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JP2007035997A - Manufacturing method of solid electrolytic capacitor - Google Patents

Manufacturing method of solid electrolytic capacitor Download PDF

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JP2007035997A
JP2007035997A JP2005218456A JP2005218456A JP2007035997A JP 2007035997 A JP2007035997 A JP 2007035997A JP 2005218456 A JP2005218456 A JP 2005218456A JP 2005218456 A JP2005218456 A JP 2005218456A JP 2007035997 A JP2007035997 A JP 2007035997A
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electrolytic capacitor
solid electrolytic
forming
injection hole
solid
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Katsumi Nakajima
克己 中島
Megumi Nabuchi
恵 名渕
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Nichicon Corp
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Nichicon Corp
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a solid electrolytic capacitor wherein its leakage current is improved, and its leakage current characteristic relative to its high-temperature loading test is improved. <P>SOLUTION: The manufacturing method of the solid electrolytic capacitor has a process for so molding pressingly a valve-action metal powder as to sinter it, a process for forming an oxidation film on the sintered body, a process for so laminating successively a solid electrolyte layer and a cathode deriving layer on the oxidation film as to obtain a capacitor element, and a process for forming an armored resin on the capacitor element. In this manufacturing method, when forming the armored resin, an injecting hole is formed as ranging from the armored surface to the capacitor element and an acidic solution is so injected into the injecting hole as to be subjected to an aging processing, and as to seal thereafter the injecting hole. Hereupon, the conductivity of the acidic solution is 10 μS/cm to 10 mS/cm, and the voltage of the aging processing is 0.3 to 4.0 times as high as the rated voltage of the solid electrolytic capacitor. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、固体電解コンデンサの製造方法に関し、特にエージング処理方法に関するものである。   The present invention relates to a method for manufacturing a solid electrolytic capacitor, and more particularly to an aging treatment method.

従来、固体電解コンデンサは、陽極リードを植立した弁作用金属粉末からなる成形体を焼結した後、酸化皮膜、固体電解質層、カーボン層と銀層からなる陰極引出層を順次形成してコンデンサ素子とし、上記陽極リードと陽極リードフレームとを接続し、陰極引出層と陰極リードフレームとを導電性接着剤を介して接続した後、外装樹脂で被覆している。しかし、外装樹脂が硬化する際、樹脂が収縮してコンデンサ素子に機械的ストレスがかかり、酸化皮膜を損傷し、固体電解コンデンサの漏れ電流の上昇を招いていた。そのため、コンデンサ素子に外装樹脂を形成した後、高温中で電圧を印加してエージング処理を行っていた。(例えば特許文献1参照)
特開2000−340466号
Conventionally, a solid electrolytic capacitor is formed by sintering a molded body made of a valve metal powder having an anode lead planted, and then sequentially forming an oxide film, a solid electrolyte layer, a cathode lead layer made up of a carbon layer and a silver layer. As an element, the anode lead and the anode lead frame are connected, and the cathode lead layer and the cathode lead frame are connected via a conductive adhesive, and then covered with an exterior resin. However, when the exterior resin is cured, the resin contracts and mechanical stress is applied to the capacitor element, damaging the oxide film and increasing the leakage current of the solid electrolytic capacitor. For this reason, after forming an exterior resin on the capacitor element, an aging treatment is performed by applying a voltage at a high temperature. (For example, see Patent Document 1)
JP 2000-340466 A

しかし、従来のエージング方法は、外装樹脂形成後、電圧印加し、酸化皮膜を修復し、漏れ電流特性の改善を図るものであるが、酸化皮膜の修復が不十分であると漏れ電流が上昇する問題があった。   However, the conventional aging method is to apply voltage after forming the exterior resin and repair the oxide film to improve the leakage current characteristics. However, if the oxide film is not sufficiently repaired, the leakage current increases. There was a problem.

本発明は、上記の課題を解決するもので、エージング後の漏れ電流特性を改善し、かつ、信頼性の高い固体電解コンデンサの製造方法を提供するものである。   The present invention solves the above-described problems, and provides a method for manufacturing a solid electrolytic capacitor with improved leakage current characteristics after aging and high reliability.

