CN110828168A - Multilayer microcrystalline glass capacitor and preparation method thereof - Google Patents
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- 239000011521 glass Substances 0.000 title claims abstract description 70
- 239000003990 capacitor Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 15
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 17
- 229910044991 metal oxide Inorganic materials 0.000 claims description 17
- 150000004706 metal oxides Chemical class 0.000 claims description 17
- 238000002425 crystallisation Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 238000000137 annealing Methods 0.000 claims description 11
- 230000008025 crystallization Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical group [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 239000004033 plastic Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 238000011049 filling Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- 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
-
- 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
-
- 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
-
- 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
- H01G4/30—Stacked capacitors
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
A multilayer glass ceramic capacitor and a preparation method thereof belong to the technical field of pulse power. The multilayer microcrystalline glass capacitor is of a multilayer structure of 'dielectric layer/(electrode layer/dielectric layer) n', wherein n is a positive integer greater than 1, and the dielectric layer is microcrystalline glass; the microcrystalline glass comprises the following components in percentage by mass: a (K)2O‑Na2O‑Li2O)‑b(xSrO‑(1‑x)BaO)‑cAl2O3‑dNb2O5‑eSiO2‑fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, and f is. The multilayer microcrystalline glass capacitor is applied to an energy storage device, and can effectively improve the energy storage density of the device; and the preparation process is suitable for large-scale popularization and application.
Description
Technical Field
The invention belongs to the technical field of pulse power, and particularly relates to a multilayer glass ceramic capacitor and a preparation method thereof.
Background
The pulse power capacitor is widely applied to a pulse power system, and is widely applied to the fields of geological exploration, blasting, detonator ignition and the like at present. Compared with other energy storage technologies (mechanical energy storage, chemical energy storage, inductive energy storage and the like), the dielectric capacitor energy storage has the technical advantages of high power density and package miniaturization, and the short board is low in energy storage density.
The traditional capacitor is prepared by taking dielectric ceramic powder as a raw material and adopting a process of a multilayer ceramic capacitor. However, unlike the microcrystalline glass, the microcrystalline glass is realized by a high-temperature melting annealing process, and the specific process is as shown in fig. 1, namely, the conventional process must be changed to realize the multilayer device structure. The invention is mainly based on the microcrystalline glass material, adopts a metal bonding mode to realize the preparation of the multilayer microcrystalline glass capacitor, and enables the application of the microcrystalline glass in the aspect of energy storage to realize industrialization.
Disclosure of Invention
The invention aims to provide a multilayer glass ceramic capacitor and a preparation method thereof aiming at the defects in the background technology. The multilayer microcrystalline glass capacitor obtained by the method is applied to an energy storage device, and the energy storage density of the device can be effectively improved; and the preparation process is suitable for large-scale popularization and application.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a multilayer glass ceramic capacitor is characterized in that the multilayer glass ceramic capacitor is of a multilayer structure of 'dielectric layer/(electrode layer/dielectric layer) n', wherein n is a positive integer greater than 1, and the dielectric layer is glass ceramic; the microcrystalline glass comprises the following components in percentage by mass: a (K)2O-Na2O-Li2O)-b(xSrO-(1-x)BaO)-cAl2O3-dNb2O5-eSiO2-fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, and f is.
Furthermore, adjacent electrode layers in the n electrode layers are arranged in a staggered mode, and the distance between each electrode layer and the edge of the dielectric layer is reserved to be more than 1mm, so that breakdown is prevented.
Further, in the multilayer glass ceramic capacitor, the electrode layers near the left side and the right side are connected and led out to serve as two electrodes of the capacitor.
Further, the thickness of the dielectric layer is 0.01-1 mm.
