CN114212998A - Preparation method and sealing process for sealing glass of supercapacitor cover group - Google Patents
Preparation method and sealing process for sealing glass of supercapacitor cover group Download PDFInfo
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- CN114212998A CN114212998A CN202111533531.3A CN202111533531A CN114212998A CN 114212998 A CN114212998 A CN 114212998A CN 202111533531 A CN202111533531 A CN 202111533531A CN 114212998 A CN114212998 A CN 114212998A
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- glass
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- sealing glass
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
- C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
-
- 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
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/02—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing by fusing glass directly to metal
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
- C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/78—Cases; Housings; Encapsulations; Mountings
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method and a sealing process for sealing glass of a cover group of a super capacitor, and provides a sealing glass material with corrosion resistance of fluorine-containing electrolyte and excellent electrochemical and mechanical properties. Selecting SiO2‑B2O3‑Al2O3The CaO-BaO glass system is a main body, and the thermal expansion coefficient, the glass softening temperature and the chemical stability of the glass are adjusted by adding various metal oxidesAnd the like. Introduction of Na2O、K2O, MgO adjusting the coefficient of thermal expansion and softening temperature of the glass; meanwhile, cations with different ionic radii form compact accumulation, so that the strength and the electric insulation performance of the glass are improved; introducing small amount of ZnO and ZrO2Enter a glass network structure to play a role in connecting Si-O-Si and B-O-B, and improve the chemical stability of the glass; introduction of La2O3The wettability and the sealing strength between the glass and the metal are improved. The prepared thermal expansion coefficient is 80-150 multiplied by 10‑7The silico-aluminoborate glass with the glass softening temperature of 560-760 ℃ can be used for sealing and connecting the cover group of the super capacitor of iron-based alloy, nickel-based alloy and iron-nickel-based alloy material.
Description
Technical Field
The invention belongs to the field of glass-metal sealing, relates to a preparation method and a sealing process of sealing glass, and particularly relates to a preparation method and a sealing process of sealing glass for a cover group of a super capacitor.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a rechargeable battery, and has the characteristics of quick charge and discharge of the capacitor and the energy storage characteristic of the battery. Because of its high charge and discharge power, the super capacitor is widely used as a power source for various power type components. However, the electrolyte contains fluorine ions, so that the electrolyte has certain corrosion performance on glass sealing materials, and the service life and the use of the electrolyte are severely limited.
Along with the development of the internet of things and artificial intelligence, the super capacitor is more and more valued and applied by people, and is widely applied to a memory and a backup power supply. In various electronic systems, the supercapacitor cover group is used for electrical connection and signal transmission between devices, assemblies and components and between systems, and is a necessary basic element for forming a complete system. At present, in various intelligent mechanical equipment, the using amount of the super capacitor is huge, so that the reliability and the stability of the super capacitor are paid more and more attention by people, and the super capacitor cover group is also widely applied to various intelligent manufacturing systems due to the high quality and the high reliability of the super capacitor cover group. One of the key factors in the reliability and stability of supercapacitors is the cap set.
The stainless steel and the iron-nickel alloy have the advantages of low cost, easy processing, good heat conductivity, good electrical conductivity and the like. In addition, in air and neutral water environment, the metal material has very good chemical stability and corrosion resistance, and is widely applied to lithium batteries.
Most of glass used for sealing the cover group of the conventional super capacitor is high silicate glass, electrolyte corrosion resistance is poor, mechanical vibration resistance is poor and other factors cause easy leakage of the battery, so that the service life and the performance of the battery are severely limited, and the glass belongs to low silicate glass.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method and a sealing process for sealing glass of a cover group of a super capacitor.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of sealing glass for a cover group of a super capacitor comprises the following raw materials in percentage by mole: SiO 22：50％～65％、B2O3：10％～35％、Al2O3：5％～10％、CaO：3％～5％、BaO：5％～10％、Na2O：3％～8％、K2O：2％～5％、MgO：2％～5％、TiO2：0％～5％、ZrO2：0％～5％、ZnO：0％～5％、La2O3: 0% -5%; various oxides in the raw materials comprise various salts and acid-base compounds thereof; the preparation method of the sealing glass comprises the following steps:
step 1), weighing the raw materials according to a formula, and then placing the raw materials into an ultra-high speed dispersion machine for mixing and dispersing, so that different raw materials are fully mixed to obtain uniformly dispersed raw materials;
step 2), placing the uniformly dispersed raw materials into a crucible, then placing the crucible into a silicon-molybdenum furnace, heating the crucible to 300-600 ℃ from room temperature at a heating rate of 5-10 ℃/min in an air atmosphere, and preserving the heat at 300-600 ℃ for 30-60min to promote the decomposition of the raw materials; raising the temperature to 1500-1700 ℃ at a heating rate of 10-15 ℃/min, and preserving the heat at 1500-1700 ℃ for 1-2 hours; stirring for several times during the process to make the molten material uniform and obtain completely molten and clear molten glass; quenching the glass liquid by water quenching to obtain glass slag;
step 3), placing the obtained glass cullet into an oven, drying for 12 hours at 100-150 ℃, placing the dried glass cullet into a corundum ball milling tank, grinding for 4 hours at the rotating speed of 200-400r/min, and sieving with a 150-mesh sieve to obtain the special sealing glass material for the acceleration sensor; the prepared sealing glass material is processed into a glass blank by a pulping-spraying granulation-blank making method, and then subsequent sealing can be carried out.
