CN102070301A - Corrosion-resistant sealing glass material for primary lithium battery and preparation method thereof - Google Patents
Corrosion-resistant sealing glass material for primary lithium battery and preparation method thereof Download PDFInfo
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- CN102070301A CN102070301A CN 201010561976 CN201010561976A CN102070301A CN 102070301 A CN102070301 A CN 102070301A CN 201010561976 CN201010561976 CN 201010561976 CN 201010561976 A CN201010561976 A CN 201010561976A CN 102070301 A CN102070301 A CN 102070301A
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Abstract
The invention discloses a corrosion-resistant sealing glass material for a primary lithium battery and a preparation method thereof. The corrosion-resistant sealing glass material comprises the following components in percentage by mole: 40-60 percent of SiO2, 10-30 percent of B2O3, 5-10 percent of BaO, 5-10 percent of K2O, 5-10 percent of Na2O, 5-10 percent of Al2O3, 0-5 percent of CaO, and 0-5 percent of SrO. The sealing glass material disclosed by the invention resists the corrosion of lithium and electrolyte, has good air tightness and insulativity and is applicable to sealing of the primary lithium battery. The sealing temperature of the glass is 940 DEG C-1010 DEG C. The thermal expansion coefficient is in the range of 65-95*10-7/DEG C, more metal pole columns can be selected, the corrosion-resistant sealing glass material can be matched and sealed with molybdenum pole columns and iron-nickel alloy wires such as 4J52 and the like with excellent welding performance, the leakage caused by internal stress explosion of the glass is prevented, and the air tightness of a sealing device is ensured.
Description
Technical field
The invention belongs to battery seal glass technical field, relate to a kind of sealing glass material and preparation method thereof, especially a kind of disposable lithium-battery is with anti-corrosion sealing glass material and preparation method thereof.
Background technology
Seal glass is a kind of novel scolder, and such glass has good thermotolerance, chemical stability and high-insulativity, is widely used in fields such as electrovacuum and microelectronics, automobile, novel electron product, has realized glass and intermetallic tight the connection.Disposable lithium-battery carries out sealing-in with seal glass with the positive terminal and the negative pole matrix metal loam cake of disposable lithium-battery, plays sealing, insulating effect, is the crucial starting material of disposable lithium-battery, and the quality of its quality directly influences the performance of disposable lithium-battery.If the solidity to corrosion of seal glass, chemical stability does not reach corresponding requirement, so after the sealing-in under the very strong electrolytic solution effect of corrodibility, the phenomenon that is corroded will appear in glass, thereby cause leakage of disposable lithium-battery product even short circuit, equipment around also can corroding when serious, consequence is very serious.
At present, domestic most employing DM305, DM308, Elan13, Elan19 glass powder is as disposable lithium-battery metallic glass sealing-in lid group seal, sealing materials, mostly is kovar alloy, molybdenum pole with the positive terminal of its coupling.But weak point is pole and is difficult for welding, is difficult for processing, easily crisp; Sealing glass material is subject to the corrosion of electrolytic solution and metallic lithium when the disposable lithium-battery standing storage, cause battery leakage to lose efficacy.
The existing both at home and abroad glass that can be used for the disposable lithium-battery sealing-in has following several:
Domestic patent 200920032470.0 adopts and add the solidity to corrosion macromolecular material under vitreum, though produce effect, technology is comparatively complicated.
No. 4556613 disclosed glass of United States Patent (USP) is formed molecular fraction and is: SiO
270～75%, B2O320%, Al
2O
34～8%, Na
2O 4～7%, K
2O 6%, and BaO 0～2%, and the sealing temperature of this system glass is 1050 ℃, and thermal expansivity is 40～45 * 10
-7/ ℃.Shortcoming is SiO
2Too high levels is subject to the erosion of metallic lithium and electric liquid and causes leakage; Can only be molybdenum and molybdenum alloy for the metal of sealing-in.
No. 3770568 disclosed Ta-23 glass of United States Patent (USP) is formed molecular fraction and is: SiO
263～65%, K
2O 6～8%, B
2O
315～17%, Al
2O
32～3%, Na
2O 2～3%, and BaO 4～6%.The thermal expansivity of this system glass is 50～57 * 10
-7/ ℃.Shortcoming is that the not anti-electric liquid erosion of glass Ta23 causes leakage.
No. 6090503 disclosed Cabal P series glass CaO 20% of United States Patent (USP), B
2O
325～40%, Al2O320%, MgO 20%, SiO210～15%, SrO 0～10%.The sealing temperature of this system glass is 860～920 ℃, thermal expansivity 60～86 * 10
-7/ ℃.The anti-electric liquid erosion performance of Cabal P series glass is better than Ta23, and the system coefficient of expansion changes greatly, and available metal is many, but the water resistance extreme difference is bad with glass wettability and resistance to air loss, and leakage rate can only reach 1.0 * 10
-9Pa.m
3/ s.He causes leakage.
