CN100514518C - Electrolytic capacitor dielectric oxide film manufacturing method - Google Patents

Electrolytic capacitor dielectric oxide film manufacturing method Download PDF

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Publication number
CN100514518C
CN100514518C CNB200510003286XA CN200510003286A CN100514518C CN 100514518 C CN100514518 C CN 100514518C CN B200510003286X A CNB200510003286X A CN B200510003286XA CN 200510003286 A CN200510003286 A CN 200510003286A CN 100514518 C CN100514518 C CN 100514518C
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China
Prior art keywords
current
electrolytic capacitor
oxide film
pulse current
dielectric oxide
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CN1767102A (en
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张选红
黄波
毛云武
李仁海
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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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Abstract

The invention discloses a method for preparing electrolytic capacitor media oxide film in the field of electric chemistry technology. It uses the multi-holes sintered body of valve mental as base material and uses the base material as anode to do anodic oxidize to the exert current in the forming liquid; the current is an interrupt exert impulse current; the valve mental is one of tantalum, titanium, niobium and aluminum.

Description

Electrolytic capacitor dielectric oxide film manufacturing method
Technical field: the present invention relates to a kind of method that forms oxide-film in the metal surface, relate in particular to a kind of method that forms dielectric oxide film on the surface of electrolytic capacitor anode piece.
Background technology: at present, the manufacture method of electrolytic capacitor anodized film generally is to be to pass to constant electric current in the electrolytical aqueous solution continuously to carry out anodic oxidation with phosphoric acid.Granted publication number be that " on February 16th, 2005 ", invention and created name are the manufacture method that the Chinese patent literature of " the formation method and the titanium electrolytic capacitor of titanium oxide film " discloses a kind of electrolytic capacitor anodized film for " CN1189401C ", Granted publication day, its shortcoming is: because formed oxide-film density is little, make electrolytic capacitor breakdown voltage resistant low, rated value is little, and leakage current and series impedance are big, thereby cause the capacitor percent defective to rise.
Summary of the invention: at the above-mentioned defective that exists in the prior art, the present invention aims to provide a kind of electrolytic capacitor dielectric oxide film manufacturing method that can improve dielectric oxide film density and quality.
Technical scheme of the present invention is: the porous sintered body with valve metal is a base material, and to be anode apply electric current to it in forming liquid carry out anodic oxidation with this base material; Described electric current is to be to be interrupted the pulse current that applies in 10: 1~25: 1 by switching electricity time scale, the switching electricity time scale of the impulse wave of described pulse current in one-period is 5: 1~1: 1, and the current density of pulse current is 10mA/g~200mA/g; Described valve metal is one of tantalum, titanium, niobium or aluminium.
The current density of pulse current is 15mA/g~80mA/g, and described valve metal is a tantalum.
Wherein, the time scale of switching electricity, the switching electricity time scale of the impulse wave of pulse current, and the current density fibrous root of pulse current is determined according to kind, the weight of base material and the specification of product of the valve metal that forms base material.
Compared with the prior art, the present invention is owing to changed the constant current that applies continuously in the conventional art into pulse current that interruption applies, distribute release with gas thereby help heat in the anode oxidation process, guarantee oxide-film even compact more, more stable quality.
Embodiment: following is that the tantalum electrolytic capacitor of 16V/10 μ F is that specific embodiment is done step explanation to the present invention with the product specification:
Embodiment 1: with specific volume is the tantalum powder method routinely of the 3.2 ten thousand μ FV/g porous sintered body that to make 5000 weight be 0.015g, with 5000 these sintered bodies is base material, and with it and be connected in the positive pole of power supply, in 70 ℃ formation liquid, pass to current strength and be (the pulse current of 0.015g * 5000 * 200mA/g) ÷ 1000=15A, 30 minutes conduction time, cut off the power supply then 3 minutes, repeated multiple times like this is until the required thickness requirement of tantalum electrolytic capacitor anode dielectric oxide film that reaches 16V/10 μ F; Wherein, the switching electricity time scale of the impulse wave of described pulse current in one-period is 5: 1.
Concrete reaction equation is as follows:
Ta-5e=Ta +5
H 2O=H ++OH -
2H ++2e=H 2
Ta +5+5OH -=Ta(OH) 5
2Ta(OH) 5=Ta 2O 5+5H 2O
Embodiment 2: method is with embodiment 1; Wherein, 50 minutes conduction time, cut off the power supply 2 minutes; The switching electricity time scale of the impulse wave of described pulse current in one-period is 1: 1, and the current strength of pulse current is (0.015g * 5000 * 10mA/g) ÷ 1000=0.75A.
Embodiment 3: method is with embodiment 1; Wherein, 30 minutes conduction time, cut off the power supply 2 minutes; The switching electricity time scale of the impulse wave of described pulse current in one-period is 3: 1, and the current strength of pulse current is (0.015g * 5000 * 15mA/g) ÷ 1000=1.125A.
Embodiment 4: method is with embodiment 1: wherein, 40 minutes conduction time, cut off the power supply 2 minutes; The switching electricity time scale of the impulse wave of described pulse current in one-period is 2: 1, and the current strength of pulse current is (0.015g * 5000 * 80mA/g) ÷ 1000=6A.
In like manner, adopt the anode dielectric oxide film that uses the same method and also can make titanium, niobium or aluminium electrolytic capacitor.
Facts have proved that after the anode block that technical solution of the present invention is produced was made tantalum electrolytic capacitor, the multinomial technical indicator of capacitor all had raising in various degree.Concrete detection, comparing result see the following form:
Product specification: 16V/10 μ F unit (propping up)
Amount detection Puncture quantity (I) The capacity quantity (C) that exceeds standard Loss quantity (tg δ) Leakage current quantity (i) The series resistance quantity (ESR) that exceeds standard Qualified quantity Qualification rate (%)
New product batch
1 batch 4224 31 16 34 28 15 4100 97.06
2 batches 5472 60 41 66 22 39 5244 95.83
Old product batch
1 batch 11904 210 158 142 155 1749 9490 79.72
2 batches 4944 40 55 85 20 59 4685 94.76
3 batches 16224 187 149 298 68 154 15368 94.72
4 batches 15840 154 149 305 101 168 14963 94.46
5 batches 14592 202 101 1 114 886 13288 91.06
Add up to 63504 793 612 831 458 3016 57794
Percent defective (%) 1.24 0.96 1.30 0.72 4.74 91.00

