CN103295783A - Method for manufacturing electrolytic capacitor - Google Patents
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- CN103295783A CN103295783A CN2013101819557A CN201310181955A CN103295783A CN 103295783 A CN103295783 A CN 103295783A CN 2013101819557 A CN2013101819557 A CN 2013101819557A CN 201310181955 A CN201310181955 A CN 201310181955A CN 103295783 A CN103295783 A CN 103295783A
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Abstract
The invention relates to a method for manufacturing an electrolytic capacitor, in particular to a method for manufacturing an electrolytic capacitor which is high in breakdown voltage, volumetric efficiency (relative maximum capacitance per unit volume), insulation resistance and corrosion resistance, long in service life and low in leakage current. The method is used for manufacturing the electrolytic capacitor by means of sectioned electrochemical oxidation. The method includes steps of metal anode block forming and sintering, electrochemical forming, medium oxidation film cleaning and heat treatment, freezing, cleaning, coating, electric welding and packaging, and the like. The method has the advantages that the thickness of an internal medium oxidation film can be effectively reduced, a medium oxidation film of an outer layer of an anode block of the porous capacitor is thick, and the medium oxidation film inside a core of the capacitor is thin relatively, so that the voltage resistance of a product is guaranteed, the breakdown probability of the capacitor is effectively reduced, and the volumetric efficiency of the product can be greatly improved.
Description
Technical field
The present invention relates to a kind of manufacture method of electrolytic capacitor, relate in particular to a kind of employing segmentation electrochemical oxidation and form and have puncture voltage and volume efficiency (unit volume reaches relative maximum capacitance) is high, the life-span is long, insulation resistance is high, leakage current is little, the manufacture method of corrosion-resistant strong electrolytic capacitor.
Background technology
Electrolytic capacitor is one of important components and parts of electronic technology, and along with the fast development of electronic technology, fields such as Aeronautics and Astronautics, communication and microelectronics require the electrolytic capacitor microminiaturization, capacitance is big, the life-span is long.A lot of manufacturers adopt various measures to improve the inner space utilance of capacitor, use specific volume etc. as using high specific capacitance tantalum powder to produce, suitably reduce anode tantalum piece sintering temperature or changing sintering curre to improve the tantalum powder.The enforcement of these measures, especially the application of high specific capacitance tantalum powder makes the expansion effect of capacitor static capacity the most remarkable, but must select lower formation voltage or the tantalum powder of higher specific volume, though improved the volume efficiency of product, reduce qualification rate and the reliability of product.A large amount of failure analysis data and DPA analyze data and show, it all is that the not enough or oxide-film self-defect of the dielectric oxide film anti-pressure ability on metal derby surface of sintering causes that the product leakage current is big, breakdown potential is forced down and caused that electrolytic capacitor lost efficacy.
In order to improve the performance of dielectric oxide film, patent U.S.Pat.No.5,716,511, patent U.S.Pat.No.2,288,889, patent EP1591,564, A2 proposes the electrolyte of preparation high conductivity, can effectively improve the quality of dielectric oxide film, improve reliability of products, but the conductivity of raising solution can make its flash over voltage reduce.
