CN103390500B - A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage - Google Patents
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage Download PDFInfo
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- CN103390500B CN103390500B CN201310325121.9A CN201310325121A CN103390500B CN 103390500 B CN103390500 B CN 103390500B CN 201310325121 A CN201310325121 A CN 201310325121A CN 103390500 B CN103390500 B CN 103390500B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 43
- 239000007787 solid Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 107
- 239000002322 conducting polymer Substances 0.000 claims abstract description 96
- 239000002002 slurry Substances 0.000 claims abstract description 61
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 59
- 238000003466 welding Methods 0.000 claims abstract description 14
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- 230000004913 activation Effects 0.000 claims abstract description 11
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- 229910002804 graphite Inorganic materials 0.000 claims abstract description 10
- 239000010439 graphite Substances 0.000 claims abstract description 10
- 229910052709 silver Inorganic materials 0.000 claims abstract description 10
- 239000004332 silver Substances 0.000 claims abstract description 10
- 238000003487 electrochemical reaction Methods 0.000 claims abstract description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 59
- 229910000077 silane Inorganic materials 0.000 claims description 59
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
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- OHLUUHNLEMFGTQ-UHFFFAOYSA-N N-methylacetamide Chemical compound CNC(C)=O OHLUUHNLEMFGTQ-UHFFFAOYSA-N 0.000 description 1
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- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical group OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
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- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
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- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
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- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical compound CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps: (1), by electrochemical reaction until tantalum block surface formed unbodied Ta2O5 dielectric layer; (2), activation processing; (3) the first conducting polymer rete, is formed; (4), intermediate adhesion layer is formed; (5) the second conducting polymer rete, is formed; (6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.The invention has the beneficial effects as follows: the electrical quantity characteristic that improve solid electrolytic capacitor, reduces ESR and leakage current, improves the puncture voltage of capacitor, adds the stability of capacitor in high frequency and hyperbaric environment simultaneously.
Description
Technical field
The present invention relates to a kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, belong to electrolytic capacitor manufacturing technology field.
Background technology
Along with electronic equipment digitlization, microminiaturization and lightweight acceleration, require that capacitor has small-sized, Large Copacity, high frequency performance and stablizes and have the feature of very strong resistance to ripple current.Particularly in recent years, along with the high speed of signal processing circuit in the electronic equipment such as personal computer, smart mobile phone, must be instantaneous to this signal processing circuit supply electric current, therefore the demand of the solid electrolytic capacitor that high-frequency region equivalent series resistance (ESR) is little is day by day urgent and huge.Electrostrictive polymer electrolysis condenser receives much attention because of lower ESR and good high frequency characteristics.But electrostrictive polymer electrolysis condenser makes one deck conductive polymer electrolyte on oxide film dielectric surface by the method for in-situ chemical polymerization, electrochemical polymerization or surface-coated polymeric size.This capacitor ubiquity Railway Project, product that is as large in leakage current or short-circuit failure is many; Contact resistance between conductive polymer electrolyte and dielectric oxide film is large, or adhesive strength between conductivity dielectric substrate and dielectric layer is lower etc., causes the increase of ESR.Conducting polymer comprises pi-conjugated key, has very high conductivity, is generally overlayed on dielectric surface by the method for in-situ oxidizing-polymerizing or electrochemical polymerization, and the polymer film of formation is as the electrolyte of solid electrolytic capacitor.Patent CN1992110A improves adhesive strength therebetween to by interpolation polyethylene glycol adhesive linkage in the middle of conductive polymer coating and dielectric layer, thus reaches the object reducing ESR.Patent CN101714464A uses the coupling agent substituted silane coupling agent of phosphonate group to process to reaching the object reducing leakage current and ESR to dielectric surface, patent CN102005313A adds silane in conducting polymer, and change the concentration of silane at the thickness direction of conducting polymer, with the defective products incidence of the leakage current and short circuit that reduce product.Several method plays improvement result in various degree to the leakage current of product and ESR above.But in later stage reliability test and reflow welding test, still there is leakage current increase, or the phenomenon of short circuit, particularly higher to rated voltage product, this type of phenomenon is more serious.