No. 5015530 disclosed Babal P series glass of United States Patent (USP) formed molecular fraction and be: BaO 40～60%, B
2O
330～50%, Al
2O
310～25%.The sealing temperature of this system glass is 615～750 ℃, thermal expansivity 90～114 * 10
-7/ ℃.The adjustment of this composition can be mated the seal, sealing materials of high expansion coefficient, and for example (coefficient of expansion is 11.4 * 10 to 446 (4J28) stainless steel
-6/ ℃) and 4J52 (coefficient of expansion is 9.8 * 10
-6/ ℃)..Shortcoming is that the glass water resistance is poor, and is bad with glass wettability and resistance to air loss, and leakage rate can only reach 1.0 * 10
-9Pa.m
3/ s.He causes leakage.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of disposable lithium-battery with anti-corrosion sealing glass material and preparation method thereof, this kind sealing glass material can effectively reduce glass powder principal constituent SiO by its preparation process of rational component batching and optimization
2In use suffer the erosion of electric liquid and metallic lithium in the lithium cell.And can effectively improve the flowability and the chemical stability of glass, not only can improve the wetting capacity of glass, and make the better tightness of glass metal.
The objective of the invention is to solve by the following technical programs:
The anti-corrosion sealing glass material of this disposable lithium-battery is characterized in that, in molar percentage, comprises following component:
SiO
2：40～60％；B
2O
3：10～30％；BaO：5～10％；K
2O：5～10％；Na
2O：5～10％；Al
2O
3：5～10％；CaO：0～5％；SrO：0～5％。
The present invention also provides a kind of preparation method of above-mentioned sealing glass material, may further comprise the steps:
1) according to the mole proportioning of each component, prepares burden in the mode of introducing oxide raw material;
Wherein introduce sodium oxide, analytical pure salt of wormwood introducing potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash;
2) with the oxide raw material uniform mixing of above each component, make admixtion;
3) above-mentioned admixtion is put into platinum crucible, found in silicon molybdenum High Temperature Furnaces Heating Apparatus, with the speed intensification of 50 ℃/min, insulation 30min～90min founds into glass metal in the time of 1450～1480 ℃;
4) obtain described sealing glass material after the glass metal that melts being poured in the cold water into cooling.
The present invention has following beneficial effect:
Sealing glass material of the present invention with silicon-dioxide as the glass skeleton structure, the oxide compound Al of adding
2O
3And B
2O
3, can make B
2O
3Replace part Si O
2Network skeleton.Al
2O
3As network intermediate web frame system, can effectively reduce glass powder principal constituent SiO
2In use suffer the erosion of electric liquid and metallic lithium in the lithium cell.And for the thermal expansivity of regulating glass with improve glass flow, in glass, added barium oxide.The alkali-metal adding of the present invention can improve the flowability and the chemical stability of glass, makes the better tightness of glass.And according to the basic metal effect, when its quality of alkalimetal oxide that adds was close, its chemical stability was best.The SrO of Tian Jiaing has effectively improved the wetting capacity of glass to metal as modified oxide in addition, thereby has improved the corrosion resisting property of glass powder.
In sum, the erosion of anti-lithium of glass sealing material of the present invention and electric liquid has good air-tightness and insulativity, is applicable to the sealing-in of disposable lithium-battery.940～1010 ℃ of the sealing temperatures of glass.Thermal expansivity is 65～95 * 10
-7In/℃ the scope, available metal pole is many, can both matched seal with the iron-nickel alloy wires such as 4J52 of molybdenum pole and welding property excellence, and prevented that the glass internal stress from bursting and caused leaking, guaranteed the resistance to air loss of sealing device.
Embodiment
The anti-corrosion sealing glass material of this kind disposable lithium-battery that the present invention proposes, in molar percentage, the component that comprises is: SiO
2: 40～60%; B
2O
3: 10～30%; BaO:5～10%; K
2O:5～10%; Na
2O:5～10%; Al
2O
3: 5～10%; CaO:0～5%; SrO:0～5%.The preparation method of the anti-corrosion sealing glass material of this kind comprises following four steps:
1) according to the mole proportioning of each component, prepares burden in the mode of introducing oxide raw material;
Wherein introduce sodium oxide, analytical pure salt of wormwood introducing potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash;
2) with the oxide raw material uniform mixing of above each component, make admixtion;
3) above-mentioned admixtion is put into platinum crucible, found in silicon molybdenum High Temperature Furnaces Heating Apparatus, with the speed intensification of 50 ℃/min, insulation 30min～90min founds into glass metal in the time of 1450～1480 ℃;
4) obtain described sealing glass material after the glass metal that melts being poured in the cold water into cooling.
