CN104451481A - Finished product annealing method of high voltage anode aluminum foil for electrolytic capacitor - Google Patents
Finished product annealing method of high voltage anode aluminum foil for electrolytic capacitor Download PDFInfo
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- CN104451481A CN104451481A CN201410787982.3A CN201410787982A CN104451481A CN 104451481 A CN104451481 A CN 104451481A CN 201410787982 A CN201410787982 A CN 201410787982A CN 104451481 A CN104451481 A CN 104451481A
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- 238000000137 annealing Methods 0.000 title claims abstract description 41
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 28
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000011888 foil Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000003990 capacitor Substances 0.000 title abstract description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 31
- 229910052786 argon Inorganic materials 0.000 claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 21
- 238000009413 insulation Methods 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000012299 nitrogen atmosphere Substances 0.000 abstract 1
- 239000005030 aluminium foil Substances 0.000 description 26
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010731 rolling oil Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 230000001550 time effect Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
- H01G9/045—Electrodes or formation of dielectric layers thereon characterised by the material based on aluminium
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Metal Rolling (AREA)
Abstract
The invention relates to a finished product annealing method of a high voltage anode aluminum foil for an electrolytic capacitor. The method is characterized by comprising the following steps: vacuumizing an annealing furnace to less than 0.1333pa, and charging argon or nitrogen into the annealing furnace until the pressure reaches 30kpa to 80kpa; heating the annealing furnace to 230 DEG C, performing heat preserving, vacuumizing the annealing furnace to less than 0.1333pa after the material temperature reaches 190 to 200 DEG C, and charging the argon or nitrogen until the pressure reaches 30kpa to 80kpa; heating the annealing furnace to 280 DEG C, performing heat preserving, and vacuumizing the annealing furnace to less than 0.1333pa after the material temperature reaches 250 to 260 DEG C; and charging the argon into the annealing furnace until the pressure in the furnace reaches 103kpa to 130kpa, heating the annealing furnace to 500 to 600 DEG C, performing heat preserving, rapidly cooling the annealing furnace to 50 to 100 DEG C when the material temperature reaches 500 to 560 DEG C, and discharging a material out of the annealing furnace after the material is cooled to less than 150 DEG C. The method has advantages that the problems that the vacuum annealing production period is long and the aluminum foil is secondarily oxidized and polluted when the aluminum foil is oxidized and annealed at a high temperature as well as the problems that the thickness of an aluminum foil oxidized film is excessively thick and the aluminum foil oxidiezed film is non-uniformly distributed because the nitrogen reacts with the aluminum foil for a long period of time at the high temperature when the aluminum foil is annealed in the nitrogen atmosphere can be solved; the production efficiency is greatly improved, and the oxidized film on the surface of the aluminum foil is thin and uniformly distributed, so that the specific capacitance is increased, and the specific capacitance deviation is reduced.
Description
Technical field
The present invention relates to a kind of finished products method of electrolytic condenser high voltage anode aluminum foil, belong to non-ferrous metal technical field of thermal treatment.
Background technology
Electrolytic condenser high voltage anode aluminum foil becomes electrode foil after being changed into by corrosion, is the main raw material(s) making aluminium electrolutic capacitor.The surface property of electrolytic condenser high voltage anode aluminum foil, distribution and { 100 } plane texture occupation rate etc. directly will affect the height of electrode foil capacity and the stable of performance.And the finished products of electrolytic condenser high voltage anode aluminum foil is the critical process affecting aluminium foil surface performance, distribution and { 100 } plane texture occupation rate.