Further, the sealing glass material has a thermal expansion coefficient α of 80 × 10-7-150×10-7/℃。
Furthermore, the softening temperature Ts of the sealing glass material is 560-760 ℃.
A sealing process for sealing glass of a supercapacitor cover group comprises the following steps: assembling a super capacitor cover group to be sealed and a glass blank into a component to be sealed, putting the component into a chain type atmosphere sealing furnace, introducing protective gas into the furnace to prevent oxidation, rapidly raising the temperature in the furnace to 800-1000 ℃, and preserving the heat for 15-45 min at 800-1000 ℃ to seal, thus obtaining the sealing component.
Further, the supercapacitor cover group comprises a core column and a metal shell, a through hole is formed in the metal shell, the core column is inserted into the through hole of the metal shell and penetrates through the through hole, and the metal shell and the core column are sealed through sealing glass to obtain a sealed supercapacitor cover group; the metal shell is made of stainless steel, and the stainless steel can be 304, 304L, 316 and 316L, but is not limited to the above brands; the core column is made of iron-nickel alloy, and the iron-nickel alloy can be various alloys such as 4J28, 4J50 and 4J52, but is not limited to the alloys.
Further, the protective gas is nitrogen, helium, argon or other inert gases.
Furthermore, the obtained sealing component is a super capacitor cover group with good air tightness, compressive mechanical strength, chemical stability, insulativity and resistance to corrosion of fluorine-containing electrolyte.
The invention has the beneficial effects that: compared with the prior art, the invention discloses a preparation method of sealing glass for a cover group of a super capacitor and a sealing process thereof, and provides a glass material which is resistant to corrosion of fluorine-containing electrolyte, excellent in comprehensive performances such as electrochemical performance and mechanical performance and used for sealing the cover group of the super capacitor, wherein the shell adopts stainless steel series including 304L, 316L and the like, and the core column adopts a series of iron-nickel alloys such as alloys 4J28, 4J50 and 4J 52. Selecting SiO2-B2O3-Al2O3The CaO-BaO glass system is a main body, and the performances of the glass, such as the thermal expansion coefficient, the glass softening temperature, the chemical stability and the like, are adjusted by adding various metal oxides. By introducing Na2O、K2O, MgO the coefficient of thermal expansion and softening temperature of the glass can be adjusted; meanwhile, cations with different ionic radii form compact accumulation, so that the strength and the electric insulation performance of the glass can be improved; by introducing small amount of ZnO and ZrO2The glass can enter a glass network structure to play a role in connecting Si-O-Si and B-O-B, and the chemical stability of the glass can be improved; by introducing La2O3Can improve the adhesion between glass and metalWettability and sealing strength. The thermal expansion coefficient is 80-150 multiplied by 10 by adding various oxides-7The silico-aluminoborate glass with the glass softening temperature of 560-760 ℃ can be used for sealing and connecting the cover group of the super capacitor of iron-based alloy, nickel-based alloy and iron-nickel-based alloy material.
Drawings
Fig. 1 is a schematic structural diagram of a sealed supercapacitor cap pack provided by the present invention.
1-core column; 2-sealing glass; 3-metal shell.
Detailed Description
The invention is further illustrated by the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention.