Summary of the invention
The object of the present invention is to provide a kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, the electrical quantity characteristic of solid electrolytic capacitor can be improved, reduce ESR and leakage current, improve the puncture voltage of capacitor, be increased in stability in high frequency and hyperbaric environment.
The object of the invention is to be achieved through the following technical solutions: a kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 0.03%-60% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 2-10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, drier 30 ~ 90min forms surface active layer until tantalum block is surperficial in the air ambient of 120 ~ 250 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 10-20mPa.s's, dip time is 2-10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, then in the air ambient of 80 ~ 150 DEG C dry 20-40min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 3 ~ 5min, then in the air ambient of 150 ~ 200 DEG C dry 20-40min;
(5) the second conducting polymer rete, is formed: it is 12 ~ 35mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 2-10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, dry 30-60min in the air ambient of 80 ~ 200 DEG C again, repeats this process 3 ~ 5 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 0.1% ~ 30%, and end agent is alcohols, the one of deionized water or mixed liquor.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 0.01% ~ 3% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.03 ~ 0.3% of water content, and conduction-enhancing agent is 0.01 ~ 0.1% of water content.
Generally speaking, the method for traditional making electrolytic capacitor cathode polymer dielectric has chemical polymerization and electrochemical polymerization method.By chemical polymerization and electrochemical polymerization method at the surface-coated conducting polymer thin film of dielectric oxide film, be easy to the damage causing deielectric-coating.It has been generally acknowledged that the charged free radical of the oxidized formation of monomer, these free radicals, between two in conjunction with formation dimer, also may form trimer simultaneously, and tetramer and other oligomer, finally form conducting high polymers thing.And these oligomer have very high energy and very active.Therefore, can think like this, in polymerization process, these free radicals can not only react to each other, and can react with tantalum pentoxide medium, by to implantation defect in medium (electronics or hole), thus significantly reduce the insulation property of medium, that is, the reduction of dielectric insulation performance is caused by energetic free radical and reacting to each other of medium.Because these free radicals are the intermediate products in polymerization process, therefore the reduction of polymerization process medium performance is unavoidable in position.In order to effectively reduce the leakage current of product and reduce the risk of product failure; patent CN102054596A proposes the surface-coated one deck resin protective layer at tantalum fuse; thus the destruction that can reduce dielectric oxide film; on the other hand; can effective defect in isolated oxide film itself; thus the generation of short circuit can be reduced, reduce the leakage current in product.But coated with resins protective layer is easy to block hole, affects the capacity extraction rate of product.
In order to improve the adhesive strength between conducting polymer rete and dielectric oxide film, do not destroy the performance of dielectric oxide film simultaneously, attempting using silane coupler to carry out activation processing silane coupler as pretreating agent to oxide-film surface is in fact the silane that a class has organo-functional group, there is the reactive group of energy and inorganic material chemistry combination in the molecule thereof simultaneously, have again the reactive group be combined with organic materials chemistry.Therefore, by using silane coupler, can erect between inorganic substances and the interface of organic substance " molecular bridge ", dielectric oxide film and conducting polymer are linked together.Thus the performance improving composite material and the adhesive strength increased between material.Between oxide-film and conducting polymer materials, add silane coupler, the mechanical performance of polymer capacitors, electrical property and ageing resistace can be made to be greatly improved.The silane with organic metal function added and hydrate are as 3-glycidoxy-propyltrimethoxy silane, 3-aminopropyl triethoxysilane, 3-Mercaptopropyltriethoxysilane, 3-methyl-prop allyl oxygen propyl-triethoxysilicane, vinyltrimethoxy silane, octyl group trimethoxy silane etc.
