CN108962421A - A kind of impregnated silver pulp and tantalum capacitor - Google Patents
A kind of impregnated silver pulp and tantalum capacitor Download PDFInfo
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- CN108962421A CN108962421A CN201710369904.5A CN201710369904A CN108962421A CN 108962421 A CN108962421 A CN 108962421A CN 201710369904 A CN201710369904 A CN 201710369904A CN 108962421 A CN108962421 A CN 108962421A
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- graphite
- impregnated
- silver
- tantalum
- pulp
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
Abstract
The invention discloses a kind of impregnated silver pulp and tantalum capacitor, by percentage to the quality, raw material includes following components to the impregnated silver pulp: fluoropolymer resin carrier 4~18%；Silver powder 27~50%；Graphite 1~8%；Carbon black 1~8%；Solvent 42~70%.The tantalum capacitor, including tantalum core, and the graphite linings and silver layer that are covered on tantalum core, the graphite linings are prepared by the impregnated graphite slurry, and the silver layer is prepared by the impregnated silver pulp.Impregnated graphite slurry and impregnated silver pulp in the present invention, organic matter has ingredient similar, compatibility is preferable and solidification temperature is consistent, it is carried out on dipping and curing process modified, so that forming certain transition zone between silver layer and graphite linings after solidifying, the big adhesive force of interfacial mechanical strength is good, refractory molded ability is strong, and conductive particle contact is good, job resistance is small.That the invention enables silver layer and graphite linings overlap joints is good, contact interface resistance is small, so that the ESR of tantalum capacitor be greatly lowered.
Description
Technical field
The invention belongs to technical field of electronic devices, and in particular to a kind of impregnated silver pulp and tantalum capacitor.
Background technique
Since tantalum capacitor is found, be always the basic device that is most widely used in electronics industry it
One, it is widely applied in various types of electronic circuits.In nineteen fifty-five, the wheat Courlene of AT&T Labs of the U.S.
(D.McLean) and Bauer (F.Power) successfully develops first solid electrolyte Ta capacitor of industry, is with manganese dioxide
For electrolyte, the problem of not only overcoming liquid electrolyte " desiccation ", but also greatly improve its stability characteristic (quality) and frequency is special
Property, solid foundation has been established for the business application of tantalum capacitor in the future.
Tantalum capacitor is good etc. excellent because itself having large capacity, low-leakage current, long-life, miniaturization, low-loss, stability
Good feature, so that no matter it is in the civilian neck such as phone, colour TV, refrigerator, Video Camera, digital camera, programme-controlled exchange, computer
Domain is still all widely applied in national defences such as Aeronautics and Astronautics, guided missile, satellite, radars, especially in national defence
Using the development for accelerating tantalum capacitor, new step has been marched toward.
ESR (Equivalent series Resistance) i.e. equivalent series resistance, ESR=Ra+Rb+Rc, wherein RaIt is
It is related with tantalum pentoxide dielectric oxide film that it is lost by the resistance and film and MnO of tantalum pentoxide film2Contact resistance,
RbIt is MnO inside tantalum block2Resistance, RcIt is tantalum block appearance MnO2And Conductive graphite cream, polymer silver paste etc. resistance and mutually
Between contact resistance.With the development of electronic technology and electronic component, low-power consumption and high speed processing are modern electronic equipments
Developing direction, to tantalum capacitor performance, more stringent requirements are proposed, wherein low ESR tantalum capacitor is exactly a research hot topic.
The manufacturer of domestic external capacitive body has all been the ESR (equivalent series resistance) for reducing capacitor and has largely ground
Study carefully, but compared to external capacitor producer, studies in China is later, development speed is slow, and the ESR value of the low ESR tantalum capacitor of manganese systems is basic
More than 40m Ω.External low ESR tantalum capacitor then has reached preferable level, such as: AVX Corp. releases low ESR value
Chip tantalum capacitor series " TPS Series III "；Vishay company also releases the chip of the low ESR value of 0603 type of minimum shell number
Tantalum capacitor " MicroTan-TR8 " series, the ESR value of product is down to 25m Ω or so.But low ESR tantalum capacitor is reducing
Still there is also many shortcomings in terms of ESR, still need to further perfect.So reducing the ESR of tantalum capacitor to greatest extent
It is current one of tantalum capacitor manufacturing industry primary study project both at home and abroad, is of great significance.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of immersion silver, so that silver layer and graphite linings overlap joint are good, contact
Interface resistance is small, so that the ESR of tantalum capacitor be greatly lowered.
