CN108962605A - A kind of preparation method of reliable and stable chip tantalum capacitor - Google Patents

A kind of preparation method of reliable and stable chip tantalum capacitor Download PDF

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Publication number
CN108962605A
CN108962605A CN201810676313.7A CN201810676313A CN108962605A CN 108962605 A CN108962605 A CN 108962605A CN 201810676313 A CN201810676313 A CN 201810676313A CN 108962605 A CN108962605 A CN 108962605A
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preparation
tantalum capacitor
nitrogen
reliable
chip tantalum
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CN201810676313.7A
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Chinese (zh)
Inventor
田东斌
龙道学
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China Zhenhua Group Xinyun Electronic Components Co Ltd
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China Zhenhua Group Xinyun Electronic Components Co Ltd
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Priority to CN201810676313.7A priority Critical patent/CN108962605A/en
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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
    • H01G9/07—Dielectric layers
    • 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
    • H01G9/0029—Processes of manufacture
    • H01G9/0032—Processes of manufacture formation of the dielectric layer
    • 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
    • H01G9/0029—Processes of manufacture
    • H01G9/0036—Formation of the solid electrolyte layer
    • 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
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/025—Solid electrolytes
    • H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
    • 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
    • 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

Abstract

The invention belongs to electrolytic capacitor manufacturing technology fields, especially a kind of preparation method of reliable and stable chip tantalum capacitor, it is prepared by anode, chemical conversion, shielding, nitrogen processing, after be melted into, form adhesive layer, polymer electrolytic layer is formed, post-processing, complete by totally nine steps for cooling package, effectively improve dielectric oxide film, the quality of forming film of polymer film, and the bond strength between their interfaces, solve the problems, such as that the problem of high pressure vast capacity organic solid electrolyte chip tantalum capacitor high temperature or temperature punching test static capacity increase substantially and leakage current are gradually overproof at any time, improve the stability and reliability of tantalum electrolytic capacitor.

