CN106952730B - A kind of tantalum capacitor manganese dioxide is by covering liquid and preparation method thereof - Google Patents
A kind of tantalum capacitor manganese dioxide is by covering liquid and preparation method thereof Download PDFInfo
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- CN106952730B CN106952730B CN201710168652.XA CN201710168652A CN106952730B CN 106952730 B CN106952730 B CN 106952730B CN 201710168652 A CN201710168652 A CN 201710168652A CN 106952730 B CN106952730 B CN 106952730B
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- tantalum capacitor
- manganese dioxide
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- covering liquid
- alcohol
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- 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
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- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
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- 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
- H01G9/15—Solid electrolytic capacitors
-
- 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
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G2009/05—Electrodes or formation of dielectric layers thereon characterised by their structure consisting of tantalum, niobium, or sintered material; Combinations of such electrodes with solid semiconductive electrolytes, e.g. manganese dioxide
Abstract
The invention discloses a kind of tantalum capacitor manganese dioxide by covering liquid and preparation method thereof, including：Prepare the manganese nitrate aqueous solution of 50~56wt%；The nonionic surfactant of 0.01~0.2wt% is added into manganese nitrate solution, is evenly stirred until dissolving；The water-soluble thinner of 0.01~0.1wt% is added into manganese nitrate solution again, is evenly stirred until dissolving；Continue the water-soluble alcohol that 1~2.5wt% is added into manganese nitrate solution, is evenly stirred until dissolving.Tantalum capacitor manganese dioxide prepared by the present invention can be reduced to 1.2 × 10 by covering liquid, surface tension‑2~1.5 × 10‑2N/m (25 DEG C), viscosity can be reduced to 0.6~1.2cp (25 DEG C), micropore wetting capacity greatly improves, manganese nitrate solution only needs dipping/thermal decomposition primary, the manganese dioxide cathodes of enough area can be layed onto, capacity extraction rate is made to reach 90% or more, while ensureing tantalum capacitor electrical property, production technology can significantly be simplified, improve production efficiency.
Description
Technical field
The invention belongs to solid tantalum capacitor manufacturing technology fields, and in particular to coating dioxy in tantalum capacitor production process
Change manganese cathode needed for by covering liquid and preparation method thereof.
Background technology
In recent years, all kinds of military-civil electronic products are all towards the development of slim, light-duty and miniaturization, and this requires productions
The component that product use realizes miniaturization.The remarkable advantage of solid tantalum capacitor is capacity greatly and can be easily made small-sized and piece type
Element, in addition, also low-leakage current, low-loss, long-life, good stability the features such as, thus obtained in each electronic product
Extensive use especially has consequence in national defences such as Aeronautics and Astronautics, guided missile, satellite, radars.
In solid tantalum capacitor production technology, have one it is important by membrane process, refer to through anode treated tantalum block,
Manganese nitrate solution is impregnated, then manganese nitrate is decomposed to form the processes of manganese dioxide cathodes, manganese nitrate used in hygrothermal environment
Solution is known as by covering liquid.It is very big on the influence of the electrical property of the preparation of cathode manganese dioxide and capacitor by covering liquid, if nitric acid
The excessive concentration of manganese solution is then big by the surface tension of covering liquid, viscosity is high.
By covering liquid surface tension, then wetting capacity is low greatly, and when dipping can not fill up tantalum anode micropore, then manganese nitrate heat point
Filling rate of the manganese dioxide generated in tantalum anode micropore is solved with regard to low, effective cathode area is just smaller than annode area, capacitance
The capacity extraction rate (the ratio between product actual capacity and design capacity) of device is just low.In addition, coating fluid viscosity is excessively high, will cause to be dehydrated
The bubble generated with thermal decomposition is not easy to exclude, the rupture of manganese dioxide film layer, the compactness of cathodic coating is reduced, again such that capacity draws
Extracting rate reduces.Thus, current is all the envelope in such a way that dipping/thermal decomposition is repeated several times in low concentration by membrane process.Such as, exist
Liu Yong just et al. written by《The improvement of 35V47 μ F solid tantalum capacitor preparation processes》In, it is density 1.2g/cm3 nitre by membrane process
Sour manganese solution envelope 3 times, the manganese nitrate solution envelope of density 1.5g/cm3 and 1.7g/cm3 4~5 times.《Effect of
addition of silver compounds during the pyrolysis of manganese nitate on
tantalum anodic oxide film》In, six nitroxylic acid manganese solutions dipping and heat is repeated in Takeyuki Gotoh
Decomposable process.In Chinese patent 201610719935.4, Wang Xunguo etc. artificially forms cathode manganese dioxide layer, repeated impregnations 12
The manganese nitrate solution of~18 1.2~1.5g/cm3.Bear knows jasmine et al. and exists《The influence that ethyl alcohol thermally decomposes manganese nitrate》In mention,
Ethanol in proper amount is added into manganese nitrate solution can reduce solution surface tension, but solution table when ethyl alcohol additive amount is 4% under room temperature
Face tension just drops to 6.0 × 10-2N/m, and ethyl alcohol, which is added, makes solution viscosity increase, wetting capacity improves not notable, dipping time
Unobvious are reduced, in addition, ethyl alcohol additive amount is crossed at most volatile, are cannot keep in tantalum capacitor production technology by covering liquid component
Stabilization.