Summary of the invention
In order to overcome above technical problem, the present invention takes following technical scheme:
A kind of manufacture method of electrolytic capacitor may further comprise the steps:
Step 1: the moulding of metal anode piece and sintering;
Step 2: carry out electrochemical oxidation and form dielectric oxide film in the electrolyte of being made up of the mixed solution of water, ethylene glycol and/or polyethylene glycol and phosphoric acid and/or sulfuric acid, the formation voltage of electrochemical oxidation is 1.3～3.5 times of rated voltage;
Step 3: the cleaning of dielectric oxide film and heat treatment;
Step 4: it is freezing to place cryogenic temperature to be that-20～-2 ℃ freezing liquid carries out anode block, and cooling time is 24～96 hours;
Step 5: with the electrolyte that freezing anode block places-15～-3 ℃ the mixed solution by deionized water, ethylene glycol and/or polyethylene glycol, phosphoric acid and/or sulfuric acid to form, formation voltage is 3～5 times of rated voltage;
Step 6: anode block is placed-3～0 ℃ deionized water 3～10 hours, the inner ice cube of capacitor core is separated out;
Step 7: slowly heating improves solution temperature, and the formation groove that capacitor core perhaps will be housed places normal temperature environment, and capacitor core surface ice cube melts;
Step 8: antianode piece surface is cleaned, and removing impurity such as remaining PO-4, and heat-treats in hot environment, and heat treatment time is 0.5～5 hour;
Step 9: the lining of catholyte;
Step 10: be covered with electrolytical capacitor core surface coated graphite layer and silver slurry layer successively, and spot welding, bonding, group frame and mold pressing encapsulation, form final products after the shaping, and test its electrical property.
Described in the described step 2 in the electrolyte volume ratio of ethylene glycol and/or polyethylene glycol be 15～85%, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the described electrolyte, the volume ratio of water is 10～85%, the conductivity of described electrolyte is 0.3～65mS/cm, and the temperature of described electrolyte is 45～95 ℃.
Described in the described step 2 in the electrolyte volume ratio of ethylene glycol and/or polyethylene glycol be 20～80%, phosphoric acid and/or sulfuric acid volume ratio are 0.05～5% in the described electrolyte, the conductivity of described electrolyte is 3～50mS/cm, and the temperature of described electrolyte is: 55～85 ℃.
Described in the described step 2 in the electrolyte volume ratio of ethylene glycol be 30～75%.
The formation voltage of electrochemical oxidation described in the described step 2 is 1.5～3 times of rated voltage.
Freezing liquid described in the described step 4 is the aqueous solution of ionized water, organic salt and/or inorganic salts, and described cryogenic temperature is-15～-5 ℃, and described cooling time is 36～72 hours.
Freezing liquid described in the described step 4 is ionized water.
The volume ratio of ethylene glycol is 25～85% in the electrolyte described in the described step 5, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the described electrolyte, the volume ratio of described deionized water is 15～75%, the conductivity of described electrolyte is 0.5～65mS/cm, temperature in the described electrolyte is-10～-3 ℃, and the formation voltage of described electrochemical oxidation formation dielectric oxide film is 3～5 times of rated voltage.
The volume ratio of ethylene glycol is 30～80% in the electrolyte described in the described step 5, described in the electrolyte phosphoric acid/sulfuric acid volume ratio be 0.05～5%; The conductivity of described electrolyte is 5～50mS/cm; Temperature in the described electrolyte is-9～5 ℃; The formation voltage of described electrochemical oxidation formation dielectric oxide film is 3.5～5 times of rated voltage.
The volume ratio of ethylene glycol is for being 35～75% in the electrolyte described in the described step 5.
Compared with prior art, the present invention is under the prerequisite that guarantees anode block outer surface oxide film thickness, the method that adopts the segmentation electrochemical oxidation to form has reduced the thickness of interior media oxide-film effectively, both made that the outer field dielectric oxide film of porousness anode block was thicker, and the dielectric oxide film of electrolytic capacitor in-core portion is thinner relatively, thereby guaranteed the product withstand voltage properties, effectively reduced the breakdown probability of capacitor, can improve the volume efficiency of product simultaneously again greatly.
Embodiment
Valve metal such as tantalum, aluminium and niobium etc. are fit to do the solid electrolytic capacitor of high-specific surface area very much.The dielectric layer of electrolytic capacitor generally is to form one deck dielectric oxide film on the surface of valve metal by electrochemical method, this oxide-film has conclusive effect to electrical property and stability, the reliability aspect of capacitor, particularly to the high-voltage large-capacity capacitor.In general, the solid electrolytic capacitor structure comprise through anodization form dielectric membranous layer by in the valve metals such as tantalum, niobium, aluminium, titanium one or more mixture or the porousness anode pellet made of valve metal oxides, at the metal oxide semiconductor of dielectric membranous layer surface preparation or the electric conductive polymer electrolyte as electrolytic capacitor, form capacitor by carbon-coating, conductive metal layer, both positive and negative polarity lead-out wire then, form complete capacitor by encapsulation or insulating coating at last.
