CN114671613A - 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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- CN114671613A CN114671613A CN202210230140.2A CN202210230140A CN114671613A CN 114671613 A CN114671613 A CN 114671613A CN 202210230140 A CN202210230140 A CN 202210230140A CN 114671613 A CN114671613 A CN 114671613A
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- 239000006112 glass ceramic composition Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 47
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 239000003990 capacitor Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 10
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 8
- 238000003723 Smelting Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 239000006060 molten glass Substances 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 7
- 238000005520 cutting process Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000005498 polishing Methods 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- 239000002241 glass-ceramic Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- 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, LIGHT-SENSITIVE OR TEMPERATURE-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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a glass ceramic material and a preparation method and application thereof. The composition of the glass-ceramic material of the present invention comprises TiO2、SiO2、Al2O3、B2O3、BaCO3、SrO、Bi2O3And Cs2O, the preparation method comprises the following steps: 1) mixing the raw materials in proportion, grinding, and smelting to obtain glass liquid; 2) and injecting the molten glass into a mold, cooling and crystallizing, and annealing to obtain the glass ceramic material. The glass ceramic material of the invention is prepared at 10 KHz-10 MHzThe dielectric constant under the frequency is large, the dielectric loss is small, the sintering temperature and the crystallization temperature are low, the cost is low, lead and pollution are avoided, and the industrialization and the miniaturization of the capacitor are facilitated.
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, and miniaturization and high capacity of electronic devices have become inevitable trends, and development of capacitors with high energy storage density and low loss is one of the keys. Conventional ceramic capacitors have a large dielectric constant (>1000), but also large dielectric losses, whereas conventional glass capacitors have a small dielectric loss, but also small dielectric constants (< 10). Therefore, the existing ceramic capacitor and glass capacitor cannot meet the increasing demand, and new capacitor materials need to be developed.
CN 109942195A discloses a glass ceramic with high dielectric constant and low dielectric loss, which is obtained by adding PbO, and has large dielectric constant (400-1200) and low dielectric loss (0.0007-0.0042), but is not in accordance with the green environmental protection development concept due to strong toxicity and pollution of Pb.
CN 109704584A discloses a SrNb-containing alloy6O16The phase titanate and niobate compounded glass ceramic with low dielectric loss is prepared by adding CeO2Promotes the crystallization process, further obtains glass ceramics with large dielectric constant (38-42) and low dielectric loss (0.25-1.23), but the forming temperature is very high due to the low content of alkaline earth metal oxide and alkali metal oxide in the glass ceramics: (>1400 ℃), and the energy consumption is high, and the dielectric loss is 0.25 at the minimum, which is still too large to meet the increasing demand.
Therefore, it is very important to develop a glass ceramic material with large dielectric constant and small dielectric loss.
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:
the glass ceramic material comprises the following components in percentage by mass:
TiO2：3.0％～6.5％；
SiO2：0％～10.3％；
Al2O3：0％～2.0％；
B2O3：2.9％～38.8％；
BaCO3：6.3％～13.0％；
SrO：0.8％～1.7％；
Bi2O3：38.2％～78.7％；
Cs2O：0％～3.6％。
Preferably, the glass ceramic material comprises the following components in percentage by mass:
TiO2：3.0％～3.6％；
SiO2：0％～8.0％；
Al2O3：0％～1.0％；
B2O3：2.9％～12.0％；
BaCO3：6.3％～7.0％；
SrO：0.8％～1.0％；
Bi2O3：70.0％～78.5％；
Cs2O：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 metal;
2) and injecting the molten glass into a mold, cooling and crystallizing, and annealing to obtain the glass ceramic material.
Preferably, the particle size of the raw material in step 1) is less than 180 μm after grinding.
Preferably, the smelting in step 1) is carried out at 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 and 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 comprises the capacitor.
The invention has the beneficial effects that: the glass ceramic material has large dielectric constant (>25) and small dielectric loss (<0.004) under the frequency of 10 KHz-10 MHz, has low sintering temperature and crystallization temperature, low cost and no lead and pollution, and is beneficial to the industrialization and the miniaturization of capacitors.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a glass ceramic material, the raw material composition of which is shown in the following table:
TABLE 1 raw material composition table of glass ceramic material
| Raw materials | Mass percent (%) |
| TiO2 | 3.3 |
| SiO2 | 0 |
| Al2O3 | 0 |
| B2O3 | 11.6 |
| BaCO3 | 6.6 |
| SrO | 0.8 |
| Bi2O3 | 77.7 |
| Cs2O | 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 less than 180 μm (can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding into a muffle furnace, and keeping the temperature at 1350 ℃ for 25min to obtain glass liquid;
2) and injecting the glass liquid into the 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.
And (3) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing on an alumina setter plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material of the embodiment is 35.0 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.004.
Example 2:
A glass ceramic material, the raw material composition of which is shown in the following table:
TABLE 2 raw material composition table of glass ceramic material
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 less than 180 μm (the raw materials can pass through a 80-mesh screen), then filling the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 20min to obtain glass liquid;
2) and injecting the glass liquid into the 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.
And (4) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by conductive silver paste, drying, placing on an alumina burning plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material is 29.0 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.006.