Further, the dielectric layer is prepared by adopting the following method:
firstly, weighing the raw materials according to the following formula: a (K)2O-Na2O-Li2O)-b(xSrO-(1-x)BaO)-cAl2O3-dNb2O5-eSiO2-fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, f is more than or equal to 0 weight percent and less than or equal to 10 weight percent, the mixture is placed into a corundum or platinum crucible;
secondly, pouring the molten metal oxide in a metal mold at the temperature of 1300-1600 ℃ at the temperature of 300-600 ℃, then quickly putting the metal oxide into an annealing furnace, annealing the metal oxide at the temperature of 300-600 ℃ for 1-20 h to eliminate stress, naturally cooling the metal oxide to room temperature, and taking the metal oxide out to obtain a glass block;
thirdly, crystallizing the obtained glass block by adopting a two-step crystallization method: placing the obtained glass block in a sintering furnace, heating from room temperature to 600-1000 ℃ at the speed of 5-50 ℃/min, preserving heat for 0-30 min, then cooling to 50-100 ℃ at the speed of 5-50 ℃/min, carrying out crystallization treatment for 0.1-10 h to form microcrystalline glass, finally cooling to room temperature at the speed of 0.001-0.02 ℃/min, and taking out to obtain the microcrystalline glass;
and finally, cutting, thinning and polishing the microcrystalline glass to form a regular round or square wafer, wherein the thickness of the wafer is 0.01-1 mm, and the surface roughness is 0.1-100 nm, so that the dielectric layer can be obtained.
Furthermore, the electrode layer is made of gold, silver, copper and the like, and the thickness is 100 nm-5 mu m.
The preparation method of the multilayer microcrystalline glass capacitor is characterized by comprising the following steps of:
and 3, crystallizing the glass block obtained in the step 2 by adopting a two-step crystallization method: placing the glass block obtained in the step 2 in a sintering furnace, firstly heating the glass block from room temperature to 600-1000 ℃ at the speed of 5-50 ℃/min, preserving the heat for 0-30 min, then cooling the glass block to 50-100 ℃ at the speed of 5-50 ℃/min, carrying out crystallization treatment for 0.1-10 h to form microcrystalline glass, finally cooling the glass block to room temperature at the speed of 0.001-0.02 ℃/min, and taking out the glass block to obtain the microcrystalline glass; generally, when the temperature is too high for a long time, stress (different thermal expansion coefficients of crystalline and amorphous states) is introduced or side reaction occurs due to abnormal growth of crystal grains, which directly causes deterioration of dielectric properties; the method optimizes the optimal crystallization point (namely the temperature, time and speed of the two-step crystallization) through a crystallography test means and experiments, determines that a target crystalline phase can be crystallized, and then adopts a two-step crystallization method to obtain the target microcrystalline glass, thereby not only ensuring that the target crystalline phase is separated out and does not contain impurity phases with deteriorated performance, but also controlling the grain size and the release of internal stress;
step 5, taking the wafer obtained in the step 4 as a dielectric layer, and preparing electrodes on the upper surface and the lower surface of the dielectric layer in a staggered mode;
step 6, stacking a plurality of dielectric layers with electrodes, and then welding the dielectric layers into a whole by adopting processes such as welding flux or diffusion welding, and the like to obtain a multilayer structure of 'dielectric layer/(electrode layer/dielectric layer) n', wherein n is a positive integer greater than 1;
and 7, pouring glue and carrying out plastic packaging on the multilayer structure welded in the step 6 to discharge gas in the stacked gaps, and improve the density and the mechanical strength to obtain the multilayer glass ceramic capacitor.
Further, the step 5 of preparing the electrode is to coat metal paste (thick film) or vacuum plate plating (thin film).
Further, in the step 7, the potting and the plastic packaging adopt polymers which are good in insulating property and easy to cure and mold, such as PI (polyimide), epoxy resin and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a multilayer microcrystalline glass capacitor and a preparation method thereof, and the multilayer microcrystalline glass capacitor is applied to an energy storage device and can effectively improve the energy storage density of the device; and the preparation process is suitable for large-scale popularization and application.
Drawings
FIG. 1 is a flow chart of a method for manufacturing a multilayer glass ceramic capacitor according to the present invention;
fig. 2 is a schematic cross-sectional view of a multilayer microcrystalline glass capacitor obtained in example 1 of the present invention.
Detailed Description
The technical scheme of the invention is detailed below by combining the accompanying drawings and the embodiment.
Example 1
As shown in fig. 2, a schematic cross-sectional structure diagram of the multilayer microcrystalline glass capacitor obtained in embodiment 1 includes a first dielectric layer 1, a first electrode layer 2, a second dielectric layer 3, a second electrode layer 4, a third dielectric layer 5, a third electrode layer 6, a fourth dielectric layer 7, a fourth electrode layer 8, and a fifth dielectric layer 9; the first electrode layer 2 and the third electrode layer 6 are connected and led out, and the second electrode layer 4 and the fourth electrode layer 8 are connected and led out as two electrodes of the capacitor. The dielectric layer is made of the same material and has the same thickness, and the electrode layer is made of the same material and has the same thickness.