本発明は、弁作用金属粉末を加圧成形し、焼結した焼結体に酸化皮膜を形成し、該酸化皮膜に固体電解質層、陰極引出層を順次形成したコンデンサ素子に、外装樹脂を形成してなる固体電解コンデンサの製造方法において、
外装樹脂形成時に外装表面からコンデンサ素子に至る注入孔を形成し、該注入孔に酸性溶液を注入して、エージング処理を行った後、注入孔を封止することを特徴とする固体電解コンデンサの製造方法である。
In the present invention, a valve action metal powder is pressure-formed, an oxide film is formed on a sintered sintered body, and an exterior resin is formed on a capacitor element in which a solid electrolyte layer and a cathode lead layer are sequentially formed on the oxide film. In the manufacturing method of the solid electrolytic capacitor formed,
A solid electrolytic capacitor characterized by forming an injection hole from the exterior surface to the capacitor element when forming the exterior resin, injecting an acidic solution into the injection hole, performing an aging treatment, and then sealing the injection hole It is a manufacturing method.

また、上記の酸性溶液の電導度が10μS/cm〜10mS/cmであることを特徴とする固体電解コンデンサの製造方法である。   Further, the present invention is a method for producing a solid electrolytic capacitor, wherein the electric conductivity of the acidic solution is 10 μS / cm to 10 mS / cm.

さらに、上記のエージング処理の電圧が、定格電圧に対し、0.3〜4.0倍であることを特徴とする固体電解コンデンサの製造方法である。   Furthermore, the voltage for the above aging treatment is 0.3 to 4.0 times the rated voltage.

また、上記の酸性溶液としては、酢酸、硝酸、プロピオン酸、シュウ酸、アジピン酸、マレイン酸、フマル酸、フタル酸、オキシカルボン酸を挙げることができる。   Examples of the acidic solution include acetic acid, nitric acid, propionic acid, oxalic acid, adipic acid, maleic acid, fumaric acid, phthalic acid, and oxycarboxylic acid.

弁作用金属粉末を加圧成形し、焼結して作製した焼結体に酸化皮膜、固体電解質層、カーボン層および陰極銀層からなる陰極引出層を順次形成したコンデンサ素子とし、外装樹脂形成時、外装表面からコンデンサ素子に至る注入孔を形成し、該注入孔より酸性溶液を注入した後、エージング処理を行うことで、漏れ電流特性が改善し、かつ信頼性が向上した固体電解コンデンサを得ることができる。   A capacitor element in which a cathode lead layer comprising an oxide film, a solid electrolyte layer, a carbon layer, and a cathode silver layer is sequentially formed on a sintered body produced by pressure-molding and sintering a valve action metal powder, and when forming an exterior resin Then, an injection hole extending from the outer surface to the capacitor element is formed, an acidic solution is injected from the injection hole, and then an aging treatment is performed to obtain a solid electrolytic capacitor with improved leakage current characteristics and improved reliability be able to.