Described conducting polymer slurry I and conducting polymer slurry II forms by the material of following proportioning: 0.5-10% conductive polymer particles, the polymeric anion of 2-66%, dispersant surplus, wherein, solid content in the particle diameter of the conductive polymer particles of conducting polymer slurry II, slurry and viscosity are all greater than solid content in the particle diameter of conducting polymer slurry I, slurry and viscosity, and dispersant is water or some other organic solvent.Tantalum block is flooded this slurry and in suitable environment after drying, forms the pi-conjugated conducting polymer thin film of one deck on the surface of oxide isolation film.And pi-conjugated conducting polymer has very high conductivity and thermal stability, be particularly suitable as the electrolyte of electrolytic capacitor.Pi-conjugated conducting polymer comprises polypyrrole, polythiophene, polyaniline, polyacetylene and polyphenylene oxide etc. and derivative thereof.Most importantly polythiophene, normally used is wherein a kind of derivative, namely 3 are gathered, 4-ethene dioxythiophene (being abbreviated as PEDOT), oxide because of it has very high conductivity, therefore this polymer is widely used in solid electrolytic capacitor, Organic Light Emitting Diode (OLED), in many electronic devices such as organic solar batteries and organic field-effect tube.
The electrolyte using conducting polymer slurry to make electrolytic capacitor has a lot of method, the most frequently used is the method for flooding, tantalum block is slowly immersed in slurry, at high temperature dry again after dipping a period of time, thus form one deck conducting polymer on dielectric oxide film surface.
Use low viscous slurry I in certain environment after drying, the conductance of film of the conducting polymer formed is greater than 10S/cm, than better suited be greater than 20S/cm, be more suitably greater than 50S/cm, be more preferably and be greater than 100S/cm, even 200S/cm or 1000S/cm.
First conducting polymer rete forms the electrolytical internal layer of electric conductive polymer, and the first conducting polymer rete forms intermediate adhesion layer.By forming such structure, obviously can improve the tack between dielectric layer and electroconductive polymer dielectric substrate, improve the ability of electroconductive polymer dielectric substrate resistance to mechanical intensity and resistance to electric current, voltge surge, improve the reliability and stability of electroconductive polymer electrolytic capacitor.
Intermediate adhesion layer used comprises as polyvinyl acetate than better suited adhesive, Merlon, polyvinyl butyral resin, polyacrylate, polymethacrylates, polystyrene, polyacrylonitrile, polyvinyl chloride, polybutadiene, polyisoprene, organosilicon or phenylethylene ethylene/propenoic acid ester, poly-vinyl butyrate, vinyl acetate/acrylate, ethylene/vinyl acetate copolymer, polyethers, polyester fiber, silicone, pyrroles/acrylate, ethylene/acetic acid methacrylate copolymers, polyvinyl alcohol, polyvinylpyrrolidone, according to acrylic acid ammonia, polymethacrylates, polymethylacrylic acid ammonia, phenylethylene ethylene/propenoic acid ester, vinyl acetate/propylene, polyurethane, polyamide, polyimides, polysulfones, melamine resin, epoxy resin or fiber, and polyethylene glycol, polyglycerol etc., the good polyethylene glycol of preferred bonding effect.
In addition, containing conduction-enhancing agent in the solution of intermediate adhesion layer, comprise oxolane, the compound of lactone function is (as gamma-butyrolacton, gamma-valerolactone etc.), amino or lactam. function's compound are (as caprolactam, N-methyl caprolactam, N, N-dimethylacetylamide, N-methylacetamide, N, dinethylformamide (DMF), N-METHYLFORMAMIDE, N-METHYLFORMAMIDE etc.), alkane ketone is (as 1-METHYLPYRROLIDONE (NMP), NOP, pyrrolidones etc.), sulfone and sulfoxide (as sulfolane (tetramethylene sulfone) and dimethyl sulfoxide (DMSO) (DMSO) etc.) etc.Oxolane, N-methyl nitrosourea, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), and sorbierite is preferred conductivity enhancer reagents, preferred DMSO is as conduction-enhancing agent.Because of the material that polyethylene glycol is ionic conduction, thus between polymer film, form the dielectric substrate of mixing, therefore, the residual current in electrolyte and ESR can be reduced.
