CN103390500A - Manufacturing method for solid electrolytic condenser with high puncture voltage - Google Patents
Manufacturing method for solid electrolytic condenser with high puncture voltage Download PDFInfo
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- CN103390500A CN103390500A CN2013103251219A CN201310325121A CN103390500A CN 103390500 A CN103390500 A CN 103390500A CN 2013103251219 A CN2013103251219 A CN 2013103251219A CN 201310325121 A CN201310325121 A CN 201310325121A CN 103390500 A CN103390500 A CN 103390500A
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Abstract
The invention discloses a manufacturing method for a solid electrolytic condenser with high puncture voltage, which comprises the following steps: (1) carrying out electrochemical reaction until a formless Ta2O5 dielectric layer is formed on the surface of a tantalum block; (2) carrying out activating treatment; (3) forming a first conducting polymer film layer; (4) forming a middle bonding layer; (5) forming a second conducting polymer film layer; (6) immersing the dried product into graphite and silver paste respectively, and then carrying out spot welding, bonding and mould press sealing. The method has the benefits that the electrical parameter property of the solid electrolytic condenser is improved; the ESR and the leakage current are reduced; the puncture voltage of the condenser is improved; meanwhile the stability of the condenser in the high-frequency and high-pressure environment is enhanced.
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 capacitor to have small-sized, a large capacity, high frequency performance stable and have characteristics of very strong anti-ripple current.Particularly in recent years, be accompanied by the high speed of signal processing circuit in the electronic equipments such as personal computer, smart mobile phone, must be instantaneous this signal processing circuit be supplied with electric current, so the demand of the little solid electrolytic capacitor of high-frequency region equivalent series resistance (ESR) is day by day urgent and huge.The electrostrictive polymer electrolysis condenser receives much attention because of lower ESR and good high frequency characteristics.But the electrostrictive polymer electrolysis condenser is to make one deck conducting polymer electrolyte on the oxide film dielectric surface by the method for in-situ chemical polymerization, electrochemical polymerization or surface-coated polymeric size.The several problems of this capacitor ubiquity, product as large in leakage current or short-circuit failure is many; Contact resistance between conducting polymer electrolyte and dielectric oxide film is large, and perhaps the adhesive strength between conductivity electrolysis matter layer and dielectric layer is lower etc., causes the increase of ESR.Conducting polymer comprises pi-conjugated key, has very high conductivity, and generally the method by in-situ oxidizing-polymerizing or electrochemical polymerization is overlayed on dielectric surface, and the polymer film of formation is as the electrolyte of solid electrolytic capacitor.Patent CN1992110A is to by add the adhesive strength of polyethylene glycol adhesive linkage between improving both in the middle of conductive polymer coating and dielectric layer, thereby reaches the purpose that reduces ESR.Patent CN101714464A uses the coupling agent substituted silane coupling agent of phosphonate group dielectric surface to be processed the purpose that reduces leakage current and ESR to reaching, patent CN102005313A adds silane in conducting polymer, and change the concentration of silane at the thickness direction of conducting polymer, with the leakage current that reduces product and the defective products incidence of short circuit.Top several method plays in various degree improvement effect to the leakage current of product and ESR.Increase but in the test of later stage reliability test and reflow welding, leakage current occurs still, the perhaps phenomenon of short circuit, the particularly product higher to rated voltage, 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, can improve the electrical quantity characteristic of solid electrolytic capacitor, reduce ESR and leakage current, improve the puncture voltage of capacitor, be increased in stability in high frequency and hyperbaric environment.
The objective 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), the tantalum piece after sintering is placed in the phosphoric acid solution that concentration is 0.03%-60%, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 2-10min, then dry 10～30min in the air ambient of 25～50 ℃, then in the air ambient of 120～250 ℃ dry 30～90min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 80～150 ℃ dry 20-40min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 20-40min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 12～35mPa.s conducting polymer slurry II, dip time is 2-10min, then dry 10～30min in the air ambient of 25～50 ℃, dry 30-60min in the air ambient of 80～200 ℃, repeat this process 3～5 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, the diluted concentration of silane coupler is 0.1%～30%, and end agent is a kind of or mixed liquor of alcohols, deionized water.