Examples
A preparation method of a glass material for sealing a cover group of a super capacitor comprises the following steps:
1) selecting the following raw materials in percentage by mol: SiO 22：50％～65％、B2O3：10％～35％、Al2O3：5％～10％、CaO：3％～5％、BaO：5％～10％、Na2O：3％～8％、K2O：2％～5％、MgO：2％～5％、TiO2：0％～5％、ZrO2：0％～5％、ZnO：0％～5％、La2O3: 0 to 5 percent. Wherein, the oxides should contain various salts and acid-base compounds thereof;
2) mixing and dispersing the raw materials in an ultra-high speed dispersion machine to uniformly mix and disperse various raw materials;
3) placing the uniformly mixed materials in a crucible, placing the crucible in a silicon-molybdenum furnace, heating the crucible from room temperature to 300-plus-600 ℃ at a heating rate of 5-10 ℃/min in an air atmosphere, preserving the heat at the temperature of 300-plus-600 ℃ for 30-60min to promote the decomposition of various salts and acid-base compounds, heating the crucible to 1500-plus-1700 ℃ at a heating rate of 10-15 ℃/min, and preserving the heat at the temperature of 1500-plus-1700 ℃ for 1-2 hours; stirring for several times during the process to enable the molten materials to be uniform, and obtaining molten glass after the molten materials are completely melted and clarified; pouring the glass liquid into cold distilled water, and performing water quenching to obtain glass slag;
4) placing the obtained glass broken slag in a drying oven, drying for 12 hours at the temperature of 100-150 ℃, placing the baked glass broken slag in a corundum ball milling tank, grinding for 4 hours at the rotating speed of 200-400r/min, and sieving by a 150-mesh sieve to obtain the special sealing glass powder for the cover group of the super capacitor; the prepared sealing glass material is processed into a glass blank by a pulping-spraying granulation-blank making method, and then subsequent sealing can be carried out. The coefficient of thermal expansion α of the sealing glass is 80 × 10-7-150×10-7/° c; the softening temperature Ts of the sealing glass is 560-760 ℃.
A sealing process for sealing a glass material of a cover group of a super capacitor comprises the following steps: assembling the supercapacitor cover group to be sealed and the glass blank into a component to be sealed, putting the component into a chain type atmosphere sealing furnace, introducing protective gas into the furnace to prevent oxidation, rapidly raising the temperature in the furnace to 800-1000 ℃, and preserving the heat for 15-45 min at 800-1000 ℃ for sealing to obtain the supercapacitor cover group with good air tightness, compressive mechanical strength, chemical stability, insulativity and fluorine-containing electrolyte corrosion resistance. The super capacitor cover group comprises a core column and a metal shell, wherein a through hole is formed in the metal shell, the core column is inserted into the through hole of the metal shell and penetrates through the through hole, and the metal shell and the core column are sealed through sealing glass to obtain a sealed super capacitor cover group; the metal shell is made of stainless steel, and the stainless steel can be 304, 304L, 316 and 316L, but is not limited to the above brands; the core column is made of iron-nickel alloy, and the iron-nickel alloy can be various alloys such as 4J28, 4J50 and 4J52, but is not limited to the alloys.
Specific examples are as follows:
the thermal expansion coefficient and the softening point temperature are tested by a thermal expansion instrument, the air tightness is tested by a helium mass spectrometer leak detector, the insulativity is tested by a resistance tester, the breaking strength is tested by a press machine, the corrosion resistance is tested by placing a sealed terminal in 0.01 percent F-solution, and the number of days for corrosion resistance of glass is counted.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (7)
1. The preparation method of the sealing glass for the cover group of the supercapacitor is characterized in that the sealing glass is prepared from the following raw materials in percentage by mole: SiO 22：50％～65％、B2O3：10％～35％、Al2O3：5％～10％、CaO：3％～5％、BaO：5％～10％、Na2O：3％～8％、K2O：2％～5％、MgO：2％～5％、TiO2：0％～5％、ZrO2：0％～5％、ZnO：0％～5％、La2O3: 0% -5%; various oxides in the raw materials comprise various salts and acid-base compounds thereof; the preparation method of the sealing glass comprises the following steps:
step 1), weighing the raw materials according to a formula, and then placing the raw materials into an ultra-high speed dispersion machine for mixing and dispersing, so that different raw materials are fully mixed to obtain uniformly dispersed raw materials;
step 2), placing the uniformly dispersed raw materials into a crucible, then placing the crucible into a silicon-molybdenum furnace, heating the crucible to 300-600 ℃ from room temperature at a heating rate of 5-10 ℃/min in an air atmosphere, and preserving the heat at 300-600 ℃ for 30-60min to promote the decomposition of the raw materials; raising the temperature to 1500-1700 ℃ at a heating rate of 10-15 ℃/min, and preserving the heat at 1500-1700 ℃ for 1-2 hours; stirring for several times during the process to make the molten material uniform and obtain completely molten and clear molten glass; quenching the glass liquid by water quenching to obtain glass slag;
step 3), placing the obtained glass cullet into an oven, drying for 12 hours at 100-150 ℃, placing the dried glass cullet into a corundum ball milling tank, grinding for 4 hours at the rotating speed of 200-400r/min, and sieving with a 150-mesh sieve to obtain the special sealing glass material for the acceleration sensor; the prepared sealing glass material is processed into a glass blank by a pulping-spraying granulation-blank making method, and then subsequent sealing can be carried out.