The technical solution of the present invention is as follows: a kind of impregnated silver pulp, by percentage to the quality, raw material includes following components:
Fluoropolymer resin carrier 4~18%；Silver powder 27~50%；Graphite 1~8%；Carbon black 1~8%；Solvent 42~
70%.
Preferably, the solvent is tributyl citrate, butyl acetate, ethyl caprilate, ethyl acetate, acetic acid positive penta
Ester, butyl glycol ether, 2-Butoxyethyl acetate, polyamide wax, tetraethyl titanate, terpinol, butyl carbitol acetate, second
One of ethyl acetoacetic acid ethyl ester and methylimidazole are a variety of.
Preferably, the fluoropolymer resin carrier be one of acrylic resin, epoxy resin and fluorubber or
It is a variety of.
Preferably, the following steps are included: first by solvent dissolve fluoropolymer resin carrier, add silver powder, graphite with
And carbon black, and 6~12h is stirred with 100~300rpm/min and obtains the impregnated silver pulp of 300~1000cp of range of viscosities.
The present invention also provides a kind of tantalum capacitors, including tantalum core and the silver layer being covered on tantalum core, which is characterized in that institute
Silver layer is stated to be prepared by above-mentioned impregnated silver pulp.
Preferably, further include the graphite linings being covered on tantalum core, by percentage to the quality, the raw material packet of the graphite linings
Include following components:
Conducting particles 4~15%；
Fluoropolymer resin carrier 4~20%；
Solvent 70~92%.
Preferably, the conducting particles is made of graphite and carbon black, the mass ratio of the graphite and carbon black be 1:0.3~
1:0.7。
Preferably, the fluoropolymer resin carrier be one of acrylic resin, epoxy resin and fluorubber or
It is a variety of.
Preferably, the solvent is tributyl citrate, butyl acetate, ethyl caprilate, ethyl acetate, acetic acid positive penta
Ester, butyl glycol ether, 2-Butoxyethyl acetate, polyamide wax, tetraethyl titanate, terpinol, butyl carbitol acetate, second
One of ethyl acetoacetic acid ethyl ester and methylimidazole are a variety of.
For tantalum capacitor, ESR mainly includes three parts, first is that related with tantalum pentoxide dielectric oxide film
R is lost1, including the equivalent resistance and film that are generated by tantalum pentoxide film and MnO2Contact resistance, second is that tantalum block inside MnO2
Or the resistance R of conducting polymer2, third is that tantalum block appearance MnO2, electrically conductive graphite layer, conductive silver layer, cathodic metal piece etc. resistance with
And mutual contact resistance R3.Reduction for ESR, wherein R1、R2ESR it is smaller and stablize, be gradually improved at present；And
The ESR of cathode outlet is larger, and unstable, and be significantly improved space.Therefore, in R1And R2In the case where immobilizing, this hair
The bright desired ESR for reducing tantalum capacitor, by reducing R3Mode realize, that is, reduce impregnated graphite slurry and impregnated silver pulp
Between contact resistance, the contact interface both improved guarantees there is good overlap joint therebetween, between the two to reduce
Contact resistance.
Compared with prior art, the beneficial effects of the present invention are embodied in:
(1) impregnated graphite slurry and impregnated silver pulp, organic matter have that ingredient is similar in the present invention, and compatibility is preferably and solidification temperature
Unanimously, carried out on dipping and curing process it is modified so that form certain transition zone between silver layer and graphite linings after solidifying,
The big adhesive force of interfacial mechanical strength is good, refractory molded ability is strong, and conductive particle contact is good, job resistance is small.
(2) with impregnated silver pulp compared with external import slurry, electric conductivity differs not impregnated graphite slurry provided by the invention
Greatly, but the interface resistance with respect under between the two wants much lower, and interface ESR is reduced to 9m by original the above of 15m Ω
Ω prepares impregnated graphite slurry and impregnated silver pulp hereinafter, therefore, using the present invention, and the ESR of tantalum capacitor can be greatly lowered, comprehensive
Conjunction is had excellent performance, and is worth to the industrialized production of ultralow ESR solid electrolytic tantalum capacitor with important practical.
Detailed description of the invention
Fig. 1 is tantalum capacitor enlarged section before being molded in the present invention.
Fig. 2 is that graphite and silver interface SEM scheme after the molding of tantalum capacitor sample in the present invention.
Fig. 3 is graphite and silver-colored Interface Microstructure figure in the present invention.
Fig. 4 is graphite and silver-colored interface 3D scanning figure in the present invention.
Fig. 5 is graphite and silver layer figure near silver-colored interface in the present invention.
Fig. 6 is graphite and silver layer constituent analysis figure near silver-colored interface in the present invention.