The preparation process of the multilayer microcrystalline glass capacitor comprises the following steps:
and 3, crystallizing the glass block obtained in the step 2 by adopting a two-step crystallization method: placing the glass block obtained in the step 2 in a sintering furnace, firstly heating from room temperature to 900 ℃ at the speed of 10 ℃/min, preserving heat for 3min, then cooling to 100 ℃ at the speed of 10 ℃/min, carrying out crystallization treatment for 2h to form microcrystalline glass, finally cooling to room temperature at the speed of 0.02 ℃/min, and taking out to obtain the microcrystalline glass;
step 5, taking the wafer obtained in the step 4 as a dielectric layer, and preparing gold electrodes with the thickness of 500nm on the upper surface and the lower surface of the dielectric layer in a staggered mode, wherein the distance between the gold electrodes and the edge of the dielectric layer is 1 mm;
step 6, stacking a plurality of dielectric layers with electrodes, and then welding the dielectric layers into a whole by adopting a welding flux to obtain a multilayer structure shown in figure 2;
and 7, pouring PI (polyimide) into the welded multilayer structure obtained in the step 6 for solidification so as to discharge gas in the stacked gaps and improve the density and the mechanical strength, thus obtaining the multilayer glass ceramic capacitor.
Example 1 the wafer obtained in step 4 had a dielectric constant of 50, a withstand voltage of 80kV/mm, and an energy storage density of 1.41J/cm3Is more than 1J/cm of the current commercial use3。
Example 2
This example is different from example 1 in that: step 4 the wafer thickness was adjusted to 0.05mm, and the rest of the procedure was the same as in example 1. Example 2 the wafer obtained in step 4 had a dielectric constant of 30, a withstand voltage of 120kV/mm, and an energy storage density of 1.91J/cm3。
Example 3
This example is different from example 1 in that: step 3, during crystallization treatment, placing the glass block obtained in the step 2 in a sintering furnace, heating the glass block from room temperature to 700 ℃ at the speed of 20 ℃/min, then cooling the glass block to 80 ℃ at the speed of 20 ℃/min, performing crystallization treatment for 3 hours to form microcrystalline glass, and finally cooling the glass block to room temperature at the speed of 0.02 ℃/min, and taking out the glass block to obtain the microcrystalline glass; the rest of the procedure was the same as in example 1.
Claims (8)
1. A multilayer glass ceramic capacitor is characterized in that the multilayer glass ceramic capacitor is of a multilayer structure of 'dielectric layer/(electrode layer/dielectric layer) n', wherein n is a positive integer greater than 1, and the dielectric layer is glass ceramic; the microcrystalline glass comprises the following components in percentage by mass: a (K)2O-Na2O-Li2O)-b(xSrO-(1-x)BaO)-cAl2O3-dNb2O5-eSiO2-fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, and f is.
2. The multilayer microcrystalline glass capacitor according to claim 1, wherein adjacent electrode layers in the n electrode layers are staggered, and each electrode layer is spaced from the edge of the dielectric layer by a distance of 1mm or more.
3. The multilayer microcrystalline glass capacitor according to claim 1, wherein the dielectric layer has a thickness of 0.01 to 1 mm.
4. The multilayer microcrystalline glass capacitor of claim 1, wherein the dielectric layer is prepared by the following method:
firstly, weighing the raw materials according to the following formula: a (K)2O-Na2O-Li2O)-b(xSrO-(1-x)BaO)-cAl2O3-dNb2O5-eSiO2-fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, f is more than or equal to 0 weight percent and less than or equal to 10 weight percent, and the;
secondly, pouring the metal oxide melted in the previous step into a mold at the temperature of 1300-1600 ℃, then putting the mold into an annealing furnace, annealing the mold at the temperature of 300-600 ℃ for 1-20 h, naturally cooling the mold to room temperature, and taking the mold out to obtain a glass block;
thirdly, crystallizing the obtained glass block by adopting a two-step crystallization method: placing the obtained glass block in a sintering furnace, heating from room temperature to 600-1000 ℃ at the speed of 5-50 ℃/min, preserving heat for 0-30 min, then cooling to 50-100 ℃ at the speed of 5-50 ℃/min, carrying out crystallization treatment for 0.1-10 h, finally cooling to room temperature at the speed of 0.001-0.02 ℃/min, and taking out to obtain microcrystalline glass;
and finally, cutting, thinning and polishing the microcrystalline glass to form a wafer, wherein the thickness of the wafer is 0.01-1 mm, and the dielectric layer can be obtained.
