3.6％；
SiO 2 ：0％～8.0％；
Al 2 O 3 ：0％～1.0％；
B 2 O 3 ：2.9％～12.0％；
BaCO 3 ：6.3％～7.0％；
SrO：0.8％～1.0％；
Bi 2 O 3 ：70.0％～78.5％；
Cs 2 O：0％～3.6％。
the preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding, and smelting to obtain glass liquid;
2) And injecting the glass liquid into a mould, cooling and crystallizing, and then annealing to obtain the glass ceramic material.
Preferably, the particle size of the raw material in step 1) after grinding is less than 180 μm.
Preferably, the smelting in step 1) is carried out at a temperature of 1000-1350 ℃.
Preferably, the smelting time in the step 1) is 20-80 min.
Preferably, the cooling crystallization in the step 2) is carried out at 500-600 ℃.
Preferably, the cooling crystallization time in the step 2) is 30-90 min.
Preferably, the annealing in step 2) is performed at 300℃to 400 ℃.
Preferably, the annealing time in the step 2) is 3-5 h.
A capacitor comprises the glass ceramic material.
An electronic device comprising the capacitor.
The beneficial effects of the invention are as follows: the glass ceramic material has large dielectric constant (> 25) and small dielectric loss (< 0.004) at the frequency of 10 KHz-10 MHz, and has low sintering temperature and crystallization temperature, low cost, no lead and no pollution, and is beneficial to industrialization and miniaturization of the capacitor.
Detailed Description
The invention is further illustrated and described below in connection with specific examples.
Example 1:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 1 raw materials composition Table for glass ceramic materials
| Raw materials | Mass percent (%) |
| TiO 2 | 3.3 |
| SiO 2 | 0 |
| Al 2 O 3 | 0 |
| B 2 O 3 | 11.6 |
| BaCO 3 | 6.6 |
| SrO | 0.8 |
| Bi 2 O 3 | 77.7 |
| Cs 2 O | 0 |
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 25min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 1h at 550 ℃, and then transferring into an annealing furnace for annealing for 4h at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The test shows that the dielectric constant of the glass ceramic material of the embodiment is 35.0 at the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.004.
Example 2:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 2 raw materials composition Table for glass ceramic materials
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 20min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 1h at 550 ℃, and then transferring into an annealing furnace for annealing for 4h at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The test shows that the dielectric constant of the glass ceramic material of the embodiment is 29.0 at the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.006.
Example 3:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 3 raw materials composition Table for glass ceramic materials
| Raw materials | Mass percent (%) |
| TiO 2 | 3.4 |
| SiO 2 | 7.6 |
| Al 2 O 3 | 0 |
| B 2 O 3 | 2.9 |
| BaCO 3 | 6.7 |
| SrO | 0.9 |
| Bi 2 O 3 | 78.5 |
| Cs 2 O | 0 |
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 30min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 1h at 550 ℃, and then transferring into an annealing furnace for annealing for 4h at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The glass ceramic material of the embodiment has a dielectric constant of 36.0 at a frequency of 10 KHz-10 MHz and a dielectric loss of less than 0.007.
Example 4:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 4 raw materials composition Table for glass ceramic materials
| Raw materials | Mass percent (%) |
| TiO 2 | 3.3 |
| SiO 2 | 0 |
| Al 2 O 3 | 0.8 |
| B 2 O 3 | 11 |
| BaCO 3 | 6.6 |
| SrO | 0.9 |
| Bi 2 O 3 | 77.4 |
| Cs 2 O | 0 |
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 60min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 2 hours at 550 ℃, and then transferring into an annealing furnace for annealing for 4 hours at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The glass ceramic material of the embodiment has a dielectric constant of 56.0 at a frequency of 10 KHz-10 MHz and a dielectric loss of less than 0.007.
Example 5:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 5 raw materials composition Table for glass ceramic materials
| Raw materials | Mass percent (%) |
| TiO 2 | 3.3 |
| SiO 2 | 0 |
| Al 2 O 3 | 0.9 |
| B 2 O 3 | 11 |
| BaCO 3 | 6.7 |
| SrO | 0.9 |
| Bi 2 O 3 | 76 |
| Cs 2 O | 1.2 |
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 60min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 2 hours at 550 ℃, and then transferring into an annealing furnace for annealing for 4 hours at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The test shows that the dielectric constant of the glass ceramic material of the embodiment is 36.6 at the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.005.