It can thus be seen that if the surface tension and viscosity of high concentration manganese nitrate solution can be reduced, its wetting capacity is improved,
The especially wetting capacity of micropore, and ensure the compactness of cathodic coating, so that it may to greatly reduce the dipping of manganese nitrate solution
Number simplifies production technology, improves production efficiency, has important practical significance.
Invention content
To solve the above problems, the present invention provides a kind of tantalum capacitor manganese dioxide by covering liquid and preparation method thereof.
It is found when studying this by covering liquid and preparation method thereof：
1. being unfavorable for infiltrating tantalum anode micropore by bubble is generated in covering liquid, and it is unfavorable for forming fine and close manganese dioxide film layer；
2. surfactant plays the role of significantly reducing manganese nitrate solution surface tension, but anion surfactant is easy
Bubble is generated, and is not easy to eliminate, in contrast, fatty alcohol polyoxyethylene ether is not likely to produce bubble, and boiling point is mostly on 100 DEG C of left sides
The right side has been volatilized before manganese nitrate thermal decomposition is completed, and will not remain influences electrical property in cathode；
3. water-soluble thinner can significantly reduce manganese nitrate aqueous solution viscosity；
4. water-soluble alcohol has defoaming effect, while can also further decrease surface tension.
Based on above-mentioned discovery, technical solution of the present invention can be described as：
A kind of tantalum capacitor manganese dioxide provided by the invention is included the following steps by covering liquid and preparation method thereof：
(1) a certain amount of 70wt% manganese nitrate solutions and deionized water are taken, the cathode for preparing 50~56wt% forms liquid nitre
Sour manganese aqueous solution；
(2) surfactant of 0.01~0.2wt% is added into manganese nitrate solution, is evenly stirred until dissolving；
(3) the water-soluble thinner of 0.01~0.1wt% is added into manganese nitrate solution again, is evenly stirred until dissolving；
(4) continue the water-soluble alcohol that 1~2.5wt% is added into manganese nitrate solution, be evenly stirred until dissolving.
Surfactant used in step (2) is alkyl phenol polyoxyethylene ether (JFC-1), sec-octyl alcohol polyoxyethylene ether (JFC-
2), isooctanol polyethoxylate (JFC-3), isomeric alcohol polyethenoxy ether (JFC-E), aliphatic alcohol polyethenoxy (3) ether (AEO3),
Aliphatic alcohol polyethenoxy (5) ether (AEO5), fatty acid methyl ester ethoxylate (FMEE), preferred fat alcohol polyoxyethylene ether,
Structure is：
In formula, R is selected from 7~18 saturated or unsaturated alkyl of carbon atom number, can be straight-chain alkyl, can also be band branch
The alkyl of chain；The integer that n is 1~20.The sec-octyl alcohol polyoxyethylene ether (JFC-2) that most preferably n is 1~6；
The preferred content of surfactant used in step (2) be 0.05~0.18wt%, most preferred content be 0.1~
0.15wt%.
Water-soluble thinner is lignosulfonates, Nonylphenoxy carboxylates salt, AMPS/AA/ used in step (3)
DMDAAC- Lignosulfonate Graft Copolymers thinner, lignosulfonates/organic silicon-fluorine copolymer composite viscosity reducer, it is excellent
Select lignosulfonates, Nonylphenoxy carboxylates salt, most preferably lignosulfonates；
The preferred content of water-soluble thinner used in step (3) is 0.02~0.08wt%, most preferred content is 0.03~
0.05wt%.
Water-soluble alcohol used in step (4) be methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol,
Ethylene glycol, preferred alcohol, the tert-butyl alcohol, ethylene glycol, most preferred ethanol and ethylene glycol mixture；
The preferred content of water-soluble alcohol used in step (4) is 1.5~2.5wt%, and most preferred content is 1.8~2wt%.
For tantalum capacitor manganese dioxide prepared by the present invention by covering liquid, surface tension is reduced to 1.2 × 10-2~1.5 × 10- 2N/m (25 DEG C), viscosity are reduced to 0.6~1.2cp (25 DEG C), and pore impregnation ability greatly improves, and manganese nitrate solution only needs to soak
Stain/thermal decomposition is primary, so that it may be layed onto the cathode manganese dioxide of enough area, so that capacity extraction rate is reached 90% or more and reached
To production requirement, it while ensureing tantalum capacitor electrical property, can significantly simplify production process, improve production efficiency.
Specific implementation mode
Following embodiment be to a kind of tantalum capacitor manganese dioxide of the present invention by covering liquid and preparation method thereof into
One step illustrates, rather than limits the scope of the invention.