Beneficial effect of the present invention is: form dielectric oxide film on the surface of tantalum block by electrochemical method, with silane coupler, activation processing is carried out to dielectric oxide film surface, at dielectric oxide film surface-coated first conducting polymer rete, intermediate adhesion layer is applied on the first conducting polymer rete, the second conducting polymer rete is made on intermediate adhesion layer, improve the electrical quantity characteristic of solid electrolytic capacitor, reduce ESR and leakage current, improve the puncture voltage of capacitor, add the stability of capacitor in high frequency and hyperbaric environment simultaneously.
Embodiment
Technical scheme of the present invention is further described below in conjunction with embodiment, but described in claimed scope is not limited to.
Embodiment 1
Have a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 10% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 5min, then dry 20min in the air ambient of 35 DEG C, drier 60min forms surface active layer until tantalum block is surperficial in the air ambient of 200 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 15mPa.s's, dip time is 5min, then dry 30min in the air ambient of 45 DEG C, then in the air ambient of 100 DEG C dry 30min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 4min, then in the air ambient of 180 DEG C dry 30min;
(5) the second conducting polymer rete, is formed: it is 25mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 5min, then dry 30min in the air ambient of 35 DEG C, dry 40min in the air ambient of 180 DEG C again, repeats this process 5 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 20%.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 0.05% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.1% of water content, and conduction-enhancing agent is 0.01% of water content.
Comparative examples 1
The tantalum block generating dielectric layer is immersed dipping p-methyl benzenesulfonic acid solution 5min, flood 3 again, 4-ethylenedioxythiophene (EDOT) monomer solution 5min, at 25 ~ 30 DEG C, relative humidity is polymerization reaction take place 60min in the air ambient of 30% ~ 70%, then washes remaining monomer and byproduct of reaction, thus reoxidizes deielectric-coating surface formation one deck conducting polymer thin film (PEDOT), this process repeats 6 times, increases the concentration of monomer and oxidant.Repeat said process 6 ~ 10 times, form certain thickness polyelectrolyte floor.The product of drying is immersed respectively graphite and silver slurry.Then carry out spot welding, bonding and moulded package, finally the electrical quantity of capacitor is measured.
Comparative examples 2
In embodiment 1, tantalum block is not covered with surface active layer, and directly at tantalum core surface coated with conductive polymer film I, intermediate adhesion layer and conducting polymer rete II.Then carry out spot welding, bonding and moulded package, finally the electrical quantity of capacitor is measured.
Comparative examples 3
In embodiment 1, tantalum block is not covered with surface active layer and intermediate adhesion layer, and directly at tantalum core surface coated with conductive polymer film I and conducting polymer rete II.Then carry out spot welding, bonding and moulded package, finally the electrical quantity of capacitor is measured.
Comparative examples 4
In embodiment 1, tantalum block surface silane coupler carries out activation processing, then at active layer surface-coated conducting polymer rete I and conducting polymer rete II.Then spot welding, bonding and moulded package is carried out.Finally the electrical quantity of capacitor is measured.
Comparative examples 5
In embodiment 1, the tantalum block generating dielectric layer is immersed dipping p-methyl benzenesulfonic acid solution 5min, flood 3 again, 4-ethylenedioxythiophene (EDOT) monomer solution 5min, at 25 ~ 30 DEG C, relative humidity is polymerization reaction take place 60min in the air ambient of 30% ~ 70%, then washes remaining monomer and byproduct of reaction, thus reoxidizing deielectric-coating surface formation one deck conducting polymer thin film (PEDOT), this process repeats 6 times.Again the anode block being covered with conducting polymer thin film is immersed the slurry of conducting polymer, form certain thickness polyelectrolyte floor.The product of drying is immersed respectively graphite and silver slurry.Then carry out spot welding, bonding and moulded package, finally the electrical quantity of capacitor is measured.