[実施例1]
以下、本発明の実施例について図面を参照しながら説明する。
図1に本発明の実施例における固体電解コンデンサの断面図および部分拡大図を示す。まず、タンタルの弁作用金属粉末を所定の寸法に加圧成形した後、焼結し、焼結体を作製する。続いて、該焼結体をリン酸などの酸性溶液に浸漬し、溶液中で電圧を印加して陽極酸化を行い、焼結体表面に酸化皮膜4を形成する。その後、酸化皮膜表面に固体電解質層5、カーボン層6、陰極銀層7を順次形成する。続いて、陰極リードフレーム10と陰極銀層7を導電性接着剤8を介して接続するとともに、抵抗溶接により陽極リードフレーム9と陽極リード線2を接続する。その後、酸性溶液を注入する注入孔12を外装底面に形成するため、凸部を設けたモールド金型を用いてトランスファーモールドによりエポキシ樹脂からなる外装11を形成する。外装樹脂を形成後、注入孔より電導度が10μS/cmの酢酸溶液を注入する。その後、定格電圧の1.2倍の電圧を印加し、エージング処理した後、水洗、乾燥し、酢酸溶液を除去する。続いて、エポキシ樹脂にて注入孔を封止し、固体電解コンデンサを作製した。
[Example 1]
Embodiments of the present invention will be described below with reference to the drawings.
FIG. 1 shows a cross-sectional view and a partially enlarged view of a solid electrolytic capacitor in an embodiment of the present invention. First, a tantalum valve action metal powder is pressure-molded to a predetermined size and then sintered to produce a sintered body. Subsequently, the sintered body is immersed in an acidic solution such as phosphoric acid, and a voltage is applied in the solution to perform anodization to form an oxide film 4 on the surface of the sintered body. Thereafter, the solid electrolyte layer 5, the carbon layer 6, and the cathode silver layer 7 are sequentially formed on the oxide film surface. Subsequently, the cathode lead frame 10 and the cathode silver layer 7 are connected via the conductive adhesive 8, and the anode lead frame 9 and the anode lead wire 2 are connected by resistance welding. Thereafter, in order to form the injection hole 12 for injecting the acidic solution on the bottom surface of the exterior, the exterior 11 made of an epoxy resin is formed by transfer molding using a mold having a convex portion. After forming the exterior resin, an acetic acid solution having a conductivity of 10 μS / cm is injected from the injection hole. Thereafter, a voltage 1.2 times the rated voltage is applied and subjected to an aging treatment, followed by washing with water and drying to remove the acetic acid solution. Subsequently, the injection hole was sealed with an epoxy resin to produce a solid electrolytic capacitor.

[実施例2]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Example 2]
A solid electrolytic capacitor was produced in the same manner as in Example 1 except that after the exterior resin was formed, an acetic acid solution having a conductivity of 1 mS / cm was injected from the injection hole.

[実施例3]
外装樹脂を形成後、注入孔より電導度が10mS/cmの酢酸溶液を注入した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Example 3]
A solid electrolytic capacitor was produced in the same manner as in Example 1 except that after forming the exterior resin, an acetic acid solution having a conductivity of 10 mS / cm was injected from the injection hole.

[実施例4]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入後、定格電圧の0.3倍の電圧を印加し、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Example 4]
After forming the exterior resin, after injecting an acetic acid solution having a conductivity of 1 mS / cm from the injection hole, applying a voltage 0.3 times the rated voltage and performing an aging treatment, a solid was obtained in the same manner as in Example 1. An electrolytic capacitor was produced.

[実施例5]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入後、定格電圧の2.0倍の電圧を印加し、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Example 5]
After forming the exterior resin, after injecting an acetic acid solution having a conductivity of 1 mS / cm from the injection hole, applying a voltage 2.0 times the rated voltage and performing an aging treatment, a solid was obtained in the same manner as in Example 1. An electrolytic capacitor was produced.

[実施例6]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入後、定格電圧の4.0倍の電圧を印加し、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Example 6]
After forming the exterior resin, after injecting an acetic acid solution having a conductivity of 1 mS / cm from the injection hole, applying a voltage 4.0 times the rated voltage and performing an aging treatment, a solid was obtained in the same manner as in Example 1. An electrolytic capacitor was produced.

[比較例1]
外装樹脂を形成後、注入孔より電導度が5μS/cmの酢酸溶液を注入した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Comparative Example 1]
A solid electrolytic capacitor was produced in the same manner as in Example 1 except that after the exterior resin was formed, an acetic acid solution having an electric conductivity of 5 μS / cm was injected from the injection hole.

[比較例2]
外装樹脂を形成後、注入孔より電導度が20mS/cmの酢酸溶液を注入した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Comparative Example 2]
A solid electrolytic capacitor was produced in the same manner as in Example 1 except that after forming the exterior resin, an acetic acid solution having an electric conductivity of 20 mS / cm was injected from the injection hole.