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 reinforcing agent, and wherein adhesive is 0.03～0.3% of water content, and the conduction reinforcing 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., at the surface-coated conducting polymer thin film of dielectric oxide film, be easy to cause the damage of deielectric-coating by chemical polymerization and electrochemical polymerization method.It has been generally acknowledged that the charged free radical of the oxidized formation of monomer, these free radicals, in conjunction with forming dimer, also may form trimer simultaneously in twos, and tetramer and other oligomer, form the conducting high polymers thing finally.And these oligomer have very high energy and very active.Therefore, can think like this, these free radicals not only can react to each other in polymerization process, and can react with the tantalum pentoxide medium, by implantation defect in medium (electronics or hole), thereby significantly reduced the insulation property of medium, that is to say, the reduction of dielectric insulation performance is to be caused by reacting to each other of high energy free radical and medium.Because these free radicals are the intermediate products in polymerization process, therefore the reduction of polymerization process medium performance is unavoidable in position.For the leakage current that effectively reduces product and the risk that reduces product failure; patent CN102054596A proposes the surface-coated one deck resin protective layer at the tantalum fuse; thereby can reduce the destruction to dielectric oxide film; on the other hand; effective defect in isolated oxide film itself; thereby can reduce the generation of short circuit, reduce the leakage current in product.But the coated with resins protective layer is easy to stop up 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 simultaneously the performance of dielectric oxide film, attempting using silane coupler, as pretreating agent, the activation processing silane coupler is carried out on the oxide-film surface is in fact the silane that a class has organo-functional group, have simultaneously the reactive group of energy and inorganic material chemistry combination in its molecule, the reactive group of with organic materials chemistry, being combined is arranged again.Therefore,, by using silane coupler, can erect " molecular bridge " between the interface of inorganic substances and organic substance, dielectric oxide film and conducting polymer are linked together.Thereby improve the performance of composite material and the adhesive strength between the increase material.Add silane coupler between oxide-film and conducting polymer materials, mechanical performance, electrical property and the ageing resistace of polymer capacitors are greatly improved.The silane with organic metal function and hydrate such as the 3-glycidoxy-propyltrimethoxy silane that add, the 3-aminopropyl triethoxysilane, 3-sulfydryl propyl-triethoxysilicane, 3-methyl-prop allyl oxygen propyl-triethoxysilicane, vinyltrimethoxy silane, octyl group trimethoxy silane etc.
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 polymerization anion of 2-66%, the dispersant surplus, wherein, the particle diameter of the conductive polymer particles of conducting polymer slurry II, the solid content in slurry and viscosity are all greater than the particle diameter of conducting polymer slurry I, solid content and viscosity in slurry, and dispersant is water or some other organic solvent.The tantalum piece is flooded this slurry and after drying, on the surface of oxide isolation film, form the pi-conjugated conducting polymer thin film of one deck in suitable environment.And pi-conjugated conducting polymer has very high conductivity and thermal stability, is particularly suitable as the electrolyte of electrolytic capacitor.Pi-conjugated conducting polymer comprises polypyrrole, polythiophene, polyaniline, polyacetylene and polyphenylene oxide etc. and derivative thereof.Of paramount importance is polythiophene, normally used is a kind of derivative wherein, namely gather 3,4-ethene dioxythiophene (being abbreviated as PEDOT), because its oxide has very high conductivity, therefore this polymer is widely used in solid electrolytic capacitor, and Organic Light Emitting Diode (OLED), in many electronic devices such as organic solar batteries and organic field-effect tube.
The electrolyte that uses the conducting polymer slurry to make electrolytic capacitor has a lot of methods, the most frequently used is the method for dipping, the tantalum piece is slowly immersed in slurry, at high temperature dry again after dipping a period of time, thus form one deck conducting polymer on the dielectric oxide film surface.
Use low viscous slurry I in certain environment after drying, the conductance of the film of the conducting polymer that forms is greater than 10S/cm, than better suited be greater than 20S/cm, more suitably greater than 50S/cm, be more preferably greater than 100S/cm, even 200S/cm or 1000S/cm.
The first conducting polymer rete forms the electrolytical internal layer of electric conductive polymer, forms intermediate adhesion layer on the first conducting polymer rete.By forming such structure, can obviously improve the tack between dielectric layer and electroconductive polymer dielectric substrate, improve the ability of the anti-mechanical strength of electroconductive polymer dielectric substrate and anti-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 ethyl ester copolymer, 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., preferred bonding effect is polyethylene glycol preferably.
in addition, contain the conduction reinforcing agent in the solution of intermediate adhesion layer, comprise oxolane, the compound of lactone functional group is (as gamma-butyrolacton, gamma-valerolactone etc.), amino or lactams functional compounds are (as caprolactam, the N-methyl caprolactam, N, the N-dimethylacetylamide, the 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, the N-methyl nitrosourea, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), and sorbierite is preferred conductivity reinforcing agent, preferred DMSO is as the conduction reinforcing agent.Be the material of ionic conduction because of polyethylene glycol, thereby form the dielectric substrate that mixes between polymer film, therefore, can reduce residual current and ESR in electrolyte.