Example 6:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 6 raw materials composition Table for glass ceramic materials
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 60min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 2 hours at 550 ℃, and then transferring into an annealing furnace for annealing for 4 hours at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The glass ceramic material of the present example has a dielectric constant of 49.5 and a dielectric loss of less than 0.007 at a frequency of 10KHz to 10 MHz.
Example 7:
a glass ceramic material, the raw materials of which are shown in the following table:
TABLE 7 raw materials composition Table for glass ceramic materials
The preparation method of the glass ceramic material comprises the following steps:
1) Mixing the raw materials in proportion, grinding until the particle size of the raw materials is smaller than 180 mu m (the raw materials can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 60min to obtain molten glass;
2) And (3) injecting the glass liquid into a preheated mold, preserving heat for 2 hours at 550 ℃, and then transferring into an annealing furnace for annealing for 4 hours at 350 ℃ to obtain the glass ceramic material.
Performance test:
cutting, polishing and flattening a glass ceramic material, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing the silver electrode on an alumina setter plate, placing the alumina setter plate into an electric furnace, preserving heat at 350 ℃ for 30min, and testing by using an Agilent4294A precise impedance analyzer.
The glass ceramic material of the present example has a dielectric constant of 67.0 at a frequency of 10KHz to 10MHz and a dielectric loss of less than 0.007.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (3)
1. The glass ceramic material is characterized by comprising the following raw materials in percentage by mass:
TiO 2 ：3.0％～3.6％；
SiO 2 ：0％～8.0％；
Al 2 O 3 ：0％～1.0％；
B 2 O 3 ：2.9％～12.0％；
BaCO 3 ：6.3％～7.0％；
SrO：0.8％～1.0％；
Bi 2 O 3 ：70.0％～78.5％；
Cs 2 O：0％～3.6％；
the glass ceramic material is prepared by a preparation method comprising the following steps: 1) Mixing the raw materials in proportion, grinding, and smelting to obtain glass liquid; 2) Injecting the glass liquid into a mold, cooling and crystallizing, and then annealing to obtain a glass ceramic material; the grain diameter of the raw materials in the step 1) is smaller than 180 mu m after grinding; the smelting of the step 1) is carried out at 1000-1350 ℃; the smelting time of the step 1) is 20-80 min; step 2), cooling crystallization is carried out at 500-600 ℃; the cooling crystallization time of the step 2) is 30-90 min; step 2) annealing is carried out at 300-400 ℃; and 2) annealing for 3-5 hours.
2. A capacitor having a composition comprising the glass-ceramic material of claim 1.
3. An electronic device comprising the capacitor of claim 2.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002308645A (en) * | 2001-04-05 | 2002-10-23 | Asahi Glass Co Ltd | Lead-free glass, glass-ceramics composition and glass paste |
| CN110451807A (en) * | 2019-07-29 | 2019-11-15 | 同济大学 | The bismuth niobate barium sodium base glass ceramic material of high energy storage density and its preparation and application |
| CN113830829A (en) * | 2021-09-30 | 2021-12-24 | 西安交通大学 | Flaky bismuth titanate strontium barium template crystal grain and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2361230B2 (en) * | 1973-12-08 | 1975-10-30 | Tdk Electronics Co. Ltd., Tokio | Ceramic dielectric |
| JP3381332B2 (en) * | 1993-08-24 | 2003-02-24 | 日本電気硝子株式会社 | High dielectric constant glass ceramic |
| JP3624406B2 (en) * | 1995-03-27 | 2005-03-02 | 日本電気硝子株式会社 | Glass ceramic dielectric material |
| CN107459347B (en) * | 2017-08-31 | 2020-07-14 | 陕西科技大学 | Lead-free ceramic material with high energy storage density and high energy storage efficiency and preparation method thereof |
| CN111925187A (en) * | 2020-07-03 | 2020-11-13 | 成都宏科电子科技有限公司 | Lead-free high-pressure medium-temperature sintered strontium bismuth titanium-based dielectric material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002308645A (en) * | 2001-04-05 | 2002-10-23 | Asahi Glass Co Ltd | Lead-free glass, glass-ceramics composition and glass paste |
| CN110451807A (en) * | 2019-07-29 | 2019-11-15 | 同济大学 | The bismuth niobate barium sodium base glass ceramic material of high energy storage density and its preparation and application |
| CN113830829A (en) * | 2021-09-30 | 2021-12-24 | 西安交通大学 | Flaky bismuth titanate strontium barium template crystal grain and preparation method thereof |
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