[比較例3]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入後、定格電圧の0.2倍の電圧を印加し、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Comparative Example 3]
After forming the exterior resin, after injecting an acetic acid solution having a conductivity of 1 mS / cm from the injection hole, applying a voltage 0.2 times the rated voltage and performing an aging treatment, a solid was obtained in the same manner as in Example 1. An electrolytic capacitor was produced.

[比較例4]
外装樹脂を形成後、注入孔より電導度が1mS/cmの酢酸溶液を注入後、定格電圧の5.0倍の電圧を印加し、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
[Comparative Example 4]
After forming the exterior resin, after injecting an acetic acid solution having a conductivity of 1 mS / cm from the injection hole, applying a voltage 5.0 times the rated voltage and aging treatment, a solid was obtained in the same manner as in Example 1. An electrolytic capacitor was produced.

(従来例)
外装樹脂を形成後、酢酸溶液を注入せず、エージング処理した以外は、実施例1と同様の方法で固体電解コンデンサを作製した。
(Conventional example)
A solid electrolytic capacitor was produced in the same manner as in Example 1 except that after the exterior resin was formed, an acetic acid solution was not injected and an aging treatment was performed.

上記の実施例1〜6、比較例1〜4、従来例の固体電解コンデンサについて、それぞれ漏れ電流値(10V印加、1分値)を表1に示し、高温負荷試験(85℃、10V印加)における漏れ電流値の推移を図3に示す。   Regarding the solid electrolytic capacitors of Examples 1 to 6, Comparative Examples 1 to 4, and the conventional example, the leakage current values (10 V application, 1 minute value) are shown in Table 1, respectively, and the high temperature load test (85 ° C., 10 V application) FIG. 3 shows the transition of the leakage current value.

Figure 2007035997
Figure 2007035997

表1より明らかなように、実施例1〜6は比較例1〜4、従来例と比較し、漏れ電流が低い。これは、外装樹脂形成後に、酸性溶液中でエージングを行うことで、酸化皮膜が修復されたためである。ここで、酢酸溶液の電導度が5μS/cm以下(比較例1)および20mS/cm以上(比較例2)では、漏れ電流が高くなるため、電導度は10μS/cm〜10mS/cmが望ましい。
また、定格電圧に対するエージング電圧の倍率が、0.2倍以下(比較例3)および5.0倍以上(比較例4)では、漏れ電流が高くなるため、倍率は0.3〜4.0倍が望ましい。
As is clear from Table 1, Examples 1 to 6 have lower leakage currents than Comparative Examples 1 to 4 and the conventional example. This is because the oxide film was repaired by aging in an acidic solution after forming the exterior resin. Here, when the electric conductivity of the acetic acid solution is 5 μS / cm or less (Comparative Example 1) and 20 mS / cm or more (Comparative Example 2), the leakage current becomes high. Therefore, the electric conductivity is desirably 10 μS / cm to 10 mS / cm.
Further, when the magnification of the aging voltage with respect to the rated voltage is 0.2 times or less (Comparative Example 3) and 5.0 times or more (Comparative Example 4), the leakage current becomes high, so the magnification is 0.3 to 4.0. Double is desirable.

さらに、本発明の実施例の酸性溶液は、酢酸を使用したが、硝酸、プロピオン酸、シュウ酸、アジピン酸、マレイン酸、フマル酸、フタル酸、オキシカルボン酸を使用しても同様の効果を得ることができる。   Furthermore, although the acetic acid was used for the acidic solution of the Example of this invention, even if it uses nitric acid, propionic acid, oxalic acid, adipic acid, maleic acid, fumaric acid, phthalic acid, and oxycarboxylic acid, the same effect is obtained. Obtainable.

また、本発明の実施例の弁作用金属粉末は、タンタルを使用したが、ニオブを用いても同様の効果を得ることができる。   Moreover, although the tantalum is used for the valve action metal powder of the Example of this invention, the same effect can be acquired even if it uses niobium.