Beneficial effect of the present invention is: the surface at the tantalum piece forms dielectric oxide film by electrochemical method, with silane coupler, activation processing is carried out on the dielectric oxide film surface, at dielectric oxide film surface-coated the first conducting polymer rete, apply intermediate adhesion layer on the first conducting polymer rete, make the second conducting polymer rete on intermediate adhesion layer, improved the electrical quantity characteristic of solid electrolytic capacitor, ESR and leakage current have been reduced, improve the puncture voltage of capacitor, increased simultaneously the stability of capacitor in high frequency and hyperbaric environment.
Embodiment
Further describe technical scheme of the present invention below in conjunction with embodiment, but that claimed scope is not limited to is described.
Embodiment 1
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 10% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 5min, then dry 20min in the air ambient of 35 ℃, then in the air ambient of 200 ℃ dry 60min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 100 ℃ dry 30min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 30min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 25mPa.s conducting polymer slurry II, dip time is 5min, then dry 30min in the air ambient of 35 ℃, dry 40min in the air ambient of 180 ℃, repeat this process 5 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, 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 reinforcing agent, and wherein adhesive is 0.1% of water content, and the conduction reinforcing agent is 0.01% of water content.
Comparative examples 1
The tantalum piece that generates dielectric layer is immersed dipping p-methyl benzenesulfonic acid solution 5min, flood again 3,4-vinyl dioxy thiophene (EDOT) monomer solution 5min, at 25～30 ℃, relative humidity is polymerization reaction take place 60min in 30%～70% air ambient, then washes remaining monomer and byproduct of reaction, thereby reoxidize the deielectric-coating surface, forms 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 mold pressing encapsulation, finally the electrical quantity of capacitor is measured.
Comparative examples 2
In embodiment 1, the tantalum piece is not covered with the 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 mold pressing encapsulation, finally the electrical quantity of capacitor is measured.
Comparative examples 3
In embodiment 1, the tantalum piece 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 mold pressing encapsulation, finally the electrical quantity of capacitor is measured.
Comparative examples 4
In embodiment 1, activation processing is carried out with silane coupler in tantalum piece surface, then at active layer surface-coated conducting polymer rete I and conducting polymer rete II.Then carry out spot welding, bonding and mold pressing encapsulation.Finally the electrical quantity of capacitor is measured.
Comparative examples 5
In embodiment 1, the tantalum piece that generates dielectric layer is immersed dipping p-methyl benzenesulfonic acid solution 5min, flood again 3,4-vinyl dioxy thiophene (EDOT) monomer solution 5min, at 25～30 ℃, relative humidity is polymerization reaction take place 60min in 30%～70% air ambient, then washes remaining monomer and byproduct of reaction, thereby reoxidize the deielectric-coating surface and form one deck conducting polymer thin film (PEDOT), this process repeats 6 times.The anode block that will be covered with again conducting polymer thin film immerses the slurry of conducting polymer, forms certain thickness polyelectrolyte floor.The product of drying is immersed respectively graphite and silver slurry.Then carry out spot welding, bonding and mold pressing encapsulation, finally the electrical quantity of capacitor is measured.
Table 1 embodiment 1,2 and Comparative Examples 1,2,3, the contrast of 4 performance parameter
As seen, example 1 and example 2 have improved the electrical quantity characteristic of solid electrolytic capacitor, have reduced ESR and leakage current, have improved the puncture voltage of capacitor, have increased simultaneously the stability of capacitor in high frequency and hyperbaric environment.
Embodiment 2
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 60% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 2min, then dry 30min in the air ambient of 25 ℃, then in the air ambient of 250 ℃ dry 30min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 80 ℃ dry 40min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 40min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 12mPa.s conducting polymer slurry II, dip time is 10min, then dry 30min in the air ambient of 25 ℃, dry 30min in the air ambient of 200 ℃, repeat this process 3 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, 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 reinforcing agent, and wherein adhesive is 0.3% of water content, and the conduction reinforcing agent is 0.1% of water content.
Embodiment 3
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 0.03% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 10min, then dry 10min in the air ambient of 50 ℃, then in the air ambient of 120 ℃ dry 90min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 150 ℃ dry 20min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 20min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 35mPa.s conducting polymer slurry II, dip time is 2min, then dry 10min in the air ambient of 50 ℃, dry 60min in the air ambient of 80 ℃, repeat this process 5 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, 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 reinforcing agent, and wherein adhesive is 0.03% of water content, and the conduction reinforcing agent is 0.01% of water content.
Embodiment 4
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 20% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 8min, then dry 15min in the air ambient of 40 ℃, then in the air ambient of 180 ℃ dry 70min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 120 ℃ dry 25min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 35min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 24mPa.s conducting polymer slurry II, dip time is 5min, then dry 25min in the air ambient of 30 ℃, dry 40min in the air ambient of 150 ℃, repeat this process 4 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, 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 reinforcing agent, and wherein adhesive is 0.15% of water content, and the conduction reinforcing agent is 0.05% of water content.