Fig. 7 is graphite and graphite linings figure near silver-colored interface in the present invention.
Fig. 8 is graphite and graphite linings constituent analysis figure near silver-colored interface in the present invention.
Specific embodiment
Embodiment 1
(1) preparation of impregnated graphite slurry and impregnated silver pulp
The preparation of impregnated graphite slurry: by conducting particles, acrylic resin carrier and volume according to mass ratio, conducting particles:
Acrylic resin carrier: solvent=7:9:84 carries out ingredient, and wherein conducting particles is made of graphite and carbon black, mass ratio 5:3；
Solvent be butyl glycol ether, tributyl citrate and 2-Butoxyethyl acetate composition mixed solvent, ratio of components 45:30:
25, raw material specification is as shown in table 1.The mixed solvent for first weighing 1/3 first dissolves load weighted acrylic resin, to be dissolved complete
After complete, it is gradually added into conducting particles under conditions of 100~300rpm/min stirring, after adding conducting particles, is stirred for half
A hour is until be uniformly mixed, obtained primary black lead wash；Then primary black lead wash is rolled by three-high mill, reaches fineness <
5 μm, remaining solvent is finally added in the black lead wash of rolling, obtains the impregnated graphite slurry of 300~1000cp of range of viscosities, and
Impregnated graphite is starched and carries out resistivity measurement.
The preparation of impregnated silver pulp: preparing, acrylic resin carrier 5~15%, silver powder 32~45% according to mass ratio formula,
Graphite 1~5%, carbon black 1~4%, solvent portion be tetraethyl titanate 0.3%, methylimidazole 0.1%, polyamide wax 0.3%,
Butyl acetate 30~52%, 2-Butoxyethyl acetate 13~20%.Concrete technology is first to be carried with solvent dissolution acrylic resin
Body adds conducting particles, and 100~300rpm/min stirs 6~12h and obtains the impregnated silver pulp of 300~1000cp of range of viscosities,
And resistivity measurement is carried out to impregnated silver pulp.
1 experimental raw of table and specification
(2) tantalum core dipping, solidification and test
After completing envelope and impregnating the tantalum core progress ESR test of watersoluble plumbago slurry, dipping prepared by impregnation steps (1)
Black lead wash and impregnated silver pulp, first impregnated graphite are starched, and first hang 5min at room temperature after dipping, then 20min is warming up to 120 DEG C of guarantors
Warm 20min carries out precuring, and then impregnated silver pulp, hangs 5min at room temperature, and 20min is warming up to 120 DEG C of heat preservation 20min temperature
Precuring is carried out, last tantalum core is divided into 2 batches, and a batch is warming up to 210 DEG C of heat preservation 60min and is solidified, and a batch is warming up to 240 DEG C of guarantors
Warm 60min is solidified, and carries out ESR test to tantalum core respectively, obtains the interface ESR between graphite and silver layer.
Embodiment 2
The preparation of impregnated graphite slurry: by conducting particles, acrylic resin carrier and volume according to mass ratio, conducting particles:
Epoxy resin carrier: solvent=8:10:82 carries out ingredient, and wherein conducting particles is made of graphite and conductive black, and mass ratio is
3:2；Solvent be butyl click must alcohol, butyl carbitol acetate, n-amyl acetate, ethyl acetoacetate, ratio of components 35:19:
32:14, raw material specification are as shown in table 1.The mixed solvent for first weighing 1/3 first dissolves load weighted epoxy resin, to be dissolved complete
After complete, it is gradually added into conducting particles under conditions of 100~300rpm/min stirring, after adding conducting particles, is stirred for half
A hour is until be uniformly mixed, obtained primary black lead wash；Then primary black lead wash is rolled by three-high mill, reaches thin
5 μm of < of degree, remaining 2/3 solvent is finally added in the black lead wash of rolling, obtains the dipping stone of 300~1000cp of range of viscosities
Ink slurry, and impregnated graphite is starched and carries out resistivity measurement.
The preparation of impregnated silver pulp: it is prepared according to mass ratio formula, epoxy resin carrier 5~15%, silver powder 32~42%, stone
Ink 1~5%, carbon black 1~4%, solvent portion are tetraethyl titanate 0.3%, methylimidazole 0.1%, polyamide wax 0.3%, vinegar
Acid butyl ester 20~35%, n-amyl acetate 5~15%, ethyl acetoacetate 5~15%.Concrete technology is first with solvent dissolution third
Olefin(e) acid resin carrier, adds conducting particles, and 100~300rpm/min stirs 6~12h and obtains 300~1000cp of range of viscosities
Impregnated silver pulp, and to impregnated silver pulp carry out resistivity measurement.