Description

A kind of preparation method of reliable and stable chip tantalum capacitor
Technical field
The invention belongs to electrolytic capacitor manufacturing technology field, especially a kind of preparation of reliable and stable chip tantalum capacitor Method.
Background technique
With electronic equipment high pressure, miniature and high frequency development, it is desirable that capacitor volume is smaller, and capacity is bigger, electronics The structure and performance of product have changed a lot, and high frequency, high voltage, high power and small size become the following universal elements The Main way of development, however according to this development trend and market needs, design the capacitor of these high pressure vast capacities It is to be not easy very much, usually selects the formation voltage of tantalum powder close to the critical value of its breakdown voltage；Therefore, the shape of such capacitor The problem of at being very difficult to break through, and because the volume of anode bodies is relatively large, conducting polymer slurry is porous intracorporal Permeability is restricted, and fabricated capacitors high temperature Capacitance Shift Rate is overproof, is influenced on the performance of such capacitor very big；Invention People obtains a set of effective method, dielectric formation is both carried out in low temperature environment, in high temperature on the basis of long term test Dielectric tantalum fuse will be formed in steam ambient boil washing, then carries out handling return in nitrogen environment, uses silane idol Join agent and form precoated shet in medium oxidizing film surface, carries out handling return after coating conducting polymer dispersion liquid, height can be improved Press the stability and reliability of vast capacity organic solid electrolyte chip tantalum capacitor.
Summary of the invention
The purpose of the present invention is to provide the raisings of high pressure vast capacity organic solid electrolyte chip tantalum capacitor reliability Method controls the high/low temperature volume change of capacitor, improves the stability of leakage current.
It is achieved particular by following technical scheme:
A kind of preparation method of reliable and stable chip tantalum capacitor, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 5~15 DEG C of electrolyte；
(3) it shields: boiling and wash in high temperature steam environments；
(4) nitrogen is handled: being made annealing treatment in 250-450 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5The precoated shet of dielectric surface formation silane coupling agent；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is nitric acid solution, sulfuric acid solution, any in phosphoric acid solution.
The high temperature is 95 DEG C or more.
Described boil washes the time as 20~600min.
Described boil washes the time as 80~360min.
The pressure of nitrogen is 0.05~1.5MPa in the nitrogen processing, and the processing time is 20~300min.
The pressure of nitrogen is 0.1~1.2MPa in the nitrogen processing, and the processing time is 40~240min.
The preparation method of the reliable chip tantalum capacitor of aforementioned stable, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 5~15 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 20~600min；
(4) nitrogen is handled: annealing 20-300min, nitrogen pressure 0.05- are carried out in 250-450 DEG C of nitrogen environment 1.5MPa；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
Beneficial effect of the present invention
1. dielectric oxide film is handled by three low temperature formation, thermophilic digestion, nitrogen environment annealing steps, it can It is effectively improved the temperature stability of dielectric oxide film, remaining stress in dissolution medium oxidation film is reduced or shielded and is medium oxidizing Film surface and subsurface defect improve the stability of condenser leakage current.
2. improving conducting polymer dispersion liquid big by the precoated shet for forming silane coupling agent in medium oxidizing film surface Permeability in volume anode block.
3. by the post-processing to polymer film, remaining foreign ion in net polymer of volatilizing improves polymer film The temperature stability of layer.
4. the present invention effectively improves between the quality of forming film and their interfaces of dielectric oxide film, polymer film Bond strength, solves high pressure vast capacity organic solid electrolyte chip tantalum capacitor high temperature or temperature punching test static capacity is big The problem of width increases and leakage current gradually overproof problem at any time, improve the stability and reliability of tantalum electrolytic capacitor.
Compliance test result: using 50V-150 μ F as test products, test group is handled product using the method for the present invention, Control group is handled product using normal process method, and every group is randomly selected 30 samples, and tested, and counts its average value, Wherein Δ C=(C-C0)/C0, C0For 25 DEG C of capacity, the result is as follows:
Specific embodiment
Tuberculosis specific embodiment is limited technical solution of the present invention is further below, but claimed Range is not only limited to made description.
Embodiment 1
A kind of preparation method of reliable and stable chip tantalum capacitor, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 5 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 20min；
(4) nitrogen is handled: annealing 20min, nitrogen pressure 0.05MPa are carried out in 250 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is nitric acid solution.
Embodiment 2
A kind of preparation method of reliable and stable chip tantalum capacitor, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 15 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 600min；
(4) nitrogen is handled: annealing 20-300min, nitrogen pressure 1.5MPa are carried out in 450 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is sulfuric acid solution.
Embodiment 3
A kind of preparation method of reliable and stable chip tantalum capacitor, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 8 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 80min；
(4) nitrogen is handled: annealing 40min, nitrogen pressure 0.1MPa are carried out in 300 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is phosphoric acid solution.
Embodiment 4
A kind of preparation method of reliable and stable chip tantalum capacitor, comprising the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 13 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 360min；
(4) nitrogen is handled: annealing 240min, nitrogen pressure 1.2MPa are carried out in 400 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is nitric acid solution.
Embodiment 5
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 10 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 180min；
(4) nitrogen is handled: annealing 120min, nitrogen pressure 0.2MPa are carried out in 350 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is phosphoric acid solution.
Embodiment 6
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes Anode preparation；
(2) it is melted into: forming unformed dielectric in 12 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 120min；
(4) nitrogen is handled: annealing 180min, nitrogen pressure 1.0MPa are carried out in 350 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry (PEDOT:PSS), being formed and is uniformly caused Close polymer film；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
The electrolyte is sulfuric acid solution.
It is important to point out that, above embodiments and test example are only limitted to do further technical solution of the present invention herein Elaboration and understanding, should not be understood as it is further to technical solution of the present invention limited, what those skilled in the art made The innovation and creation of non-protruding essential characteristics and marked improvement still fall within protection category of the invention.

Claims (8)