5. The multilayer glass-ceramic capacitor according to claim 1, wherein the electrode layer is gold, silver or copper and has a thickness of 100nm to 5 μm.
6. The preparation method of the multilayer microcrystalline glass capacitor is characterized by comprising the following steps of:
step 1, weighing the raw materials according to the following formula: a (K)2O-Na2O-Li2O)-b(xSrO-(1-x)BaO)-cAl2O3-dNb2O5-eSiO2-fB2O3X is more than or equal to 0 and less than or equal to 1, wherein a is more than or equal to 5 weight percent and less than or equal to 20 weight percent, b is more than or equal to 10 weight percent and less than or equal to 30 weight percent, c is more than or equal to 1 weight percent and less than or equal to 10 weight percent, d is more than or equal to 20 weight percent and less than or equal to 40 weight percent, e is more than or equal to 20 weight percent and less than or equal to 50 weight percent, f is more than or equal to 0 weight percent and less than or equal to 10 weight percent, and the;
step 2, pouring the metal oxide melted in the step 1 into a mold at the temperature of 1300-1600 ℃, then putting the mold into an annealing furnace, annealing the mold at the temperature of 300-600 ℃ for 1-20 h, naturally cooling the mold to room temperature, and taking the mold out to obtain a glass block;
and 3, crystallizing the glass block obtained in the step 2 by adopting a two-step crystallization method: placing the glass block obtained in the step 2 in a sintering furnace, firstly heating the glass block from room temperature to 600-1000 ℃ at the speed of 5-50 ℃/min, preserving the heat for 0-30 min, then cooling the glass block to 50-100 ℃ at the speed of 5-50 ℃/min, carrying out crystallization treatment for 0.1-10 h, finally cooling the glass block to room temperature at the speed of 0.001-0.02 ℃/min, and taking out the glass block to obtain microcrystalline glass;
step 4, cutting, thinning and polishing the microcrystalline glass obtained in the step 3 to form a wafer, wherein the thickness of the wafer is 0.01-1 mm;
step 5, taking the wafer obtained in the step 4 as a dielectric layer, and preparing electrodes on the upper surface and the lower surface of the dielectric layer in a staggered mode;
step 6, stacking a plurality of dielectric layers with electrodes, and welding the dielectric layers into a whole to obtain a multilayer structure of 'dielectric layer/(electrode layer/dielectric layer) n', wherein n is a positive integer greater than 1;
and 7, pouring glue and carrying out plastic packaging on the multilayer structure welded in the step 6 to discharge gas in the stacked gaps, so as to obtain the multilayer glass ceramic capacitor.
7. The method for preparing a multilayer microcrystalline glass capacitor as claimed in claim 6, wherein the method for preparing the electrode in step 5 is coating metal paste or vacuum plating.
8. The method for preparing a multilayer microcrystalline glass capacitor as claimed in claim 6, wherein PI or epoxy resin polymer is adopted in the glue filling and plastic sealing in step 7.
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| US20210009459A1 (en) * | 2019-07-12 | 2021-01-14 | Corning Incorporated | Methods for forming glass ceramic articles |
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| US20080090715A1 (en) * | 2006-04-11 | 2008-04-17 | Michael Edward Badding | Glass-ceramic seals for use in solid oxide fuel cells |
| CN101439932A (en) * | 2008-12-26 | 2009-05-27 | 中国地质科学院尾矿利用技术中心 | Low-expansion glass-ceramics with lithia ore tailings as principal raw material and manufacturing method thereof |
| CN102260044A (en) * | 2011-04-30 | 2011-11-30 | 桂林电子科技大学 | Energy storage niobate microcrystalline glass dielectric material and preparation method thereof |
| CN105271761A (en) * | 2015-11-10 | 2016-01-27 | 同济大学 | High-energy-density niobate-based glass ceramic energy storage material and preparation and application thereof |
| CN107176792A (en) * | 2017-06-28 | 2017-09-19 | 合肥博之泰电子科技有限公司 | A kind of dielectric material of glass-ceramics and preparation method thereof |
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| US20210009459A1 (en) * | 2019-07-12 | 2021-01-14 | Corning Incorporated | Methods for forming glass ceramic articles |
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