実施例における固体電解コンデンサの断面図および部分拡大図である。It is sectional drawing and the elements on larger scale of the solid electrolytic capacitor in an Example. 従来例における固体電解コンデンサの断面図および部分拡大図である。It is sectional drawing and the partial enlarged view of the solid electrolytic capacitor in a prior art example. 実施例1と従来例の高温負荷試験結果である。It is a high temperature load test result of Example 1 and a prior art example.

符号の説明Explanation of symbols

1 コンデンサ素子
2 陽極リード
3 細孔
4 酸化皮膜
5 固体電解質層
6 カーボン層
7 陰極銀層
8 導電性接着剤
9 陽極リードフレーム
10 陰極リードフレーム
11 外装樹脂
12 注入孔
DESCRIPTION OF SYMBOLS 1 Capacitor element 2 Anode lead 3 Pore 4 Oxide film 5 Solid electrolyte layer 6 Carbon layer 7 Cathode silver layer 8 Conductive adhesive 9 Anode lead frame 10 Cathode lead frame 11 Exterior resin 12 Injection hole

Claims (3)

弁作用金属粉末を加圧成形し、焼結した焼結体に酸化皮膜を形成し、該酸化皮膜に固体電解質層、陰極引出層を順次積層したコンデンサ素子に、外装樹脂を形成してなる固体電解コンデンサの製造方法において、
外装樹脂形成時に外装表面からコンデンサ素子に至る注入孔を形成し、該注入孔に酸性溶液を注入して、エージング処理を行った後、注入孔を封止することを特徴とする固体電解コンデンサの製造方法。
A solid formed by forming an exterior resin on a capacitor element in which a valve action metal powder is pressure-formed, an oxide film is formed on a sintered sintered body, and a solid electrolyte layer and a cathode lead layer are sequentially laminated on the oxide film. In the method of manufacturing an electrolytic capacitor,
A solid electrolytic capacitor characterized by forming an injection hole from the exterior surface to the capacitor element when forming the exterior resin, injecting an acidic solution into the injection hole, performing an aging treatment, and then sealing the injection hole Production method.
請求項1記載の酸性溶液の電導度が10μS/cm〜10mS/cmであることを特徴とする固体電解コンデンサの製造方法。   The method for producing a solid electrolytic capacitor, wherein the electrical conductivity of the acidic solution according to claim 1 is 10 μS / cm to 10 mS / cm. 請求項1記載のエージング処理の電圧が、定格電圧に対し、0.3〜4.0倍であることを特徴とする固体電解コンデンサの製造方法。
The method for producing a solid electrolytic capacitor, wherein the voltage of the aging treatment according to claim 1 is 0.3 to 4.0 times the rated voltage.
JP2005218456A 2005-07-28 2005-07-28 Manufacturing method of solid electrolytic capacitor Pending JP2007035997A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104882279A (en) * 2015-05-28 2015-09-02 南通华裕电子有限公司 High specific volume aluminium electrolytic capacitor aging method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5315562A (en) * 1976-07-28 1978-02-13 Matsushita Electric Industrial Co Ltd Method of aging solid state electrolytic capacitor
JPH09246115A (en) * 1996-03-13 1997-09-19 Nitsuko Corp Manufacture of solid capacitor
JPH1187187A (en) * 1997-09-01 1999-03-30 Nec Toyama Ltd Manufacture of solid electroytic capacitor
JP2005079334A (en) * 2003-08-29 2005-03-24 Nippon Chemicon Corp Method for manufacturing solid electrolytic capacitor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5315562A (en) * 1976-07-28 1978-02-13 Matsushita Electric Industrial Co Ltd Method of aging solid state electrolytic capacitor
JPH09246115A (en) * 1996-03-13 1997-09-19 Nitsuko Corp Manufacture of solid capacitor
JPH1187187A (en) * 1997-09-01 1999-03-30 Nec Toyama Ltd Manufacture of solid electroytic capacitor
JP2005079334A (en) * 2003-08-29 2005-03-24 Nippon Chemicon Corp Method for manufacturing solid electrolytic capacitor

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104882279A (en) * 2015-05-28 2015-09-02 南通华裕电子有限公司 High specific volume aluminium electrolytic capacitor aging method

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