Embodiment 5
A kind of manufacture for solid electrolytic capacitor with high-breakdown-voltage, it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 6% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta205 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 7min, then dry 14min in the air ambient of 45 ℃, then in the air ambient of 210 ℃ dry 50min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed 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 ℃, then in the air ambient of 140 ℃ dry 30min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 40min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 28mPa.s conducting polymer slurry II, dip time is 8min, then dry 28min in the air ambient of 34 ℃, dry 50min in the air ambient of 120 ℃, repeat this process 5 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
In described step (1), direct current adopts the direct voltage of 55V.
Described silane coupler dilution is by adding end dilution agent to form in silane coupler, 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 reinforcing agent, and wherein adhesive is 0.2% of water content, and the conduction reinforcing agent is 0.08% of water content.
Claims (6)
1. manufacture for solid electrolytic capacitor with high-breakdown-voltage, it is characterized in that: it comprises following steps:
(1), the tantalum piece after sintering is placed in concentration is 0.03%-60% phosphoric acid solution, logical direct current then, by electrochemical reaction until on tantalum piece surface, form unbodied Ta2O5 dielectric layer;
(2), activation processing: the tantalum piece that generates dielectric layer immerses the silane coupler dilution, dip time is 2-10min, then dry 10～30min in the air ambient of 25～50 ℃, then in the air ambient of 120～250 ℃ dry 30～90min until tantalum piece surface forms the surface active layer;
(3), form the first conducting polymer rete: the tantalum piece that will be covered with the surface active layer is immersed in the mixed liquor of silane coupler and conducting polymer slurry I, the viscosity of mixed liquor is 10～20mPas's, dip time is 2-10min, then dry 10～30min in the air ambient of 25～50 ℃, then in the air ambient of 80～150 ℃ dry 20-40min until be covered with the first conducting polymer rete on the surface active layer;
(4), form intermediate adhesion layer: the tantalum piece 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 ℃ dry 20-40min;
(5), form the second conducting polymer rete: the tantalum piece immersion viscosity that will be covered with intermediate adhesion layer is 12～35mPas conducting polymer slurry II, dip time is 2-10min, then dry 10～30min in the air ambient of 25～50 ℃, dry 30-60min in the air ambient of 80～200 ℃, repeat this process 3～5 times until be covered with the second conducting polymer rete on the surface active layer again;
(6), the product of drying is immersed respectively graphite and silver slurry, then carry out spot welding, bonding and mold pressing encapsulation.
2. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, is characterized in that: the direct voltage of direct current employing 55V in described step (1).
3. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, it is characterized in that: described silane coupler dilution is by adding end dilution agent to form in silane coupler, the diluted concentration of silane coupler is 0.1%～30%, and end agent is a kind of or mixed liquor of alcohols, deionized water.
4. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, it 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.
5. the manufacture for solid electrolytic capacitor with high-breakdown-voltage according to claim 1, it is characterized in that: described slurry is mixed by water, adhesive and conduction reinforcing agent, wherein adhesive is 0.03～0.3% of water content, and the conduction reinforcing agent is 0.01～0.1% of water content.
6. 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: 0.5-10% conductive polymer particles,, 2-66% polymerization anion, the dispersant surplus, wherein, the particle diameter of the conductive polymer particles of conducting polymer slurry II, the solid content in slurry and viscosity are all greater than the particle diameter of conducting polymer slurry I, solid content and viscosity in slurry.
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| CN103854868A (en) * | 2014-03-12 | 2014-06-11 | 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 suitable for high nominal voltage higher than 75V |
| 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 |
| CN104008883A (en) * | 2014-06-20 | 2014-08-27 | 重庆工商大学 | High-conductivity flexible composite catholyte preparing method |
| CN105609313A (en) * | 2016-01-13 | 2016-05-25 | 深圳顺络电子股份有限公司 | Manufacturing method for cathode guide layer of chip-type conductive polymer tantalum capacitor |
| CN109961955A (en) * | 2017-12-25 | 2019-07-02 | 钰邦科技股份有限公司 | Capacitor packaging structure and its manufacturing method with functional coating |
| 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 |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103854868A (en) * | 2014-03-12 | 2014-06-11 | 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 suitable for high nominal voltage higher than 75V |
| 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 |
| CN104008883A (en) * | 2014-06-20 | 2014-08-27 | 重庆工商大学 | High-conductivity flexible composite catholyte preparing method |
| CN104008883B (en) * | 2014-06-20 | 2016-07-27 | 重庆工商大学 | High conductivity flexible compound catholyte preparation method |
| CN105609313A (en) * | 2016-01-13 | 2016-05-25 | 深圳顺络电子股份有限公司 | Manufacturing method for cathode guide layer of chip-type conductive polymer tantalum capacitor |
| 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 packaging structure and its manufacturing method with functional coating |
| 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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