CN101034629A - A making method for coiled solid electrolysis capacitor - Google Patents
A making method for coiled solid electrolysis capacitor Download PDFInfo
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Abstract
The invention discloses a coiling solid electrolytic capacitor manufacture method and the used polymer response solution and the method of controlling the polymer reaction rate. The method uses the mixing solution of capacitor core marinate oxidant and polymer monomer, or first soaks monomer then soak the oxidant solution or is opposite, carries on the polyreaction under the certain temperature environment, forms the high conductivity polymer level in the core interior; Through joins the alcoholtype or the amines solvent, and increase corrosion inhibitor in the polymer response solution, may effective control speed, also may reduce the corrosive action of the acid to aluminum foil; After the response accomplish cleaning and drying, and pouring with epoxy resin and polyimide resin, seal after the high temperature crosslinking. The invention method can make large capacity, the low impedance, low electric leakage current, high stablility capacitor.
Description
Technical field
The present invention relates to the preparation method of electrolytic capacitor, particularly a kind of high reliability, the low-impedance coiled solid electrolysis capacitor of high power capacity and manufacture method thereof.
Background technology
Because being extensive use of of high-frequency electronic equipment is more and more higher to the frequency characteristic requirement of capacitor.Though the electrolytic capacitor of traditional liquid state has its cheap advantage, but more and more can not satisfy the requirement of present high-frequency electronic equipment, moreover the traditional electrical electrolysis condenser has himself a lot of defective, causes its frequency characteristic and reliability poor, and the life-span is shorter relatively.In order to solve the deficiency of traditional electrical electrolysis condenser, people replace traditional electrolyte with the higher relatively material of conductivity, the material of these high conductivity comprises metal oxide manganese dioxide, brown lead oxide of semiconductor property etc., also just like the dicyano quinone---bismethane complex salt (being called for short TCNQ), be exactly the organic conductive polymeric material in addition, these are used respectively at Chinese patent (publication number: CN1032263A, CN1012236B, CN1702788A is described in CN1297569A).These high conductivity solid electrolyte materials (metal oxide, conducting polymer composite) at first are applied in the sheet type electrolytic capacitor, owing to jumbo demand, also applied in the winding type electrolytic capacitor afterwards.
The solid electrolytic capacitor of metal oxide semiconductor class mainly be salting liquid by soaking this metal by being heated to 200 ℃～300 ℃ decomposition on the capacitor thin slice, form the layer of semiconductor metal oxide film.The manufacture method of TCNQ class electrolytic capacitor is earlier TCNQ to be heated to molten condition, soaks capacitor body again, after fully soaking into capacitor body is taken out, the cooling back just on the capacitor metal oxide film and capacitor inside formed the TCNQ layer.
Because metal oxide semiconductor and TCNQ conductivity are limited, the conducting polymer composite that people are higher with conductivity also is applied in the electrolytic capacitor, thereby present solid electrolytic capacitor adopts conducting polymer (macromolecule) material more.For conducting polymer composite being applied in this class winding-type electrolytic capacitor, people develop the preparation method of multiple conducting polymer composite.Wherein modal is the method that adopts electropolymerization and chemical polymerization, at the inner conductive polyelectrolyte layer that forms solid of capacitor body.Electropolymerization is mainly used in the sheet type electrolytic capacitor, and chemical polymerization is mainly used in the winding-type electrolytic capacitor.Chemical polymerization is exactly to generate the solid conduction polyelectrolyte layers by immersion monomer solution that replaces back and forth and oxidizing agent solution or the method for directly soaking the mixed solution of monomer and oxidant at the capacitor internal-response.Certain patent US6454817B1 also mentions the solution that adopts the immersion conducting polymer composite and heats the method that makes solvent evaporates forms conducting polymer in capacitor body inside solid electrolyte layer then.
The monomer of conducting polymer composite mainly contains the pyrroles, aniline, thiophene, Ethylenedioxy Thiophene and their derivative.Oxidant mainly contains iron chloride, ferric sulfate, and p-methyl benzenesulfonic acid iron, ammonium persulfate, sodium peroxydisulfate, potassium permanganate, hydrogen peroxide etc., what its solvent adopted usually is water or alcohol, as methyl alcohol, ethanol, isopropyl alcohol, n-butanol or ethylene glycol etc.