The performance parameter contrast of table 1 embodiment 1,2 and comparative example 1,2,3,4
Visible, example 1 and example 2 improve the electrical quantity characteristic of solid electrolytic capacitor, reduce ESR and leakage current, improve the puncture voltage of capacitor, add the stability of capacitor in high frequency and hyperbaric environment simultaneously.
Embodiment 2
Have a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 60% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 2min, then dry 30min in the air ambient of 25 DEG C, drier 30min forms surface active layer until tantalum block is surperficial in the air ambient of 250 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 10mPa.s's, dip time is 10min, then dry 10min in the air ambient of 50 DEG C, then in the air ambient of 80 DEG C dry 40min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 5min, then in the air ambient of 150 DEG C dry 40min;
(5) the second conducting polymer rete, is formed: it is 12mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 10min, then dry 30min in the air ambient of 25 DEG C, dry 30min in the air ambient of 200 DEG C again, repeats this process 3 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 30%.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 0.01% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.3% of water content, and conduction-enhancing agent is 0.1% of water content.
Embodiment 3
Have a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 0.03% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 10min, then dry 10min in the air ambient of 50 DEG C, drier 90min forms surface active layer until tantalum block is surperficial in the air ambient of 120 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 20mPa.s's, dip time is 2min, then dry 15min in the air ambient of 30 DEG C, then in the air ambient of 150 DEG C dry 20min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 3min, then in the air ambient of 200 DEG C dry 20min;
(5) the second conducting polymer rete, is formed: it is 35mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 2min, then dry 10min in the air ambient of 50 DEG C, dry 60min in the air ambient of 80 DEG C again, repeats this process 5 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 0.01%.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 3% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.03% of water content, and conduction-enhancing agent is 0.01% of water content.
Embodiment 4
Have a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 20% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 8min, then dry 15min in the air ambient of 40 DEG C, drier 70min forms surface active layer until tantalum block is surperficial in the air ambient of 180 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 16mPa.s's, dip time is 6min, then dry 20min in the air ambient of 35 DEG C, then in the air ambient of 120 DEG C dry 25min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 4min, then in the air ambient of 170 DEG C dry 35min;
(5) the second conducting polymer rete, is formed: it is 24mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 5min, then dry 25min in the air ambient of 30 DEG C, dry 40min in the air ambient of 150 DEG C again, repeats this process 4 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 10%.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 1% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.15% of water content, and conduction-enhancing agent is 0.05% of water content.
Embodiment 5
Have a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 6% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta205 dielectric layer on tantalum block surface;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 7min, then dry 14min in the air ambient of 45 DEG C, drier 50min forms surface active layer until tantalum block is surperficial in the air ambient of 210 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in by the tantalum block being covered with surface active layer in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 18mPa.s's, dip time is 5min, then dry 20min in the air ambient of 40 DEG C, then in the air ambient of 140 DEG C dry 30min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 3min, then in the air ambient of 160 DEG C dry 40min;
(5) the second conducting polymer rete, is formed: it is 28mPa.s conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 8min, then dry 28min in the air ambient of 34 DEG C, dry 50min in the air ambient of 120 DEG C again, repeats this process 5 times until surface active layer is covered with the second conducting polymer rete;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 15%.
In the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 0.5% of conducting polymer slurry I content.
Described slurry is mixed by water, adhesive and conduction-enhancing agent, and wherein adhesive is 0.2% of water content, and conduction-enhancing agent is 0.08% of water content.