Example 3:
the glass ceramic material comprises the following raw materials in percentage by weight:
TABLE 3 raw material composition table of glass ceramic material
| Raw materials | Mass percent (%) |
| TiO2 | 3.4 |
| SiO2 | 7.6 |
| Al2O3 | 0 |
| B2O3 | 2.9 |
| BaCO3 | 6.7 |
| SrO | 0.9 |
| Bi2O3 | 78.5 |
| Cs2O | 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 less than 180 μm (the raw materials can pass through a 80-mesh screen), then filling the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat for 30min at 1350 ℃ to obtain glass liquid;
2) and injecting the glass liquid into the 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.
And (4) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by conductive silver paste, drying, placing on an alumina burning plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material is 36.0 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.007.
Example 4:
the glass ceramic material comprises the following raw materials in percentage by weight:
TABLE 4 raw material composition table of glass ceramic material
| Raw materials | Mass percent (%) |
| TiO2 | 3.3 |
| SiO2 | 0 |
| Al2O3 | 0.8 |
| B2O3 | 11 |
| BaCO3 | 6.6 |
| SrO | 0.9 |
| Bi2O3 | 77.4 |
| Cs2O | 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 less than 180 μm (can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding into a muffle furnace, and keeping the temperature at 1350 ℃ for 60min to obtain glass liquid;
2) And injecting the glass liquid into the 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.
And (4) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing on an alumina setter plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material of the embodiment is 56.0 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.007.
Example 5:
the glass ceramic material comprises the following raw materials in percentage by weight:
TABLE 5 raw material composition table of glass ceramic material
| Raw materials | Mass percent (%) |
| TiO2 | 3.3 |
| SiO2 | 0 |
| Al2O3 | 0.9 |
| B2O3 | 11 |
| BaCO3 | 6.7 |
| SrO | 0.9 |
| Bi2O3 | 76 |
| Cs2O | 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 less than 180 μm (the raw materials can pass through a 80-mesh screen), then filling the raw materials into an alumina crucible, adding the alumina crucible into a muffle furnace, and preserving heat at 1350 ℃ for 60min to obtain glass liquid;
2) and injecting the glass liquid into the preheated mold, preserving heat for 2h at 550 ℃, and then transferring into an annealing furnace for annealing for 4h at 350 ℃ to obtain the glass ceramic material.
And (4) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing on an alumina setter plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material of the embodiment is 36.6 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.005.
Example 6:
the glass ceramic material comprises the following raw materials in percentage by weight:
TABLE 6 raw material composition table of glass ceramic material
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 less than 180 μm (can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding into a muffle furnace, and keeping the temperature at 1350 ℃ for 60min to obtain glass liquid;
2) and injecting the glass liquid into the 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.
And (3) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing on an alumina setter plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material is 49.5 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.007.
Example 7:
a glass ceramic material, the raw material composition of which is shown in the following table:
TABLE 7 raw material composition table of glass ceramic material
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 less than 180 μm (can pass through a 80-mesh screen), loading the raw materials into an alumina crucible, adding into a muffle furnace, and keeping the temperature at 1350 ℃ for 60min to obtain glass liquid;
2) and injecting the glass liquid into the preheated mold, preserving heat for 2h at 550 ℃, and then transferring into an annealing furnace for annealing for 4h at 350 ℃ to obtain the glass ceramic material.
And (3) performance testing:
cutting a glass ceramic material, polishing and flattening, cleaning the surface, preparing a silver electrode by using conductive silver paste, drying, placing on an alumina setter plate, placing in an electric furnace, keeping the temperature at 350 ℃ for 30min, and testing by using an Agilent4294A precision impedance analyzer.
Through tests, the dielectric constant of the glass ceramic material of the embodiment is 67.0 under the frequency of 10 KHz-10 MHz, and the dielectric loss is less than 0.007.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The glass ceramic material is characterized by comprising the following components in percentage by mass:
TiO2：3.0％～6.5％；
SiO2：0％～10.3％；
Al2O3：0％～2.0％；
B2O3：2.9％～38.8％；
BaCO3：6.3％～13.0％；
SrO：0.8％～1.7％；
Bi2O3：38.2％～78.7％；
Cs2O：0％～3.6％。
2. the method of preparing a glass-ceramic material according to claim 1, comprising the steps of:
1) mixing the raw materials in proportion, grinding, and smelting to obtain glass liquid;
2) and injecting the molten glass into a mold, cooling and crystallizing, and annealing to obtain the glass ceramic material.
3. The method for preparing a glass-ceramic material according to claim 2, characterized in that: the particle size of the raw materials in the step 1) is less than 180 μm after grinding.
4. The method for preparing a glass-ceramic material according to claim 2, characterized in that: the smelting in the step 1) is carried out at 1000-1350 ℃.
5. The method for preparing a glass-ceramic material according to any of claims 2 to 4, characterized in that: the smelting time in the step 1) is 20-80 min.
6. The method for preparing a glass-ceramic material according to claim 2, characterized in that: and 2) cooling and crystallizing at 500-600 ℃.
7. The method for preparing a glass-ceramic material according to any one of claims 2 to 4 and 6, characterized in that: the cooling and crystallization time of the step 2) is 30-90 min.
8. The method for preparing a glass-ceramic material according to any one of claims 2 to 4 and 6, wherein: step 2) annealing is carried out at 300-400 ℃; the annealing time in the step 2) is 3-5 h.
9. A capacitor having a composition comprising the glass-ceramic material of claim 1.
10. An electronic device characterized in that the composition comprises the capacitor of claim 9.
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2022
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