In convoluted electrolytic capacitor, directly contact with Cathode Foil for fear of anode foils, with barrier film it is separated usually, and avoid the phenomenon that is short-circuited between them.The electrolytic capacitor of conventional liquid usually adopts be electrolytic paper as barrier film, and convoluted conducting polymer electrolytic capacitor will be made electrolytic paper high temperature cabonization usually and just can effectively reduce impedance.Carbonization treatment generally all will be more than 250 ℃, and such temperature may be damaged to some extent to dielectric oxide film, increase leakage current.The lead-out wire of capacitor body also can be therefore oxidized, makes that the wettability to scolder descends greatly when doing welding, and for overcoming this problem, people have adopted the strong silver-plated lead-in wire of non-oxidizability.Chinese patent (publication number: adopted nonwoven fabrics as barrier film CN1321322A), just avoided carbonisation for example.But the employing of these means all can cause the cost of capacitor to rise undoubtedly.
The conducting polymer composite that uses in the present Wound capacitor is in the majority with poly-Ethylenedioxy Thiophene (PEDT), monomer is Ethylenedioxy Thiophene (EDT), oxidant all is the alcoholic solution of p-methyl benzenesulfonic acid iron usually, because EDT costs an arm and a leg, and causes the electrolytic capacitor price of takeup type conducting polymer composite of today also higher.And less in the wound capacitor that the relatively low pyrroles of price uses, and performance is less than the winding type electrolytic capacitor of PEDT class.
No matter be chip or coiled electrolytic capacitor, the process that the cutting metal thin slice all can be arranged in manufacture process, formed undoubtedly at cut surface as the anode foils of electrolytic capacitor like this and do not had the conduction of oxide-film section, and the electrolytic capacitor of this type of conducting polymer composite, because conducting polymer composite is not an ionic conduction, dielectric oxide film to the metal surface does not have repair ability, therefore all must carry out the edge of anode paillon foil and the oxide-film repair process on surface after being made into capacitor body.
In the manufacture process of this class solid electrolytic capacitor, because what use is monomer and oxidizing agent solution chemical reaction and form conducting polymer electrolysis ply of paper in inside, can generate a large amount of acid in the chemical reaction process, this can cause damage to dielectric oxide film, and this class infringement is relatively littler under anhydrous condition.The conducting polymer composite that uses mostly in the present winding type electrolytic capacitor is poly-Ethylenedioxy Thiophene (PEDT), monomer is Ethylenedioxy Thiophene (EDT), oxidant all is the alcoholic solution of p-methyl benzenesulfonic acid iron usually, because EDT costs an arm and a leg, and causes the electrolytic capacitor price of takeup type conducting polymer composite of today also higher.And the relatively low pyrroles of price is applied in less in the wound capacitor, and the capacitor performance of preparing is less than the winding type electrolytic capacitor of PEDT class.Mainly be that polymerization reaction is difficult to be used in the chip capacitor mostly with control because the pyrroles gets, and the Wound capacitor application is less, Chinese patent (publication number: report is arranged CN1567492A).The oxidant that adopts is the ammonium persulfate aqueous solution, because the sulfuric acid that generates can cause serious corrosion to aluminium foil, in order to reduce corrosion, they have used ammonium hydroxide to alleviate the corrosivity of acid, but can impact capacitor performance, cause prepared capacitor performance to descend.
Summary of the invention
Defective or deficiency at above-mentioned prior art existence, the objective of the invention is to, the manufacture method of the coiled solid electrolysis capacitor of a kind of manufacturing high-performance with low cost, high reliability is provided, this method is used a kind of polymeric reaction solution for preparing polymer, and by the control temperature with add mode such as corrosion inhibiter and control the speed of chemical polymerization in the solution and acid corrosion, and utilize this reaction solution to prepare the coiling type solid electrolytic capacitor of high-performance, high reliability to metal forming.