Below in conjunction with specific examples the present invention is specifically addressed:
Table 1 has provided the molar percentage of the anti-corrosion sealing glass material component of participating in correlated each embodiment, according to the molar percentage compositing range of above-mentioned glass, determines glass formula, calculates weight of glass per-cent, and according to its batching.Carry out founding of glass, moulding according to above-mentioned glass processing preparation method.Sample after the processing is tested, testing method is: the mean coefficient of linear thermal expansion α of glass adopts the two bar coefficient of expansion determinators of ZNO-II to measure, after glass sample made bar-shaped sample about 100mm, rise to 300 ℃ by room temperature, temperature rise rate is 3～5 ℃/min.Corrosion-resistant property is by the simulation to disposable lithium-battery Working electrolyte Working environment, adopt the test of high temperature accelerated weathering test method, put into the ampoule that electric liquid is housed after glass coated with the lithium band, 150 ℃ of conditions were preserved after 21 days, taking-up glass is weighed, calculated weight corrodes ratio, represents with surperficial weightless w%.Sealing property adopts the test of He mass spectrograph.
Table 1
Embodiment 1:
Prepare burden by the composition of the molar percentage in the table 1, prepare burden in the mode of introducing oxide raw material, be specially: introduce potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash introducing sodium oxide, analytical pure salt of wormwood.With the oxide raw material uniform mixing of each component, make admixtion.
Pretreated glass compound is placed platinum crucible, found in silicon molybdenum stove: the speed with 50 ℃/min heats up, and is heated to 1450 ℃ of insulation 40min, and clarifies in 1460 ℃.
Pour the glass metal that melts into mould according to test request and prepare sample, all the other are poured into and obtain described sealing glass material in the cold water.
The taking-up of sample in the mould is handled and tested according to test request, and test result sees Table 1.
This example is preferred the composition, and its mean thermal expansion coefficients at 25～300 ℃ is 92 * 10
-7/ ℃, mate good with 4j28a, 4j52 center pole; Leak rate≤1.0 * 10
-10Pa.m3/s; Weight corrodes than 0.05.
Embodiment 2:
Prepare burden by the composition in the table 1, compare with embodiment 1, reduce strontium oxide content, relatively the anti-electric liquid of glass corrodes.
Pretreated glass compound is placed platinum crucible, in silicon molybdenum stove, be incubated 40min, and clarify in 1450 ℃ to be heated to 1440 ℃.
Pour the glass metal that melts into mould according to test request and prepare sample, all the other are poured in the cold water.
The taking-up of sample in the mould is handled and tested according to test request, and test result sees Table 1.
This example is 85 * 10 at 25～300 ℃ mean thermal expansion coefficients
-7/ ℃, mate good with 4j28a, 4j52 center pole; Leak rate≤3.0 * 10
-10Pa.m3/s; Weight corrodes than 0.12.
Embodiment 3:
Prepare burden by the composition in the table 1, compare with embodiment 1, embodiment 2, reduce the content of boron oxide and aluminum oxide, increase the content of silicon oxide, relatively the anti-electric liquid of glass corrodes.
Pretreated glass compound is placed platinum crucible, in silicon molybdenum stove, be incubated 40min, and clarify in 1500 ℃ to be heated to 1480 ℃.
Pour the glass metal that melts into mould according to test request and prepare sample, all the other are poured in the cold water.
The taking-up of sample in the mould is handled and tested according to test request, and test result sees Table 1.
This example is 80 * 10 at 25～300 ℃ mean thermal expansion coefficients
-7/ ℃, mate good with 4j29,4j52 center pole; Leak rate≤2.0 * 10
-10Pa.m3/s; Weight corrodes than 0.07.
Embodiment 4:
Prepare burden by the composition in the table 1, compare with embodiment 3, reduce barium oxide content, relatively the anti-electric liquid of glass corrodes and the closure stopping property.
Pretreated glass compound is placed platinum crucible, in silicon molybdenum stove, be incubated 40min, and clarify in 1440 ℃ to be heated to 1450 ℃.
Pour the glass metal that melts into mould according to test request and prepare sample, all the other are poured in the cold water.
The taking-up of sample in the mould is handled and tested according to test request, and test result sees Table 1.
This example is 72 * 10 at 25～300 ℃ mean thermal expansion coefficients
-7/ ℃, mate good with Mo, Ta center pole; Leak rate≤1.0 * 10
-10Pa.m3/s; Weight corrodes than 0.10.