The current domestic method for annealing mainly taked has vacuum annealing and nitrogen (N
2) annealing.In this regard; there is China Patent No. to be CN03108574.1 " middle high-pressure electronics aluminum foil finished product method for annealing in a vacuum furnace " and CN03109901.7 " method for quenching high voltage electronic aluminum foil finished products ", disclose vacuum annealing method and protective gas respectively with nitrogen (N
2) be main method for annealing.But, the intelligent development more and more higher along with electronics, electrical equipment industry and frequency transformer, LED illumination, photovoltaic, automobile and other industries energy-conserving and environment-protective future development are to the demand of aluminium electrolutic capacitor heavy body, high stability, existing finished products production technology decapacitation ensures that outside { 100 } plane texture occupation rate, visual appearance and surface corrosion characteristics etc. cannot meet service requirements all.In industrialized production, mainly production cycle long-acting rate is low for the drawback of vacuum annealing, and high temperature section more than 500 DEG C because of poor without convection of air anneal uniformity, oxidative phenomena is serious in addition, the partially thick and heterogeneity of surface oxidation film thickness.Protective gas nitrogen (N
2) annealing shortens annealing time, and improves the homogeneity of annealing to a certain extent, but problem is on the one hand at long-time high temperature section more than 500 DEG C nitrogen (N
2) chemical reaction can be there is with aluminium (Al), form aluminium nitride (AlN); Be foreign matter such as aluminium foil attachment itself aqueous vapor, greasy dirt etc. on the other hand, fail to discharge in time, in annealing process, cause aluminium foil secondary oxidation, pollution, make aluminium foil surface quality deteriorated.Above problem, in corrosion formation process, all causes that ratio capacitance is on the low side and deviation is larger.
Summary of the invention
The object of the invention is the series of problems existed in above-mentioned method for annealing for electrolytic condenser high voltage anode aluminum foil, under a kind of prerequisite ensureing { 100 } plane texture occupation rate being provided, not only can shortening annealing time but also the partially thick and finished products method of the electrolytic condenser high voltage anode aluminum foil of inhomogenous problem of aluminum foil annealing lack of homogeneity, surface film oxide can have been improved.
The technical scheme taked that the present invention solves the problems of the technologies described above comprises the steps:
(1) annealing furnace is evacuated to lower than below 0.1333pa, after namely reaching high vacuum, is filled with argon gas (Ar) or nitrogen (N
2) within the scope of 30kpa ~ 80kpa;
(2) furnace temperature rises to 200 ~ 240 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 190 ~ 200 DEG C, is filled with argon gas (Ar) or nitrogen (N
2) within the scope of 30kpa ~ 80kpa;
(3) furnace temperature rises to 260 ~ 300 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 250 ~ 260 DEG C; (4) be filled with argon gas (Ar) in stove within the scope of 103kpa ~ 130kpa, furnace temperature rises to 500 ~ 600 DEG C of insulations, and material temperature reaches 500 ~ 560 DEG C;
(5) furnace temperature is quickly cooled to 40 ~ 100 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
Argon gas (Ar) in described step (1), (2), (3), (4) reaches the high-purity argon gas (Ar) of volume ratio more than 99.999% for purity; Nitrogen (N
2) reach the high pure nitrogen (N of volume ratio more than 99.999% for purity
2);
The present invention is pumping high vacuum in stove in step (1), is to reduce oxygen level as far as possible, avoids the aluminium foil oxidation when annealing.Be filled with argon gas (Ar) or nitrogen (N
2) within the scope of 30kpa ~ 80kpa, be to allow aluminium foil after the heating, the foreign matter such as aqueous vapor, greasy dirt of aluminium foil attachment itself is easy to volatilize from aluminium foil surface.If furnace pressure is on the low side, though it is long for heat-up time to be easy to volatilization, if furnace pressure is higher, though short volatilization heat-up time effect is bad.
The present invention adopts the mode of differential heating in step (2), is to shorten heat-up time.Aluminium foil vacuumizes ventilation below 200 DEG C, because aluminium foil oxidizing reaction can not occur at this temperature, and the aqueous vapor etc. of aluminium foil surface attachment is all volatilized, adopt the mode vacuumized the furnace atmosphere having aqueous vapor etc. to pollute all to be replaced, guarantee that aluminium foil is not oxidized in continuation heat-processed.
The present invention again vacuumizes ventilation in step (3) aluminium foil below 260 DEG C, is that the foreign matters such as the cold-rolling oil of surface attachment in producing because of aluminium foil can all volatilize at this temperature, avoids aluminium foil in continuation heat-processed by secondary pollution.
The present invention is filled with argon gas (Ar) within the scope of 103kpa ~ 130kpa in step (4) high temperature section, is to guarantee that stove is interior higher than normal atmosphere, allows extraneous air cannot enter stove internal oxidition aluminium foil, can accelerate rate of heating again; Do not adopt nitrogen (N
2), be avoid nitrogen (N
2) lower and aluminium foil surface reacts for a long time at high temperature under high pressure; In addition, furnace pressure is unsuitable too high, and too high then argon gas (Ar) consumes comparatively large, and cost increases, and causes certain influence to equipment.