Tantalum core dipping, solidification and test operating procedure are the same as embodiment 1.
Embodiment 3
The preparation of impregnated graphite slurry: by conducting particles, acrylic resin carrier and volume according to mass ratio, conducting particles:
Fluoropolymer resin carrier: solvent=6:7:87 carries out ingredient, and wherein conducting particles is made of watersoluble plumbago and conductive black, quality
Than for 5:3；Solvent is the mixed solvent of butyl glycol ether, n-amyl acetate and 2-Butoxyethyl acetate composition, and ratio of components is
50:25:25, fluoropolymer resin are made of acrylic resin and fluorubber, ratio 5:5, and raw material specification is as shown in table 1.First
The mixed solvent for weighing 1/3 first dissolves load weighted fluoropolymer resin, it is to be dissolved completely after, in 100~300rpm/min
It is gradually added into conducting particles under conditions of stirring, after adding conducting particles, continues to stir half an hour up to being uniformly mixed, is made
Primary black lead wash；Then primary black lead wash is rolled by three-high mill, reaches 5 μm of fineness <, finally in the stone of rolling
Ink slurry in add remaining 2/3 solvent, obtain 300~1000cp of range of viscosities impregnated graphite slurry, and to impregnated graphite starch into
Row resistivity measurement.
The preparation of impregnated silver pulp: preparing, silver powder 34~44%, fluoropolymer resin carrier 8~12% according to mass ratio formula,
Graphite 1~2%, carbon black 1~2%, solvent group become tetraethyl titanate 0.3%, methylimidazole 0.1%, polyamide wax 0.3%,
Terpinol 10%, butyl acetate 28~40%, 2-Butoxyethyl acetate 8~20%, wherein fluoropolymer resin carrier is by propylene
Acid resin and fluorubber composition, mass ratio 5:5.Concrete technology is first to dissolve fluoropolymer resin carrier with solvent, adds and leads
Charged particle, 100~300rpm/min stir 6~12h and obtain the impregnated silver pulp of 300~1000cp of range of viscosities, and to immersion silver
Slurry carries out resistivity measurement.
Tantalum core dipping, solidification and test specific operation process are the same as embodiment 1.
Comparative example 1
Using imported from America impregnated silver pulp and the impregnated graphite slurry of Japanese import, to completion envelope and dipping watersoluble plumbago slurry
Tantalum core carry out ESR test after, impregnated graphite is starched first, and 30min is warming up to 210 DEG C of heat preservation 60min and is solidified after dipping, so
Impregnated silver pulp afterwards, tantalum core are divided into 2 batches, and a collection of 30min is warming up to 210 DEG C of heat preservation 60min and is solidified, and a collection of 30min is warming up to
240 DEG C of heat preservation 60min are solidified, and carry out ESR test to tantalum core respectively, obtain the interface ESR between graphite and silver layer.
The test result of comparative example 1 and 3 embodiments is as shown in table 2:
Interface ESR between 2 tantalum capacitor graphite linings of table and silver layer
As can be found from Table 2, compared with external import impregnated silver pulp and impregnated graphite slurry and application method, due to the present invention
The resin carrier of two kinds of prepared dipping sizing agents is the same, and is carried out in dipping and solidification process bond material performance
Process optimization ensure that between two kinds of heterogeneous conductor paste interfaces there is good contact, and compatibility is fine, silver layer and graphite linings it
Between there are also certain diffusion, so as to cause the interface resistance very little between them, reached the effect for reducing tantalum capacitor interface ESR
Fruit, interface ESR are reduced to 9m Ω or less by original the above of 15m Ω.
In addition, after the hot press moulding plastic packaging for completing tantalum capacitor, to the interfacial microstructure and ingredient of graphite and silver layer
It is tested such as attached drawing 1-8, it will thus be seen that (1) silver layer contacts preferably with the interfacial conductive particle of graphite linings, no hole, layering
And the defects of crack, exists, therefore interface be improved significantly, ESR is significantly reduced；(2) exist between graphite linings and silver layer
More apparent transition zone, the Ag and C distribution of particles in transition zone change linearly, and reduce far from silver layer close to graphite linings Ag, C
Increase, obvious contribution is made in the reduction for existing for interface ESR of the transition zone.
Claims (9)
1. a kind of impregnated silver pulp, which is characterized in that by percentage to the quality, raw material includes following components:
Fluoropolymer resin carrier 4~18%；Silver powder 27~50%；Graphite 1~8%；Carbon black 1~8%；Solvent 42~70%.