Embodiment 1：
Deionized water 40g is weighed in 250ml cleaning beakers, the manganese nitrate solution of 100g70wt% is added, stirs evenly
To dissolving；0.14g sec-octyl alcohols polyoxyethylene ether (JFC-2) is added, is evenly stirred until dissolving；Add 0.05g lignin sulfonic acids
Salt is evenly stirred until dissolving；2.1g absolute ethyl alcohols, 0.7g ethylene glycol are continuously added, is evenly stirred until dissolving to get tantalum capacitor
Then manganese dioxide conventionally carries out envelope, encapsulation, test by covering liquid, acquired results are as shown in table 1.
Embodiment 2,3：
Basic step is with embodiment 1, and it is different by the composition of covering liquid and content that difference lies in manganese dioxide, and concrete composition contains
Amount is as shown in table 1, then conventionally carries out envelope, encapsulation, test, and acquired results are as shown in table 1.
Comparative example：
Comparative example is for illustrating tantalum capacitor manganese dioxide in the prior art by covering liquid.Basic step is the same as embodiment 1, area
It is not that manganese dioxide is different by the composition of covering liquid and content, concrete composition, content are (current by membrane process as shown in table 1
Low concentration manganese nitrate solution can only be used, has been described in detail in background technology), envelope, encapsulation, test are then carried out as embodiment,
Acquired results are as shown in table 1.
Table 1 is by covering liquid composition and effect
Claims (10)
1. a kind of tantalum capacitor manganese dioxide is by the preparation method of covering liquid, and in particular to prepare coating in tantalum capacitor production process
Liquid manganese nitrate aqueous solution is formed by covering liquid, including the cathode of 50~56wt% of preparation needed for manganese dioxide cathodes；Toward manganese nitrate
The surfactant of 0.01~0.2wt% is added in solution so that surface tension significantly reduces, and impregnability greatly improves；Again
The water-soluble thinner of 0.01~0.1wt% is added into manganese nitrate solution, solution viscosity can be significantly reduced；Continue to manganese nitrate
The water-soluble alcohol of 1~2.5wt% is added in solution, has defoaming effect, can also further decrease surface tension.
2. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that table used
Face activating agent is alkyl phenol polyoxyethylene ether (JFC-1), sec-octyl alcohol polyoxyethylene ether (JFC-2), isooctanol polyethoxylate
(JFC-3), isomeric alcohol polyethenoxy ether (JFC-E), aliphatic alcohol polyethenoxy (3) ether (AEO3), aliphatic alcohol polyethenoxy (5) ether
(AEO5), fatty acid methyl ester ethoxylate (FMEE).
3. a kind of tantalum capacitor manganese dioxide according to claim 2 is by the preparation method of covering liquid, characterized in that the table
The preferred sec-octyl alcohol polyoxyethylene ether (JFC-2) of face activating agent.
4. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that table used
The preferred content of face activating agent is 0.1~0.15wt%.
5. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that water used
Dissolubility thinner is that lignosulfonates, Nonylphenoxy carboxylates salt, AMPS/AA/DMDAAC- lignosulfonates connect
Graft copolymer thinner, lignosulfonates/organic silicon-fluorine copolymer composite viscosity reducer.
6. a kind of tantalum capacitor manganese dioxide according to claim 5 is by the preparation method of covering liquid, characterized in that the water
The preferred lignosulfonates of dissolubility thinner.
7. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that water used
The preferred content of dissolubility thinner is 0.03~0.05wt%.
8. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that water used
Dissolubility alcohol is methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol, sec-butyl alcohol, the tert-butyl alcohol, ethylene glycol.
9. a kind of tantalum capacitor manganese dioxide according to claim 8 is by the preparation method of covering liquid, characterized in that the water
The composition of dissolubility alcohol preferred alcohol and ethylene glycol.
10. a kind of tantalum capacitor manganese dioxide according to claim 1 is by the preparation method of covering liquid, characterized in that used
The preferred content of water-soluble alcohol is 1.5~2wt%.
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| CN106952730B true CN106952730B (en) | 2018-10-16 |
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| CN109300695B (en) * | 2018-11-06 | 2020-10-16 | 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) | Cathode of low ESR tantalum electrolytic capacitor and preparation method thereof |
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| US4945452A (en) * | 1989-11-30 | 1990-07-31 | Avx Corporation | Tantalum capacitor and method of making same |
| JPH0722285A (en) * | 1993-06-22 | 1995-01-24 | Matsushita Electric Ind Co Ltd | Production of solid electrolytic capacitor |
| US20040231119A1 (en) * | 2003-05-21 | 2004-11-25 | Brenneman Keith R. | Method of electrolytic deposition of an intrinsically conductive polymer upon a non-conductive substrate |
| JP5933397B2 (en) * | 2012-08-30 | 2016-06-08 | エイヴィーエックス コーポレイション | Solid electrolytic capacitor manufacturing method and solid electrolytic capacitor |
| GB2516529B (en) * | 2013-05-13 | 2018-08-29 | Avx Corp | Solid electrolytic capacitor containing a multi-layered adhesion coating |
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