Be example with the tantalum electrolytic capacitor, the tantalum fuse of compression moulding is a porous structure, in the incipient stage that oxidation forms, the oxidation that the electrochemical process that anode block boosts by constant current in electrolyte continues, because the porous design feature of anode block, electrolyte can be in the internal flow of anode block, thereby causes that anode block generates heat in oxidizing process.And oxidizing process is continuous, and the electrolyte of heating just is not easy to flow out from the inside of anode block.On the contrary, the temperature of electrolyte is along with oxidizing process continues to raise.Obviously, have the gradient of a temperature between the interface of the dielectric oxide film that the electrolyte of heating and electrochemical oxidation form, along with the increase of temperature gradient, the electrolyte of high temperature just produces certain destruction to dielectric oxide film.Therefore, the electrolyte of high temperature is the cut that causes dielectric oxide film surface and anode block inside, crackle, and crystallization and other flaw play main cause.
In addition, the quality of puncture voltage and dielectric oxide film and electrolytic conductivity have very big relation, and electrical conductivity of solution is determined by the attribute of solution and the concentration of effects of ion, and the puncture voltage of electrolyte must be higher than the formation voltage of the anode block of oxidation.The conductivity that increases electrolyte just can reduce the puncture voltage of anode oxide film.On the other hand, if the conductivity of solution is too low, will produce a lot of electrolysis heat on anode block, thereby cause " ashing " of anode block, the puncture voltage of dielectric oxide film is relatively low, and reduces the performance of dielectric oxide film." ashing " is not wish the phenomenon that occurs in the tantalum anode forming process, and particularly to the anode block of high pressure, " ashing " is easy to cause the crystallization of anode oxide film, produces higher relatively leakage current.Therefore, the control of the relevant parameter of the composition of electrolyte and forming process can effectively suppress the generation of " ashing ".But low conductivity electrolyte can make that also forming voltage reduces, and electrolytic acid cleaning oxydation process should not be controlled.
The present invention proposes the method that the segmentation electrochemical oxidation forms dielectric oxide film.Existing relatively patent, the present invention does not advocate and improves the electrochemical oxidation that electrical conductivity of solution is realized high die pressing product, but with the temperature of traditional electrolyte by change solution, forms the thickness that environmental condition increases the dielectric oxide film layer in other words.Its implementation process comprises three parts: at first, and according to the technology formation dielectric oxide film of routine.Adopt the mixed solution of water, organic acid and inorganic acid, usually the mixed solution of water, ethylene glycol and/or polyethylene glycol and phosphoric acid and/or sulfuric acid is the electrolyte that generally uses in the electrochemistry forming process, in the mixed solution of phosphoric acid and/or sulfuric acid and deionized water, add ethylene glycol, the volume ratio of ethylene glycol is 15～85%, what relatively be fit to is 20～80%, preferred 30～75%.Phosphoric acid and/or sulfuric acid volume ratio are 0.01～10%, and be preferred 0.05～5%, and the volume ratio of water is 10～85%, and the conductivity of electrolyte is 0.3～65mS/cm, preferred 3～50mS/cm; Formation temperature is 45～95 ℃, preferred 55～85 ℃; Formation voltage is 1.3～3.5 times of rated voltage, preferred 1.5～3 times.Current density is 2～50mA/g.The electrochemistry forming process was boosted under particular current before this, dielectric oxide film thickens along with the rising of voltage, growth rate is 1.7～2.3nm/V, voltage remains unchanged after being raised to given voltage, carry out constant-pressure drop stream again, the output current of power supply is more and more littler, means dielectric oxide film, the dielectric that is electrolytic capacitor becomes more and more finer and close, and conductivity worse and worse.Secondly, it