The present invention can preferentially adopt nitrogen (N in step (1), (2), (3)
2), because nitrogen cost is more cheap.
Advantage of the present invention is: solve vacuum annealing production cycle length, high temperature oxidation; Aluminium foil attachment aqueous vapor, greasy dirt etc. anneal time to aluminium foil secondary oxidation, pollution; And nitrogen (N
2) annealing time high temperature long-time section nitrogen (N
2) react with aluminium foil, make that aluminum foil oxidation film thickness is partially thick, the first-class a series of bad problem of skewness.The utilization of the method, makes production efficiency significantly promote, aluminium foil surface oxide film is thin and be evenly distributed, thus promotes ratio capacitance, reduces ratio capacitance deviation.
Embodiment
Embodiment one: carry out as follows:
(1) annealing furnace is evacuated to below 0.1333pa, is filled with nitrogen (N
2) to 60kpa;
(2) furnace temperature rises to 240 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 200 DEG C, is filled with nitrogen (N
2) to 60kpa;
(3) furnace temperature rises to 280 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 250 DEG C;
(4) be filled with argon gas (Ar) in stove to 105kpa, furnace temperature rises to 580 DEG C of insulations, and material temperature reaches 530 DEG C;
(5) furnace temperature is quickly cooled to 100 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
Embodiment two: carry out as follows:
(1) annealing furnace is evacuated to below 0.1333pa, is filled with argon gas (Ar) to 35kpa;
(2) furnace temperature rises to 230 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 200 DEG C, is filled with argon gas (Ar) to 35kpa;
(3) furnace temperature rises to 300 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 260 DEG C;
(4) be filled with argon gas (Ar) in stove to 110kpa, furnace temperature rises to 600 DEG C of insulations, and material temperature reaches 540 DEG C;
(5) furnace temperature is quickly cooled to 80 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
Embodiment three: carry out as follows:
(1) annealing furnace is evacuated to below 0.1333pa, is filled with nitrogen (N
2) to 75kpa;
(2) furnace temperature rises to 240 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 190 DEG C, is filled with nitrogen (N
2) to 75kpa;
(3) furnace temperature rises to 300 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 260 DEG C;
(4) be filled with argon gas (Ar) in stove to 115kpa, furnace temperature rises to 560 DEG C of insulations, and material temperature reaches 520 DEG C;
(5) furnace temperature is quickly cooled to 100 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
Comparative example one: original vacuum annealing method carries out as follows:
(1) annealing furnace is evacuated to below 0.1333pa, and furnace temperature rises to 300 DEG C of insulations, and material temperature reaches 250 DEG C;
(2) furnace temperature rises to 550 DEG C of insulations, and material temperature reaches 520 DEG C;
(3) furnace temperature is quickly cooled to 100 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
Comparative example two: original protective gas nitrogen (N
2) method for annealing carries out as follows:
(1) annealing furnace is evacuated to below 0.1333pa, is filled with nitrogen (N
2) to 45kpa;
(2) furnace temperature rises to 300 DEG C of insulations, and material temperature reaches 250 DEG C;
(3) furnace temperature rises to 550 DEG C of insulations, and material temperature reaches 530 DEG C;
(4) furnace temperature is quickly cooled to 80 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
The aluminium foil produced above-mentioned method for annealing carries out the detection of { 100 } plane texture occupation rate and corrosion changes into rear horizontal stroke, longitudinal detection of ratio capacitance deviation and the statistics of production efficiency, and concrete outcome is as following table:
In the present invention, the measuring method of { 100 } plane texture occupation rate adopts " YS/T455.8-2007 aluminium foil test method " the 8th part: the measuring method of aluminium foil cubic texture content detects.
In the present invention, the testing method of specific volume adopts the measuring method of ratio capacitance in " SJ/T 11140-2012 electrode foil for aluminum electrolytic capacitors " to carry out the mensuration of 520V ratio capacitance.
From above-mentioned enforcement, comparative example, by the finished products method of electrolytic condenser high voltage anode aluminum foil of the present invention under the prerequisite ensureing { 100 } plane texture occupation rate, production efficiency can be increased substantially, avoid the secondary oxidation on aluminium foil surface in annealing process, pollution, reduce aluminium foil surface oxide thickness and uneven distribution problem, reduce ratio capacitance deviation while promoting ratio capacitance, meet the performance requriements that market is more and more higher to aluminium electrolutic capacitor.