In order to realize above-mentioned task, the present invention takes following technical solution:
1. the manufacture method of a coiled solid electrolysis capacitor is characterized in that, comprises the following steps:
A. anode foils that capacitor is used and Cathode Foil clip membrane coil coiled traditional electrical electrolysis condenser fuse, and carry out the repairing of oxide-film with changing into liquid;
B. with capacitor body after handling 1～120min under 240 ℃～450 ℃, repair with changing into the second time that liquid carries out oxide-film again;
C. prepare oxidizing agent solution, after the K cryogenic treatment, add the conductive high polymer monomer of polypyrrole class, mix, and capacitor body is immersed in the reaction solution, under-70 ℃～+ 60 ℃ environment, react 5～120min.
D. take out capacitor body after reaction is finished and clean, oven dry with methyl alcohol and deionized water;
E. then the capacitor body of drying is immersed in the mixed solution of epoxy resin and polyimide resin, takes out and under 60 ℃～150 ℃, dry, resin crosslinks is solidified;
F. encapsulation, seasoned behind the dry 30min in vacuum drying chamber at last can obtain coiled solid electrolysis capacitor.
The present invention has following feature:
1, the present invention uses the conducting polymer composite of the high polypyrrole class of conductivity to replace traditional electrolyte.Solved the problem of higher and conventional liquid electrolytic capacitor frequency characteristic of present solid electrolytic capacitor cost and poor stability.
2, the liquid that changes into of wherein repairing oxide-film is ammonium adipate solution, borax/boric acid solution, any one in the ammonium salt solution of phosphoric acid.
3, the monomer of compositing conducting high score material is pyrroles and derivative thereof, oxidant is persulfate (comprising ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate or persulfuric acid iron etc.), ferric sulfate, iron chloride, copper chloride, ferric perchlorate, potassium permanganate, p-methyl benzenesulfonic acid iron, hydrogen peroxide, the mixture of one or more in the DDQ.
4, add surfactant and corrosion inhibiter in oxidizing agent solution, thereby can produce the capacity height, leakage current is little, the high reliability solid electrolytic capacitor that impedance is low.
The surfactant that is added in the oxidizing agent solution is the water soluble surfactant active, be selected from alkyl sulfonic acid and sodium salt thereof, alkyl benzene sulphonate and sodium salt thereof, (alkyl substituent on aromatic rings can have 0～10 for alkyl aryl sulfonate such as alkyl naphthalene sulfonic acid and sodium salt thereof and sodium salt derivative thereof, the C chain length of alkyl is between 1～20 carbon atom, it can be straight chain, also can be side chain), and anion surfactant such as two (2-ethylhexyl) sodium sulfosuccinate, the alkyl polyoxyethylene derivative, non-ionic surface active agents such as APEO compounds, softex kw, cationic surfactants such as OTAC.
The corrosion inhibiter that adds in the oxidizing agent solution is selected from trisodium citrate, ammonium adipate, ammonium oxalate, sodium acetate, solvable carbonate, the mixture of one or several in the salts of weak acid such as solvable phosphate.
5, in the oxidant aqueous solution, added the organic solvent of alcohols, amine, acyl ammonium class or derivatives thereof, or mix the mixed solvent that obtains by a certain percentage by these a few class materials, make oxidizing agent solution in low temperature environment, can store the long period and do not separate out crystal, and then it is lower to make condensance.
Add organic solvents such as alcohol, amine, acid amides and derivative thereof in the oxidizing agent solution.Wherein alcohol is selected from methyl alcohol, ethanol, isopropyl alcohol, the mixture of one or more in the water miscible alcohol such as ethylene glycol, glycerol; Amine is selected methylamine, ethamine, the mixture of one or more of water miscible amine such as ethylenediamine or the various amine of C atom number between 1～10; The acid amides of C atom number between 1～10 of acid amides, and N, dinethylformamide, N, the mixture of one or more of amide derivatives such as N-dimethylacetylamide.
6, soak used epoxy resin and the polyimide resin solution ratio of fuse be about 1: 10～10: 1, what solvent used is ordinary organic solvents, concentration is 5～90%.