is freezing anode block to be placed the aqueous solution of-20～-2 ℃ deionized water, organic salt and inorganic salts carry out, and cooling time is 24～96 hours, guarantees that anode block inside is freezing fully, and namely the hole of anode block inside is all by the ice cube shutoff.At last, freezing anode block is placed-10～0 ℃ electrolyte, use the electrolyte identical with the phase I, formation voltage is 3～5 times of rated voltage.The electrochemistry forming process was boosted under particular current before this, and the surface dielectric oxide-film thickens along with the rising of voltage, and voltage remains unchanged after being raised to given voltage, carried out constant-pressure drop stream again.Electrochemical oxidation process in the low temperature environment can only take place on the surface of anode block or near surperficial very little scope, because the hole of tantalum in-core portion is stopped up by freezing back, electrolyte can not flow in tantalum in-core portion, can only electrochemical reaction take place on the surface of anode block.And the formation voltage of second stage will exceed 1.5～5 times of phase I formation voltages, thereby form the abundant dielectric oxide film of one deck in the tantalum core surface, and oxide-film is to form in the solution of low temperature and low conductivity, so just avoided because the too hot thermic crystallization that causes of electrolyte and since field intensity cause too greatly cause crystallization.Therefore, the flaw on the dielectric oxide film surface that skin is abundant will significantly reduce, thereby improve the puncture voltage of capacitor, reduce leakage current, and in addition, the dielectric oxide film of internal layer is thinner relatively, thereby has increased capacity, has improved the volume efficiency of capacitor.Of paramount importancely be; abundant dielectric oxide film can be resisted very big surge voltage and electric current, powerful mechanical shock effect, thus can protect the dielectric oxide film of internal layer well; greatly reduce the probability that capacitor lost efficacy, prolonged the useful life of capacitor.
With the valve metal tantalum, niobium and niobium oxide are example, and the detailed preparation process of this method may further comprise the steps:
Step 1: the moulding of metal anode piece and sintering;
Step 2: by water, carry out electrochemical oxidation in the electrolyte that the mixed solution of ethylene glycol and/or polyethylene glycol and phosphoric acid and/or sulfuric acid is formed and form dielectric oxide film, the formation voltage of electrochemical oxidation is 1.3～3.5 times of rated voltage, preferred 1.5～3 times, the volume ratio of ethylene glycol and/or polyethylene glycol is 15～85% in the electrolyte, preferably 20～80%, the volume ratio of preferred ethylene glycol is 30～75%, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the electrolyte, preferred 0.05～5%, the volume ratio of water is 10～85%, the conductivity of electrolyte is 0.3～65mS/cm, preferred 3～50mS/cm, the temperature of described electrolyte is 45～95 ℃, preferred 55～85 ℃.
Step 3: the cleaning of dielectric oxide film and heat treatment;
Step 4: it is freezing to place cryogenic temperature to be that freezing liquid that-20～-2 ℃ the aqueous solution by ionized water, organic salt and/or inorganic salts is formed carries out anode block, and cooling time is 24～96 hours; Preferred-15～-5 ℃ of described cryogenic temperature, preferred 36～72 hours of described cooling time, described freezing liquid preferred ion water.
Step 5: with the electrolyte that freezing anode block places-15～-3 ℃ the mixed solution by deionized water, ethylene glycol and/or polyethylene glycol, phosphoric acid and/or sulfuric acid to form, formation voltage is 3～5 times of rated voltage; The volume ratio of ethylene glycol is 25～85% in the electrolyte, preferably 30～80%, and preferred 35～75%, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the described electrolyte, preferred 0.05～5%; The volume ratio of described deionized water is 15～75%, and the conductivity of described electrolyte is 0.5～65mS/cm, preferred 5～50mS/cm; Temperature in the described electrolyte is-10～-3 ℃, and preferred-9～5 ℃, the formation voltage of described electrochemical oxidation formation dielectric oxide film is 3～5 times of rated voltage, preferred 3.5～5 times.