2. impregnated silver pulp as described in claim 1, which is characterized in that the solvent is tributyl citrate, butyl acetate, pungent
Acetoacetic ester, ethyl acetate, n-amyl acetate, butyl glycol ether, 2-Butoxyethyl acetate, polyamide wax, tetraethyl titanate, pine
One of oleyl alcohol, butyl carbitol acetate, ethyl acetoacetate and methylimidazole are a variety of.
3. impregnated silver pulp as described in claim 1, which is characterized in that the fluoropolymer resin carrier is acrylic resin, ring
One of oxygen resin and fluorubber are a variety of.
4. the preparation method of the impregnated silver pulp as described in claims 1 to 3 is any, which comprises the following steps: first
Solvent is dissolved into fluoropolymer resin carrier, adds silver powder, graphite and carbon black, and with 100~300rpm/min stirring 6~
12h obtains the impregnated silver pulp of 300~1000cp of range of viscosities.
5. a kind of tantalum capacitor, including tantalum core and the silver layer being covered on tantalum core, which is characterized in that the silver layer is by claim
1~3 any impregnated silver pulp is prepared.
6. tantalum capacitor as claimed in claim 5, which is characterized in that further include the graphite linings being covered on tantalum core, with quality
The raw material of percentages, the graphite linings includes following components:
Conducting particles 4~15%；
Fluoropolymer resin carrier 4~20%；
Solvent 70~92%.
7. tantalum capacitor as claimed in claim 6, which is characterized in that the conducting particles is made of graphite and carbon black, described
The mass ratio of graphite and carbon black is 1:0.3~1:0.7.
8. tantalum capacitor as claimed in claim 6, which is characterized in that the fluoropolymer resin carrier is acrylic resin, ring
One of oxygen resin and fluorubber are a variety of.
9. tantalum capacitor as claimed in claim 6, which is characterized in that the solvent is tributyl citrate, butyl acetate, pungent
Acetoacetic ester, ethyl acetate, n-amyl acetate, butyl glycol ether, 2-Butoxyethyl acetate, polyamide wax, tetraethyl titanate, pine
One of oleyl alcohol, butyl carbitol acetate, ethyl acetoacetate and methylimidazole are a variety of.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710369904.5A CN108962421A (en) | 2017-05-23 | 2017-05-23 | A kind of impregnated silver pulp and tantalum capacitor |
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| CN201710369904.5A CN108962421A (en) | 2017-05-23 | 2017-05-23 | A kind of impregnated silver pulp and tantalum capacitor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114530279A (en) * | 2022-03-30 | 2022-05-24 | 上海腾烁电子材料有限公司 | Low-impedance conductive silver paste for polymer chip tantalum capacitor and preparation method thereof |
| CN116072434A (en) * | 2023-03-02 | 2023-05-05 | 福建火炬电子科技股份有限公司 | Sheet type high polymer tantalum fixed capacitor without humidity sensitivity grade and preparation method thereof |
| CN116072434B (en) * | 2023-03-02 | 2024-05-03 | 福建火炬电子科技股份有限公司 | Sheet type high polymer tantalum fixed capacitor without humidity sensitivity grade and preparation method thereof |
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|---|---|---|---|---|
| JP2014120382A (en) * | 2012-12-18 | 2014-06-30 | Sumitomo Metal Mining Co Ltd | Conductive resin paste and electronic element using the same |
| CN103915133A (en) * | 2014-02-24 | 2014-07-09 | 西北稀有金属材料研究院 | Silver paste for macromolecule solid tantalum electrolytic capacitor and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014120382A (en) * | 2012-12-18 | 2014-06-30 | Sumitomo Metal Mining Co Ltd | Conductive resin paste and electronic element using the same |
| CN103915133A (en) * | 2014-02-24 | 2014-07-09 | 西北稀有金属材料研究院 | Silver paste for macromolecule solid tantalum electrolytic capacitor and preparation method thereof |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114530279A (en) * | 2022-03-30 | 2022-05-24 | 上海腾烁电子材料有限公司 | Low-impedance conductive silver paste for polymer chip tantalum capacitor and preparation method thereof |
| CN116072434A (en) * | 2023-03-02 | 2023-05-05 | 福建火炬电子科技股份有限公司 | Sheet type high polymer tantalum fixed capacitor without humidity sensitivity grade and preparation method thereof |
| CN116072434B (en) * | 2023-03-02 | 2024-05-03 | 福建火炬电子科技股份有限公司 | Sheet type high polymer tantalum fixed capacitor without humidity sensitivity grade and preparation method thereof |
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Application publication date: 20181207 |