2. The method of claim 1, wherein the step of preparing a sealing glass for a cover assembly of a supercapacitor comprises: the thermal expansion coefficient alpha of the sealing glass material is 80 multiplied by 10-7-150×10-7/℃。
3. The method of claim 1, wherein the step of preparing a sealing glass for a cover assembly of a supercapacitor comprises: the softening temperature Ts of the sealing glass material is 560-760 ℃.
4. A sealing process for sealing glass of a supercapacitor cover group is characterized by comprising the following steps: assembling a super capacitor cover group to be sealed and a glass blank into a component to be sealed, putting the component into a chain type atmosphere sealing furnace, introducing protective gas into the furnace to prevent oxidation, rapidly raising the temperature in the furnace to 800-1000 ℃, and preserving the heat for 15-45 min at 800-1000 ℃ to seal, thus obtaining the sealing component.
5. A sealing process for a sealing glass of a cap group of a supercapacitor according to claim 4, wherein: the super capacitor cover group comprises a core column and a metal shell, wherein a through hole is formed in the metal shell, the core column is inserted into the through hole of the metal shell and penetrates through the through hole, and the metal shell and the core column are sealed through sealing glass to obtain a sealed super capacitor cover group; the metal shell is made of stainless steel, and the core column is made of iron-nickel alloy.
6. A sealing process for a sealing glass of a cap group of a supercapacitor according to claim 4, wherein: the protective gas is nitrogen, helium, argon or other inert gases.
7. A sealing process for a sealing glass of a cap group of a supercapacitor according to claim 4, wherein: the obtained sealing component is a super capacitor cover group with good air tightness, compressive mechanical strength, chemical stability, insulativity and resistance to corrosion of fluorine-containing electrolyte.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111533531.3A CN114212998A (en) | 2021-12-15 | 2021-12-15 | Preparation method and sealing process for sealing glass of supercapacitor cover group |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111533531.3A CN114212998A (en) | 2021-12-15 | 2021-12-15 | Preparation method and sealing process for sealing glass of supercapacitor cover group |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002094727A1 (en) * | 2001-05-08 | 2002-11-28 | Forschungszentrum Jülich GmbH | Glass solder materials as jointing materials for use at high temperatures, production and use thereof |
| CN102070300A (en) * | 2010-11-26 | 2011-05-25 | 西安华泰有色金属实业有限责任公司 | Glass sealing material for thermal battery and preparation method thereof |
| CN202977550U (en) * | 2012-12-29 | 2013-06-05 | 惠州亿纬锂能股份有限公司 | Sealing element for lithium ion battery capacitor |
| CN112599360A (en) * | 2020-12-31 | 2021-04-02 | 上海奥威科技开发有限公司 | Super capacitor, liquid injection equipment and liquid injection method |
| CN112694257A (en) * | 2020-12-27 | 2021-04-23 | 西安赛尔电子材料科技有限公司 | Preparation method and sealing process of explosion-proof lithium primary battery cover group and sealing glass |
-
2021
- 2021-12-15 CN CN202111533531.3A patent/CN114212998A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002094727A1 (en) * | 2001-05-08 | 2002-11-28 | Forschungszentrum Jülich GmbH | Glass solder materials as jointing materials for use at high temperatures, production and use thereof |
| CN102070300A (en) * | 2010-11-26 | 2011-05-25 | 西安华泰有色金属实业有限责任公司 | Glass sealing material for thermal battery and preparation method thereof |
| CN202977550U (en) * | 2012-12-29 | 2013-06-05 | 惠州亿纬锂能股份有限公司 | Sealing element for lithium ion battery capacitor |
| CN112694257A (en) * | 2020-12-27 | 2021-04-23 | 西安赛尔电子材料科技有限公司 | Preparation method and sealing process of explosion-proof lithium primary battery cover group and sealing glass |
| CN112599360A (en) * | 2020-12-31 | 2021-04-02 | 上海奥威科技开发有限公司 | Super capacitor, liquid injection equipment and liquid injection method |
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