Step 6: anode block is placed-3～0 ℃ deionized water 3～10 hours, the inner ice cube of capacitor core is separated out;
Step 7: slowly heating improves solution temperature, and the formation groove that capacitor core perhaps will be housed places normal temperature environment, and capacitor core surface ice cube melts;
Step 8: antianode piece surface is cleaned, and removing impurity such as remaining PO-4, and heat-treats in hot environment, and heat treatment time is 0.5～5 hour;
Step 9: the lining of catholyte;
Step 10: be covered with electrolytical capacitor core surface coated graphite layer and silver slurry layer successively, and spot welding, bonding, group frame and mold pressing encapsulation, form final products after the shaping, and test its electrical property.
Embodiment one
The preparation of anode block
Be example with the tantalum, add a certain amount of adhesive during commercial dedicated capacitor is Ta powder used, moulded section is of a size of 3.1 * 0.9 * 4.6(mm) tantalum piece, the high-temperature vacuum sintering makes the adhesive volatilization, and make the tantalum powder that effective adhesive be arranged, the sintering specific volume is 36,600CV/g, and the tantalum piece behind these sintering is used in following examples.
Embodiment 1
It is 0.3% 75 ℃ deionized water, ethylene glycol and phosphoric acid solution that tantalum piece behind the sintering is placed concentration, adds the voltage of voltage regulation of 30V, by electrochemical reaction on tantalum piece surface with innerly form unbodied Ta
2O
5Medium.The tantalum piece that generates dielectric layer is immersed carry out freezingly in the deionized water of (20～-2) ℃, cooling time is 48 hours.Freezing anode block placed-8 ℃ deionized water, ethylene glycol and phosphoric acid solution, forming voltage is that rated voltage is 3.5 times (56V), carry out the electrochemical oxidation process that constant current is boosted and constant-pressure drop flows, form abundant dielectric oxide film on tantalum anode piece surface.The tantalum anode piece is placed-3 ℃ of aqueous solution freezing 4 hours, placed normal temperature environment again 1 hour.Boil in the deionized water with 95 ℃ of anode block immersions and wash 2 hours, and heat-treat 320 ℃ hot environment, heat treatment time is 0.5 hour.
Make conducting polymer or manganese dioxide solid electrolyte on the anode block surface, again at electrolytical surface-coated graphite and silver slurry, carry out spot welding, bonding and mold pressing encapsulation then.
At last the electrical quantity of capacitor is measured.Test result sees Table one.
Comparative examples one
Anode block behind one group of sintering is carried out moulding and sintering according to embodiment one identical process conditions, it is 0.3% 75 ℃ deionized water, ethylene glycol and phosphoric acid solution that tantalum piece behind the sintering is placed concentration, the direct voltage that adds 56V, carry out the electrochemical oxidation process that constant current is boosted and constant-pressure drop flows, at tantalum anode piece surface and the inner identical dielectric oxide film of thickness that forms.Anode block placed to boil with 95 ℃ deionized water wash 2 hours, and heat-treated 0.5 hour 320 ℃ hot environment.
Make conducting polymer or manganese dioxide solid electrolyte on anode block surface, again at electrolytical surface-coated graphite and silver slurry, carry out bonding, spot welding and mold pressing encapsulation then.At last the electrical quantity of capacitor is measured.Concrete data see Table 1.