Embodiment 5
1) according to the mole proportioning of following component, prepares burden in the mode of introducing oxide raw material;
SiO
2：60％；B
2O
3：10％；BaO：8％；K
2O：6％；Na
2O：5％；Al
2O
3：6％；CaO：3％；SrO：2％。Wherein introduce sodium oxide, analytical pure salt of wormwood introducing potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash.
2) with the oxide raw material uniform mixing of above each component, make admixtion;
3) above-mentioned admixtion is put into platinum crucible, found in silicon molybdenum High Temperature Furnaces Heating Apparatus, with the speed intensification of 50 ℃/min, insulation 90min founds into glass metal in the time of 1450 ℃;
4) obtain described sealing glass material after the glass metal that melts being poured in the cold water into cooling.
Embodiment 6
1) according to the mole proportioning of following component, prepares burden in the mode of introducing oxide raw material;
SiO
2：42％；B
2O
3：30％；BaO：6％；K
2O：7％；Na
2O：6％；Al
2O
3：7％；CaO：1％；SrO：1％。Wherein introduce sodium oxide, analytical pure salt of wormwood introducing potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash.
2) with the oxide raw material uniform mixing of above each component, make admixtion;
3) above-mentioned admixtion is put into platinum crucible, found in silicon molybdenum High Temperature Furnaces Heating Apparatus, with the speed intensification of 50 ℃/min, insulation 30min founds into glass metal in the time of 1480 ℃;
4) obtain described sealing glass material after the glass metal that melts being poured in the cold water into cooling.
Claims (2)
1. the anti-corrosion sealing glass material of disposable lithium-battery is characterized in that, in molar percentage, comprises following component:
SiO
2：40～60％；B
2O
3：10～30％；BaO：5～10％；K
2O：5～10％；Na
2O：5～10％；Al
2O
3：5～10％；CaO：0～5％；SrO：0～5％。
2. the preparation method of the described sealing glass material of claim 1 is characterized in that, may further comprise the steps:
1) according to the mole proportioning of each component, prepares burden in the mode of introducing oxide raw material;
Wherein introduce sodium oxide, analytical pure salt of wormwood introducing potassium oxide, aluminium hydroxide introducing aluminium sesquioxide, lime carbonate introducing calcium oxide, analytical pure strontium oxide introducing strontium oxide with quartz sand introducing silicon-dioxide, analytical pure boric acid introducing boron trioxide, analytical pure barium carbonate introducing barium oxide, analytical pure yellow soda ash;
2) with the oxide raw material uniform mixing of above each component, make admixtion;
3) above-mentioned admixtion is put into platinum crucible, found in silicon molybdenum High Temperature Furnaces Heating Apparatus, with the speed intensification of 50 ℃/min, insulation 30min～90min founds into glass metal in the time of 1450～1480 ℃;
4) obtain described sealing glass material after the glass metal that melts being poured in the cold water into cooling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010561976 CN102070301A (en) | 2010-11-26 | 2010-11-26 | Corrosion-resistant sealing glass material for primary lithium battery and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010561976 CN102070301A (en) | 2010-11-26 | 2010-11-26 | Corrosion-resistant sealing glass material for primary lithium battery and preparation method thereof |
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ID=44029086
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| CN109180003A (en) * | 2013-11-26 | 2019-01-11 | 肖特股份有限公司 | Anti- sodium seal glass and application thereof |
| CN105502933B (en) * | 2015-12-29 | 2017-10-13 | 江苏建达恩电子科技有限公司 | Glass tube for intelligence sensor and preparation method thereof |
| CN105502933A (en) * | 2015-12-29 | 2016-04-20 | 江苏建达恩电子科技有限公司 | Glass tube for smart sensor and manufacturing method thereof |
| CN108164145A (en) * | 2016-12-07 | 2018-06-15 | 辽宁省轻工科学研究院 | A kind of easy crystallization can cut down sealing glass material and its preparation method and application |
| CN109250916A (en) * | 2018-09-25 | 2019-01-22 | 西安赛尔电子材料科技有限公司 | A kind of sealing glass material and preparation method thereof |
| CN109250916B (en) * | 2018-09-25 | 2022-04-05 | 西安赛尔电子材料科技有限公司 | Sealing glass material and preparation method thereof |
| CN112645598A (en) * | 2020-12-27 | 2021-04-13 | 西安赛尔电子材料科技有限公司 | Preparation method and packaging process of sealing glass material for lithium-manganese dioxide battery cover group |
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| CN115974412A (en) * | 2021-10-15 | 2023-04-18 | 北京玻璃研究院有限公司 | Glass for sealing sapphire and kovar alloy and preparation method thereof |
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Application publication date: 20110525 |