JPH02256224A - Manufacture of electrolytic capacitor - Google Patents
Manufacture of electrolytic capacitorInfo
- Publication number
- JPH02256224A JPH02256224A JP7894589A JP7894589A JPH02256224A JP H02256224 A JPH02256224 A JP H02256224A JP 7894589 A JP7894589 A JP 7894589A JP 7894589 A JP7894589 A JP 7894589A JP H02256224 A JPH02256224 A JP H02256224A
- Authority
- JP
- Japan
- Prior art keywords
- electrolytic capacitor
- concentration
- phosphorus
- oxide film
- contained
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000003990 capacitor Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 20
- 239000011574 phosphorus Substances 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract description 14
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000007787 solid Substances 0.000 abstract description 5
- 229910052715 tantalum Inorganic materials 0.000 abstract description 5
- 230000006866 deterioration Effects 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 230000006355 external stress Effects 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 229910000679 solder Inorganic materials 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- PDBGNMOCNKXQDD-UHFFFAOYSA-N [Ni].[Pb].[Ag] Chemical compound [Ni].[Pb].[Ag] PDBGNMOCNKXQDD-UHFFFAOYSA-N 0.000 description 1
- ROSDCCJGGBNDNL-UHFFFAOYSA-N [Ta].[Pb] Chemical compound [Ta].[Pb] ROSDCCJGGBNDNL-UHFFFAOYSA-N 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001721 transfer moulding Methods 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、タンタルの弁作用金属粉末成形体を使用した
電解コンデンサの製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for manufacturing an electrolytic capacitor using a tantalum valve metal powder compact.
［従来の技術］
一般に、電解コンデンサは、弁作用金属粉末の成形体を
真空焼結した焼結体の表面上に、酸化皮膜の誘電体層を
設け、この誘電体層に密着するように、順次、二酸化マ
ンガン層、グラファイト層、銀ペースト層などを被着し
て陰極とするコンデンサである。[Prior Art] In general, electrolytic capacitors include a dielectric layer of an oxide film provided on the surface of a sintered body obtained by vacuum sintering a molded body of valve metal powder, and a dielectric layer of an oxide film so as to be in close contact with the dielectric layer. It is a capacitor in which a manganese dioxide layer, a graphite layer, a silver paste layer, etc. are sequentially deposited to form a cathode.
この様な電解コンデンサの構成を以下に詳述する。即ち
、平均粒子径が数μｍの弁作用金属粉に、陽極のリード
線を構成する弁作用金属粉末と同種の金属線を植立しな
がら、同粉末を所定の形状、寸法に加圧、成形した後、
ＩＸｌｏ−４ｍｍＨｇ以下の真空度で、１６００〜１８
００°Ｃで、１５〜３０分間焼結して焼結体を形成する
。The structure of such an electrolytic capacitor will be described in detail below. In other words, a metal wire of the same type as the valve metal powder constituting the lead wire of the anode is planted on a valve metal powder with an average particle diameter of several μm, and the powder is pressed and molded into a predetermined shape and size. After that,
IXlo-1600-18 at vacuum level below 4mmHg
Sinter at 00°C for 15-30 minutes to form a sintered body.
次に、焼結体表面に誘電体層となる酸化皮膜を、リン酸
水溶液などの電解質中で、陽極化成によって形成する。Next, an oxide film that will become a dielectric layer is formed on the surface of the sintered body by anodization in an electrolyte such as an aqueous phosphoric acid solution.
次いで、二酸化マンガン層を、素子に含浸させた硝酸マ
ンガン液を熱分解すると同時に、前記陽極化成素子の表
面上に焼付は形成する。Next, a manganese dioxide layer is formed on the surface of the anodized element at the same time as the manganese nitrate solution with which the element is impregnated is thermally decomposed.
その後、順次、グラファイト層、銀ペースト層を形成し
、陰極リード線となる適当な金属を半田もしくは導電性
接着剤などを用いて接続し、樹脂などで補強してコンデ
ンサを完成する。After that, a graphite layer and a silver paste layer are sequentially formed, and a suitable metal that will become the cathode lead wire is connected using solder or conductive adhesive, and reinforced with resin or the like to complete the capacitor.