Table 1
| Sample | Generation type | Capacity (μ F) | ESR(mΩ) | Leakage current (μ A) |
| Experiment 1 | Segmentation forms | 65～73 | 23～31.5 | 0.7～1.6 |
| Contrast 1 | Once form | 42～47 | 28.5～40 | 0.8～1.6 |
Comparative examples two
Anode block behind one group of sintering is carried out moulding and sintering according to embodiment one identical process conditions, it is 0.3% 75 ℃ deionized water, ethylene glycol and phosphoric acid solution that tantalum piece behind the sintering is placed concentration, the direct voltage that adds 48V, carry out the electrochemical oxidation process that constant current is boosted and constant-pressure drop flows, at tantalum anode piece surface and the inner identical dielectric oxide film of thickness that forms.Anode block was washed 2 hours with 95 ℃ deionization poach, and heat-treated 0.5 hour 320 ℃ hot environment.
Make conducting polymer or manganese dioxide solid electrolyte on anode block surface, again at electrolytical surface-coated graphite and silver slurry, carry out bonding, spot welding and mold pressing encapsulation then.At last the electrical quantity of capacitor is measured.Concrete data see Table 2.
Comparative examples three
Anode block behind one group of sintering is carried out moulding and sintering according to embodiment one identical process conditions, it is 0.5% 65 ℃ deionized water, ethylene glycol and phosphoric acid solution that tantalum piece behind the sintering is placed concentration, the direct voltage that adds 56V, carry out the electrochemical oxidation process that constant current is boosted and constant-pressure drop flows, at tantalum anode piece surface and the inner identical dielectric oxide film of thickness that forms.Anode block placed to boil with 95 ℃ deionized water wash 2 hours, and heat-treated 0.5 hour 320 ℃ hot environment.
Make conducting polymer or manganese dioxide solid electrolyte on anode block surface, again at electrolytical surface-coated graphite and silver slurry, carry out bonding, spot welding and mold pressing encapsulation then.At last the electrical quantity of capacitor is measured.Concrete data see Table 2.
Table 2
From top comparative examples as can be seen, the dielectric of electrolytic capacitor is an of paramount importance part in the electrolytic capacitor, and it has direct influence to each electrical quantity of capacitor, and is to cause the main factor that capacitor lost efficacy.Reduce forming voltage, each electrical quantity generation marked change of capacitor, wherein the variation of leakage current is the most obvious, increases the conductivity of solution, also causes the significantly variation of capacitor electrode parameter.And the capacitor that the present invention makes forms back test electrical quantity, and capacity increases more than 20%, and leakage current and loss are also considerably little.Therefore, the method that adopts the segmentation electrochemical oxidation to form improves the volume efficiency of electrolytic capacitor effectively, has improved the high temperature resistant and voltage endurance of electrolytic capacitor, effectively reduces the breakdown probability of capacitor, and the electrical quantity of the electrolytic capacitor of made is all very good.
This shows that the electrolytic capacitor that adopts the method for above segmentation electrochemical oxidation to make has puncture voltage and volume efficiency height, the life-span is long, insulation resistance is high, leakage current is little, corrosion-resistant advantage such as strong.
Claims (10)
1. the manufacture method of an electrolytic capacitor is characterized in that, may further comprise the steps:
Step 1: the moulding of metal anode piece and sintering;
Step 2: carry out electrochemical oxidation and form dielectric oxide film in the electrolyte of being made up of the mixed solution of water, ethylene glycol and/or polyethylene glycol and phosphoric acid and/or sulfuric acid, the formation voltage of electrochemical oxidation is 1.3～3.5 times of rated voltage;
Step 3: the cleaning of dielectric oxide film and heat treatment;
Step 4: it is freezing to place cryogenic temperature to be that-20～-2 ℃ freezing liquid carries out anode block, and cooling time is 24～96 hours;
Step 5: with the electrolyte that freezing anode block places-15～-3 ℃ the mixed solution by deionized water, ethylene glycol and/or polyethylene glycol, phosphoric acid and/or sulfuric acid to form, formation voltage is 3～5 times of rated voltage;
Step 6: anode block is placed-3～0 ℃ deionized water 3～10 hours, the inner ice cube of capacitor core is separated out;
Step 7: slowly heating improves solution temperature, and the formation groove that capacitor core perhaps will be housed places normal temperature environment, and capacitor core surface ice cube melts;
Step 8: antianode piece surface is cleaned, and removing impurity such as remaining PO-4, and heat-treats in hot environment, and heat treatment time is 0.5～5 hour;
Step 9: the lining of catholyte;
Step 10: be covered with electrolytical capacitor core surface coated graphite layer and silver slurry layer successively, and spot welding, bonding, group frame and mold pressing encapsulation, form final products after the shaping, and test its electrical property.