Claims (2)

1. electrolytic capacitor dielectric oxide film manufacturing method is a base material with the porous sintered body of valve metal, and is that anode applies electric current to it and carries out anodic oxidation in forming liquid with this base material; It is characterized in that: described electric current is to be to be interrupted the pulse current that applies in 10: 1~25: 1 by switching electricity time scale, the switching electricity time scale of the impulse wave of described pulse current in one-period is 5: 1~1: 1, and the current density of pulse current is 10mA/g~200mA/g; Described valve metal is one of tantalum, titanium, niobium or aluminium.
2. electrolytic capacitor dielectric oxide film manufacturing method according to claim 1 is characterized in that: the current density of pulse current is 15mA/g~80mA/g, and described valve metal is a tantalum.
CNB200510003286XA 2005-11-16 2005-11-16 Electrolytic capacitor dielectric oxide film manufacturing method Active CN100514518C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB200510003286XA CN100514518C (en) 2005-11-16 2005-11-16 Electrolytic capacitor dielectric oxide film manufacturing method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB200510003286XA CN100514518C (en) 2005-11-16 2005-11-16 Electrolytic capacitor dielectric oxide film manufacturing method

Publications (2)

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CN1767102A CN1767102A (en) 2006-05-03
CN100514518C true CN100514518C (en) 2009-07-15

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781788B (en) * 2010-04-22 2015-05-13 兰州大学 Method for preparing specially-shaped titanium dioxide nano-tube films
CN102808209B (en) * 2011-06-03 2015-06-10 上海造币有限公司 Method for oxidizing and coloring surfaces of niobium and niobium alloy
CN103572350B (en) * 2012-08-07 2016-05-18 中国振华(集团)新云电子元器件有限责任公司 A kind of oxide-film of consistency of thickness forms technology
CN103354178A (en) * 2013-07-31 2013-10-16 株洲宏达电子有限公司 Method for manufacturing high-voltage solid tantalum capacitor dielectric oxide film
CN108091491A (en) * 2017-12-12 2018-05-29 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) The method for reducing the method for non-solid electrolyte tantalum capacity fall off flow valuve and preparing non-solid electrolyte tantalum capacitance

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Application publication date: 20060503

Assignee: Sinowatt Dongguan Limited

Assignor: China Zhenhua (Group) Xinyun Electronic Component Co., Ltd.

Contract record no.: 2012520000012

Denomination of invention: Electrolytic capacitor dielectric oxide film manufacturing method

Granted publication date: 20090715

License type: Exclusive License

Record date: 20120802

EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20060503

Assignee: Sinowatt Dongguan Limited

Assignor: China Zhenhua (Group) Xinyun Electronic Component Co., Ltd.

Contract record no.: 2012520000012

Denomination of invention: Electrolytic capacitor dielectric oxide film manufacturing method

Granted publication date: 20090715

License type: Exclusive License

Record date: 20120802

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