Embodiment
The manufacture method of making solid electrolytic capacitor of the present invention will be clipped in as the electrolytic paper of barrier film between anode aluminium foil and the cathode aluminum foil earlier, reel to form capacitor body; Make the electrolytic paper carbonization with changing at high temperature fuse to be handled after repairing that liquid carries out the edge oxide-film is repaired, perhaps earlier the repairing of oxide-film is carried out in the fuse carbonization again; Soak the mixed solution of oxidant and polymer monomer, perhaps soak monomer earlier and soak oxidizing agent solution or opposite again; Be placed on and carry out polymerization reaction under the uniform temperature environment, wherein lower temperature environment helps control rate, also can reduce the corrosiveness of acid to aluminium foil; Carry out cleaning-drying after reaction is finished,, encapsulate behind the high-temperature cross-linking with epoxy resin and polyimide resin perfusion.
Concrete manufacture method is as follows:
A. anode aluminium foil that capacitor is used and cathode aluminum foil clip membrane coil coiled traditional capacitor fuse, and carry out the repairing of edge oxide-film with changing into liquid;
B. with capacitor body after handling 1～120min under 240 ℃～450 ℃, repair with changing into the second time that liquid carries out the edge oxide-film again;
C. prepare oxidizing agent solution, after the K cryogenic treatment, add the conductive high polymer monomer of polypyrrole class, mix, and capacitor body is immersed in the reaction solution, under-70 ℃～+ 60 ℃ environment, react 5～120min.
D. take out capacitor body after reaction is finished and clean, oven dry with methyl alcohol and deionized water;
E. then the capacitor body of drying is immersed in the mixed solution of epoxy resin and polyimide resin, takes out and under 60 ℃～150 ℃, dry, resin crosslinks is solidified;
F. encapsulation, seasoned behind the dry 30min in vacuum drying chamber at last can obtain coiled solid electrolysis capacitor.
Below be the embodiment that the inventor provides, need to prove that these embodiment are embodiment preferred, the invention is not restricted to these embodiment.Part of hereinafter being mentioned all refers to weight.
Embodiment 1:
Electrolytic paper is clipped between anode aluminium foil and the cathode aluminum foil is wound into capacitor body, the capacitor body design capacity is 560 microfarads, operating voltage 10V;
In 10% the ammonium adipate aqueous solution, carry out earlier oxide-film and repaired 1～10 hour, capacitor body is placed on carries out the taking-up of 10min carbonization treatment under 320 ℃ then, and oxide-film repairing 1～10 hour is carried out in energising in 10% the ammonium adipate aqueous solution;
Then 4 parts of ammonium persulfates are mixed with 6 parts of deionized waters, 5 parts of isopropyl alcohols, add an amount of surfactant and be mixed with oxidizing agent solution, under-70 ℃, deposit 30min, add 1 part of pyrrole monomer again, mix;
In capacitor body vacuum impregnation mixed solution, and be placed on reaction 60min under-70 ℃ of environment;
After reaction is finished, take out capacitor body and clean the final vacuum drying with methyl alcohol and deionized water, put then to epoxy resin and polyimide resin mixture solution, the ratio of epoxy resin and polyimide resin is 1: 1, is placed on 150 ℃ after the immersion and solidifies 2h down.
Be placed on again in the vacuum drying chamber and encapsulate behind the dry 30min, can obtain coiled solid electrolysis capacitor.
Embodiment 2:
Except add 3 parts of trisodium citrates again in ammonium persulfate solution, other are all identical with embodiment 1.
Embodiment 3:
Mixture with 4 parts of ammonium persulfates and 6 parts of deionized waters, 5 parts of ethylene glycol adds an amount of surfactant, again as oxidizing agent solution.Other are all identical with embodiment 1.
Embodiment 4:
With 3 parts of iron chloride, 2 parts of deionized waters, 5 parts of ethanol, proper amount of surfactant, 1 part of pyrrole monomer is as the used reaction solution of dipping.Other are identical with embodiment 1.
Embodiment 5:
Change the reaction solution of dipping usefulness into 4 parts of p-methyl benzenesulfonic acid iron, 6 parts of n-butanols, 1 part of pyrrole monomer adds proper amount of surfactant, and other are identical with embodiment 1.
Embodiment 6:
Change the reaction solution of dipping usefulness into 2 parts of p-methyl benzenesulfonic acid iron, 2 parts of ammonium persulfates, 6 parts of deionized waters, 5 parts of isopropyl alcohols, other are identical with embodiment 1.