2. the manufacture method of electrolytic capacitor according to claim 1, it is characterized in that: described in the described step 2 in the electrolyte volume ratio of ethylene glycol and/or polyethylene glycol be 15～85%, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the described electrolyte, the volume ratio of water is 10～85%, the conductivity of described electrolyte is 0.3～65mS/cm, and the temperature of described electrolyte is 45～95 ℃.
3. the manufacture method of electrolytic capacitor according to claim 1, it is characterized in that: described in the described step 2 in the electrolyte volume ratio of ethylene glycol and/or polyethylene glycol be 20～80%, phosphoric acid and/or sulfuric acid volume ratio are 0.05～5% in the described electrolyte, the conductivity of described electrolyte is 3～50mS/cm, and the temperature of described electrolyte is: 55～85 ℃.
4. the manufacture method of electrolytic capacitor according to claim 1 is characterized in that: described in the described step 2 in the electrolyte volume ratio of ethylene glycol be 30～75%.
5. the manufacture method of electrolytic capacitor according to claim 1, it is characterized in that: the formation voltage of electrochemical oxidation described in the described step 2 is 1.5～3 times of rated voltage.
6. according to the manufacture method of the described electrolytic capacitor of claim 1, it is characterized in that: freezing liquid described in the described step 4 is the aqueous solution of ionized water, organic salt and/or inorganic salts, described cryogenic temperature is-15～-5 ℃, and described cooling time is 36～72 hours.
7. according to the manufacture method of the described electrolytic capacitor of claim 1, it is characterized in that: freezing liquid described in the described step 4 is ionized water.
8. according to the manufacture method of the described electrolytic capacitor of claim 1, it is characterized in that: the volume ratio of ethylene glycol is 25～85% in the electrolyte described in the described step 5, phosphoric acid and/or sulfuric acid volume ratio are 0.01～10% in the described electrolyte, the volume ratio of described deionized water is 15～75%, the conductivity of described electrolyte is 0.5～65mS/cm, temperature in the described electrolyte is-10～-3 ℃, and the formation voltage of described electrochemical oxidation formation dielectric oxide film is 3～5 times of rated voltage.
9. according to the manufacture method of the described electrolytic capacitor of claim 1, it is characterized in that: the volume ratio of ethylene glycol is 30～80% in the electrolyte described in the described step 5, described in the electrolyte phosphoric acid/sulfuric acid volume ratio be 0.05～5%; The conductivity of described electrolyte is 5～50mS/cm; Temperature in the described electrolyte is-9～5 ℃; The formation voltage of described electrochemical oxidation formation dielectric oxide film is 3.5～5 times of rated voltage.
10. according to the manufacture method of the described electrolytic capacitor of claim 1, it is characterized in that: the volume ratio of ethylene glycol is for being 35～75% in the electrolyte described in the described step 5.
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| CN105810459A (en) * | 2016-04-05 | 2016-07-27 | 电子科技大学 | Energizing process for preventing positive electrode crystallization of tantalum capacitor |
| CN111149183A (en) * | 2017-09-29 | 2020-05-12 | 松下知识产权经营株式会社 | Electrolytic capacitor |
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| CN111149183B (en) * | 2017-09-29 | 2022-04-26 | 松下知识产权经营株式会社 | Electrolytic capacitor |
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