Claims (2)
1. a finished products method for electrolytic condenser high voltage anode aluminum foil, is characterized in that: comprise the steps:
(1) annealing furnace is evacuated to lower than below 0.1333pa, after namely reaching high vacuum, is filled with argon gas (Ar) or nitrogen (N
2) within the scope of 30kpa ~ 80kpa;
(2) furnace temperature rises to 200 ~ 240 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 190 ~ 200 DEG C, is filled with argon gas (Ar) or nitrogen (N
2) within the scope of 30kpa ~ 80kpa;
(3) furnace temperature rises to 260 ~ 300 DEG C of insulations, and material temperature is evacuated to below 0.1333pa after reaching 250 ~ 260 DEG C;
(4) be filled with argon gas (Ar) in stove within the scope of 103kpa ~ 130kpa, furnace temperature rises to 500 ~ 600 DEG C of insulations, and material temperature reaches 500 ~ 560 DEG C;
(5) furnace temperature is quickly cooled to 40 ~ 100 DEG C, makes material temperature be cooled to less than 150 DEG C and comes out of the stove.
2. the finished products method of a kind of electrolytic condenser high voltage anode aluminum foil according to claim 1, is characterized in that: the argon gas (Ar) in described step (1), (2), (3), (4) reaches the high-purity argon gas (Ar) of volume ratio more than 99.999% for purity; Nitrogen (N
2) reach the high pure nitrogen (N of volume ratio more than 99.999% for purity
2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410787982.3A CN104451481A (en) | 2014-12-19 | 2014-12-19 | Finished product annealing method of high voltage anode aluminum foil for electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410787982.3A CN104451481A (en) | 2014-12-19 | 2014-12-19 | Finished product annealing method of high voltage anode aluminum foil for electrolytic capacitor |
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|---|---|
| CN104451481A true CN104451481A (en) | 2015-03-25 |
Family
ID=52898220
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| CN201410787982.3A Pending CN104451481A (en) | 2014-12-19 | 2014-12-19 | Finished product annealing method of high voltage anode aluminum foil for electrolytic capacitor |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109671569A (en) * | 2018-12-14 | 2019-04-23 | 扬州宏远电子股份有限公司 | A kind of heat treatment method improving Waste Acid From Hua Cheng Foil specific volume |
| CN110904397A (en) * | 2019-11-27 | 2020-03-24 | 新疆众和股份有限公司 | Multi-stage annealing process of high-voltage anode aluminum foil for electrolytic capacitor |
| CN111876701A (en) * | 2020-06-29 | 2020-11-03 | 河南科源电子铝箔有限公司 | Finished product annealing method for improving cubic texture of high-voltage anode electronic aluminum foil |
| CN114085096A (en) * | 2021-11-17 | 2022-02-25 | 鄂尔多斯市紫荆创新研究院 | Annealing method of lithium cobaltate positive electrode target material and lithium cobaltate positive electrode target material |
| CN115725915A (en) * | 2022-12-01 | 2023-03-03 | 乳源县立东电子科技有限公司 | Optical foil crystal grain control method and preparation method of anode foil for electrolytic capacitor |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109671569A (en) * | 2018-12-14 | 2019-04-23 | 扬州宏远电子股份有限公司 | A kind of heat treatment method improving Waste Acid From Hua Cheng Foil specific volume |
| CN110904397A (en) * | 2019-11-27 | 2020-03-24 | 新疆众和股份有限公司 | Multi-stage annealing process of high-voltage anode aluminum foil for electrolytic capacitor |
| CN111876701A (en) * | 2020-06-29 | 2020-11-03 | 河南科源电子铝箔有限公司 | Finished product annealing method for improving cubic texture of high-voltage anode electronic aluminum foil |
| CN114085096A (en) * | 2021-11-17 | 2022-02-25 | 鄂尔多斯市紫荆创新研究院 | Annealing method of lithium cobaltate positive electrode target material and lithium cobaltate positive electrode target material |
| CN115725915A (en) * | 2022-12-01 | 2023-03-03 | 乳源县立东电子科技有限公司 | Optical foil crystal grain control method and preparation method of anode foil for electrolytic capacitor |
| CN115725915B (en) * | 2022-12-01 | 2023-11-17 | 乳源县立东电子科技有限公司 | Optical foil grain control method and preparation method of anode foil for electrolytic capacitor |
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Application publication date: 20150325 |