Claims (5)
1. there is a manufacture for solid electrolytic capacitor for high-breakdown-voltage, it is characterized in that: it comprises following steps:
(1), by the tantalum block after sintering the phosphoric acid solution that concentration is 0.03% ~ 60% is placed in, then logical direct current, by electrochemical reaction until form unbodied Ta on tantalum block surface
2o
5dielectric layer;
(2), activation processing: the tantalum block generating dielectric layer immerses silane coupler dilution, dip time is 2 ~ 10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, drier 30 ~ 90min forms surface active layer until tantalum block is surperficial in the air ambient of 120 ~ 250 DEG C;
(3) the first conducting polymer rete, is formed: be immersed in the mixed liquor of silane coupler and conducting polymer slurry I by the tantalum block being covered with surface active layer, the viscosity of mixed liquor is 10 ~ 20mPas, dip time is 2 ~ 10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, then in the air ambient of 80 ~ 150 DEG C dry 20 ~ 40min until surface active layer is covered with the first conducting polymer rete;
(4), form intermediate adhesion layer: the tantalum block that will be covered with the first conducting polymer rete immerses in adhesive solution, and dip time is 3 ~ 5min, then in the air ambient of 150 ~ 200 DEG C dry 20 ~ 40min;
(5) the second conducting polymer rete, is formed: it is 12 ~ 35mPas conducting polymer slurry II that the tantalum block being covered with intermediate adhesion layer is immersed viscosity, dip time is 2 ~ 10min, then dry 10 ~ 30min in the air ambient of 25 ~ 50 DEG C, dry 30 ~ 60min in the air ambient of 80 ~ 200 DEG C, repeats this process 3 ~ 5 times until surface active layer is covered with the second conducting polymer rete again;
(6), by the product of drying immerse graphite and silver slurry respectively, then carry out spot welding, bonding and moulded package;
Described silane coupler dilution forms by adding end dilution agent in silane coupler, and the diluted concentration of silane coupler is 0.1% ~ 30%, and end agent is alcohols, the one of deionized water or mixed liquor.
2. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, is characterized in that: in described step (1), direct current adopts the direct voltage of 55V.
3. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, is characterized in that: in the mixed liquor of described silane coupler and conducting polymer slurry I, silane coupler is 0.01% ~ 3% of conducting polymer slurry I content.
4. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, it is characterized in that: described adhesive solution is mixed by water, adhesive and conduction-enhancing agent, wherein adhesive is 0.03 ~ 0.3% of water content, and conduction-enhancing agent is 0.01 ~ 0.1% of water content.
5. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, it is characterized in that: described conducting polymer slurry I and conducting polymer slurry II form by the material of following proportioning: the conductive polymer particles of 0.5 ~ 10%, the polymeric anion of 2 ~ 66%, dispersant surplus, wherein, the solid content in the particle diameter of the conductive polymer particles of conducting polymer slurry II, slurry and viscosity are all greater than solid content in the particle diameter of the conductive polymer particles of conducting polymer slurry I, slurry and viscosity.
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| CN103854868B (en) * | 2014-03-12 | 2016-06-29 | 中国振华（集团）新云电子元器件有限责任公司 | Manufacture method suitable in more than 75V high voltage-rated solid electrolytic capacitor |
| CN103985548A (en) * | 2014-04-28 | 2014-08-13 | 中国振华（集团）新云电子元器件有限责任公司 | Method for manufacturing solid electrolytic capacitor |
| CN104008883B (en) * | 2014-06-20 | 2016-07-27 | 重庆工商大学 | High conductivity flexible compound catholyte preparation method |
| CN105609313B (en) * | 2016-01-13 | 2018-05-11 | 深圳顺络电子股份有限公司 | A kind of manufacture method of chip conducting polymer tantalum capacitor cathode guide layer |
| CN109961955A (en) * | 2017-12-25 | 2019-07-02 | 钰邦科技股份有限公司 | Capacitor package structure with functional coating and method of making the same |
| CN114068190A (en) * | 2021-11-16 | 2022-02-18 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Method for improving insulation strength of tantalum capacitor |
| CN114050056A (en) * | 2021-11-18 | 2022-02-15 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | Tantalum capacitor anode and preparation method thereof, and tantalum capacitor and preparation method thereof |
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