1. a kind of preparation method of reliable and stable chip tantalum capacitor, which comprises the following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes anode Preparation；
(2) it is melted into: forming unformed dielectric in 5~15 DEG C of electrolyte；
(3) it shields: boiling and wash in high temperature steam environments；
(4) nitrogen is handled: being made annealing treatment in 250-450 DEG C of nitrogen environment；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5The precoated shet of dielectric surface formation silane coupling agent；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry, forming the polymer film of even compact；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
2. the preparation method of reliable and stable chip tantalum capacitor as described in claim 1, which is characterized in that the electrolyte is nitre It is acid solution, sulfuric acid solution, any in phosphoric acid solution.
3. the preparation method of reliable and stable chip tantalum capacitor as described in claim 1, which is characterized in that the high temperature is 95 DEG C More than.
4. the preparation method of reliable and stable chip tantalum capacitor as described in claim 1, which is characterized in that described boil washes the time and be 20~600min.
5. the preparation method of reliable and stable chip tantalum capacitor as claimed in claim 4, which is characterized in that described boil washes the time and be 80~360min.
6. the preparation method of reliable and stable chip tantalum capacitor as described in claim 1, which is characterized in that nitrogen in the nitrogen processing The pressure of gas is 0.05~1.5MPa, and the processing time is 20~300min.
7. the preparation method of reliable and stable chip tantalum capacitor as claimed in claim 6, which is characterized in that nitrogen in the nitrogen processing The pressure of gas is 0.1~1.2MPa, and the processing time is 40~240min.
8. the preparation method of reliable and stable chip tantalum capacitor as described in any one of claim 1~7, which is characterized in that including Following steps:
(1) prepared by anode: preparing special process according to high-voltage large-capacity organic solid electrolyte chip tantalum capacitor and completes anode Preparation；
(2) it is melted into: forming unformed dielectric in 5~15 DEG C of electrolyte；
(3) it shields: being boiled in 95 DEG C or more high temperature steam environments and wash 20~600min；
(4) nitrogen is handled: annealing 20-300min, nitrogen pressure 0.05- are carried out in 250-450 DEG C of nitrogen environment 1.5MPa；
(5) it is melted into afterwards: completing dielectric benefit formation and drying according to common processes；
(6) adhesive layer is formed: in Ta2O5Dielectric surface forms silane coupler solution and forms surface precoated shet；
(7) polymer electrolytic layer is formed: in precoated shet surface conducting polymer graphic slurry, forming the polymer film of even compact；
(8) it post-processes: polymer film being made annealing treatment in high temperature air environment；
(9) cooling package: it is coated carbon slurry and silver paste after cooling, and encapsulates.
CN201810676313.7A 2018-06-27 2018-06-27 A kind of preparation method of reliable and stable chip tantalum capacitor Pending CN108962605A (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114121492A (en) * 2021-08-09 2022-03-01 湖南艾华集团股份有限公司 Preparation method of solid-state aluminum electrolytic capacitor based on PEDOT (PolyEthylenediamine) PSS (PolyEthylenediamine)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1184653C (en) * 1999-12-03 2005-01-12 松下电器产业株式会社 Method for mfg. solid electrolytic capacitor, and said solid electrolytic capacitor
JP2009032895A (en) * 2007-07-27 2009-02-12 Japan Carlit Co Ltd:The Solid-state electrolytic capacitor, and manufacturing method thereof
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
CN104538180A (en) * 2014-12-24 2015-04-22 中国振华（集团）新云电子元器件有限责任公司 Method for manufacturing solid organic electrolytic capacitor
CN105489376A (en) * 2016-01-14 2016-04-13 中国振华（集团）新云电子元器件有限责任公司 Method for manufacturing high-reliability electrolytic capacitor
CN106206029A (en) * 2016-08-14 2016-12-07 中国振华（集团）新云电子元器件有限责任公司 A kind of low temperature forming method of chip tantalum capacitor anode

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1184653C (en) * 1999-12-03 2005-01-12 松下电器产业株式会社 Method for mfg. solid electrolytic capacitor, and said solid electrolytic capacitor
JP2009032895A (en) * 2007-07-27 2009-02-12 Japan Carlit Co Ltd:The Solid-state electrolytic capacitor, and manufacturing method thereof
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
CN104538180A (en) * 2014-12-24 2015-04-22 中国振华（集团）新云电子元器件有限责任公司 Method for manufacturing solid organic electrolytic capacitor
CN105489376A (en) * 2016-01-14 2016-04-13 中国振华（集团）新云电子元器件有限责任公司 Method for manufacturing high-reliability electrolytic capacitor
CN106206029A (en) * 2016-08-14 2016-12-07 中国振华（集团）新云电子元器件有限责任公司 A kind of low temperature forming method of chip tantalum capacitor anode

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114121492A (en) * 2021-08-09 2022-03-01 湖南艾华集团股份有限公司 Preparation method of solid-state aluminum electrolytic capacitor based on PEDOT (PolyEthylenediamine) PSS (PolyEthylenediamine)
CN114121492B (en) * 2021-08-09 2023-09-01 湖南艾华集团股份有限公司 Preparation method of solid aluminum electrolytic capacitor based on PEDOT (polymer electrolyte manufacturing) PSS (power system stabilizer)

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