Comparative examples 1:
Do not add in oxidizing agent solution the surfactant, other are all identical with embodiment 1.
Comparative examples 2:
Except changing electrolytic paper into polypropylene non-woven fabric, thickness is 120 μ m, and without carbonization treatment, other are all identical with embodiment 1.
Comparative examples 3:
Except the mixed solution that does not soak epoxy resin and polyimide resin, other are all identical with embodiment 1.
Coiled solid electrolysis capacitor to specific embodiment 1～6 and comparative examples 1～3 preparation is tested, during test result is listed in the table below, capacitance uses 120Hz to test, and the time 100kHz that impedance is used tests, the leakage current 2min that switches under rated voltage 10V.
| Capacitance (μ F, 120Hz) | Impedance (m Ω, 100kHz) | Leakage current (μ A, 2min) | |
| Embodiment 1 | 501 | 6 | 56 |
| Embodiment 2 | 498 | 16 | 32 |
| Embodiment 3 | 491 | 11 | 75 |
| Embodiment 4 | 436 | 18 | 586 |
| Embodiment 5 | 473 | 10 | 36 |
| Embodiment 6 | 495 | 7 | 58 |
| Comparative examples 1 | 357 | 46 | 63 |
| Comparative examples 2 | 232 | 389 | 67 |
| Comparative examples 3 | 458 | 9 | 1076 |
In embodiment 1～6,, make the impedance of capacitor all lower, and in specific embodiment 4, use the stronger iron chloride of corrosivity, so leakage current is bigger owing to generated the polypyrrole of high conductivity in capacitor body inside; Owing to lack the effect of surfactant, capacitor metal oxide film surface is poor slightly with combining of polypyrrole material, causes capacity lower in comparative examples 1; And too thick owing to this nonwoven fabrics in comparative examples 2, reach 120 microns, and traditional electrolytic paper has only about 50 microns, so cause inside in conjunction with very poor, electrical property does not reach requirement; In comparative examples 3,, cause leakage current bigger owing to do not use epoxy resin and polyimide resin that capacitor body is coated at last comprehensively.And the capacitor body that uses epoxy resin and polyimide resin to coat because the part of its seriously corroded obtains covering and plays insulating effect, descends leakage current, thereby leakage current is lower.In addition since the adhesive attraction of epoxy resin and polyimide resin with polypyrrole material tightly attached on the tinsel, also make capacitor more stable.
The method according to this invention can produce big capacity, Low ESR, low-leakage current, the capacitor of high stability.This capacitor has that capacity is big, and the impedance leakage current is little, and frequency characteristic is good, the advantage that reliability is high.And manufacturing process only needs to add simple several steps on traditional handicraft, and more exchange device, so this solid electrolytic capacitor all has wide prospect and large market on producing and using.That the present invention is cited all is the embodiment of convoluted capacitor, but method of the present invention is not limited only to convoluted capacitor, can be equally applicable to the electrolytic capacitor of other types.Has industrial applicibility.
Claims (10)
1. the manufacture method of a coiled solid electrolysis capacitor is characterized in that, comprises the following steps:
A. anode aluminium foil that capacitor is used and cathode aluminum foil clip membrane coil coiled traditional capacitor fuse, and carry out the repairing of oxide-film with changing into liquid;
B. with capacitor body after handling 1～120min under 240 ℃～450 ℃, repair with changing into the second time that liquid carries out oxide-film again;
C. prepare oxidizing agent solution, after the K cryogenic treatment, add the conductive high polymer monomer of polypyrrole class, mix, and capacitor body is immersed in the reaction solution, under-70 ℃～+ 60 ℃ environment, react 5～120min.
D. take out capacitor body after reaction is finished and clean with methyl alcohol and deionized water, and oven dry;
E. then the capacitor body of drying is immersed in the mixed solution of epoxy resin and polyimide resin, takes out and under 60 ℃～150 ℃, dry, resin crosslinks is solidified;
F. encapsulation, seasoned behind the dry 30min in vacuum drying chamber at last can obtain coiled solid electrolysis capacitor.
2. the method for claim 1 is characterized in that, described change into liquid be ammonium adipate solution, borax/boric acid solution or phosphoric acid ammonium salt solution wherein any one or mix the mixed liquor obtain by arbitrary proportion by three kinds of solution.
3. the method for claim 1 is characterized in that, the conductive high polymer monomer of described polypyrrole class is pyrroles and derivative thereof.
4. the method for claim 1, it is characterized in that described oxidizing agent solution is one or more the mixture in persulfate, ferric sulfate, iron chloride, copper chloride, ferric perchlorate, potassium permanganate, p-methyl benzenesulfonic acid iron, hydrogen peroxide or the DDQ.
5. the method for claim 1 is characterized in that, described persulfate is ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate or persulfuric acid iron.
6. method as claimed in claim 4 is characterized in that, also is added with surfactant, corrosion inhibiter in the described oxidizing agent solution.
7. method as claimed in claim 6 is characterized in that described surfactant is the water soluble surfactant active, comprises water-soluble anionic surfactant, non-ionic surface active agent or cationic surfactant;
Said water soluble anionic surfactant is two (2-ethylhexyl) sodium sulfosuccinate, alkyl sulfonic acid and sodium salt, alkyl benzene sulphonate and sodium salt thereof, alkyl naphthalene sulfonic acid and sodium salt thereof or alkyl aryl sulfonate and sodium salt derivative thereof, at the alkyl substituent on the aromatic rings between 0～10, the carbon chain lengths of alkyl is between 1～20 carbon atom, these carbochains are straight chains, or side chain;
Said water soluble nonionic surfactant is alkyl polyoxyethylene derivative or APEO compounds;
Said water-soluble cationic surfactant is softex kw or OTAC.
8. method as claimed in claim 6 is characterized in that, described corrosion inhibiter is selected from one or several the mixture in trisodium citrate, ammonium adipate, ammonium oxalate, sodium acetate, solvable carbonate or the solvable phosphate.
9. method as claimed in claim 4 is characterized in that, also is added with the organic solvent of alcohols, amine, acyl ammonium class or derivatives thereof in the described oxidizing agent solution, or mixes the mixed solvent that obtains by a certain percentage by these a few class materials; Wherein, alcohol is selected from methyl alcohol, ethanol, isopropyl alcohol, the mixture of one or more in ethylene glycol, the glycerol; Amine is selected methylamine, ethamine, the mixture of one or more of ethylenediamine or amine or the various amine of C atom number between 1～10; The acid amides of C atom number between 1～10 of acid amides, or N, dinethylformamide, N, the mixture of one or more of N-dimethylacetylamide.
10. the method for claim 1 is characterized in that, about 1: 10～10: 1 of the mixed solution ratio of described epoxy resin and polyimide resin, and wherein the solvent of mixed solution uses ordinary organic solvents, and its concentration is 5～90%.
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| CN109637810A (en) * | 2018-11-29 | 2019-04-16 | 肇庆绿宝石电子科技股份有限公司 | A kind of preparation method of solid-liquid mixed type electrolytic capacitor |
| CN109637810B (en) * | 2018-11-29 | 2020-09-25 | 肇庆绿宝石电子科技股份有限公司 | Preparation method of solid-liquid mixed electrolytic capacitor |
| CN111029175A (en) * | 2019-11-28 | 2020-04-17 | 肇庆绿宝石电子科技股份有限公司 | SMD solid capacitor with long service life and manufacturing method thereof |
| CN111785524A (en) * | 2020-07-15 | 2020-10-16 | 常州华威电子有限公司 | High temperature resistant polymer aluminium solid capacitor |
| CN112017865A (en) * | 2020-07-24 | 2020-12-01 | 东莞东阳光科研发有限公司 | Hydration treatment method for reducing leakage current of formed foil |
| CN115083781A (en) * | 2022-06-27 | 2022-09-20 | 丰宾电子（深圳）有限公司 | Material of high-molecular capacitor and manufacturing process thereof |
| CN115083781B (en) * | 2022-06-27 | 2023-09-01 | 丰宾电子科技股份有限公司 | Manufacturing process of monopole sheet of high-molecular capacitor |
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