［発明が解決しようとする課題］
しかしながら、上述した様な従来の電解コンテンサにお
いては、以下に述べる様な問題点があった。[Problems to be Solved by the Invention] However, the conventional electrolytic capacitor as described above has the following problems.
即ち、上述した様な電解コンデンサは、破壊電圧が高く
、漏れ電流が小さいことが望まれ、この目的を達成する
ために、特に弁作用金属以外の元素（不純物と称し、金
属、非金属、酸素、水素を総称する）の含有量を少なく
することが重要である。なぜならば、弁作用金属以外の
元素は、陽極酸化されにくいため、これらの不純物によ
って酸化皮膜が形成されにくくなり、漏れ電流が増大す
るといった欠点があるためである。In other words, electrolytic capacitors such as those described above are desired to have high breakdown voltage and low leakage current. It is important to reduce the content of hydrogen (generic term for hydrogen). This is because elements other than the valve metal are difficult to be anodized, so these impurities make it difficult to form an oxide film, resulting in an increase in leakage current.
本発明は、以上の様な問題点を解消するために提案され
たもので、その目的は、漏れ電流の小さい、高品質の電
解コンデンサを得ることのできる電解コンデンサの製造
方法を提供することにある。The present invention was proposed to solve the above-mentioned problems, and its purpose is to provide a method for manufacturing an electrolytic capacitor that can produce a high-quality electrolytic capacitor with low leakage current. be.
［課題を解決するための手段］
本発明の電解コンデンサの製造方法は、弁作用金属粉末
として、その中に含有される燐濃度を４０ＰＰＭ以下に
抑えたものを用いたことを特徴とするものである。[Means for Solving the Problems] The method for manufacturing an electrolytic capacitor of the present invention is characterized in that a valve metal powder containing phosphorus concentration of 40 PPM or less is used. be.
［作用］
本発明の電解コンデンサの製造方法によれば、弁作用金
属粉末中に含有される燐濃度を４０ＰＰＭ以下に抑える
ことにより、酸化皮膜の欠陥部を減少させ、酸化皮膜に
亀裂が生じることを防止できる。[Function] According to the method for manufacturing an electrolytic capacitor of the present invention, by suppressing the phosphorus concentration contained in the valve metal powder to 40 PPM or less, defects in the oxide film are reduced and cracks are not generated in the oxide film. can be prevented.
［実施例］
以下、本発明の一実施例を第１図乃至第４図に基づいて
具体的に説明する。[Example] Hereinafter, an example of the present invention will be specifically described based on FIGS. 1 to 4.
本実施例の構成＊
本実施例の電解コンデンサにおいては、弁作用金属粉末
として、その中に含まれる燐濃度を４０ＰＰＭ以下に抑
えたものを使用する。Structure of this embodiment* In the electrolytic capacitor of this embodiment, a valve metal powder containing phosphorus concentration of 40 PPM or less is used.
本実施例の作用＊
この様な構成を有する本実施例の電解コンデンサの効果
を調べるために、以下に述べる様な実験を行った。即ち
、化成皮膜形成後の漏れ電流特性を調べるために、燐濃
度を変えたタンタル粉末を、厚さ１．５ｍｍ、高さ３．
５ｍｍ、幅２．０ｍｍに成形し、その中に０，３φのタ
ンタル線を植立させ、成形素子としたタンタルペレット
を、１×１Ｏ−６Ｔｏｒｒの真空度で、１５５０°Ｃ１
３０分焼結を行った。この様にして得られたタンタルペ
レットを、４０°Ｃ２６０°Ｃ１９０°Ｃのリン酸電解
質中で、化成電圧１００Ｖ、化成時間３時間で酸化皮膜
を形成し、その後、常温のリン酸水溶液中において、４
１１定電圧７０Ｖを印加、２分後の漏れ電流を測定した
。Effects of this Example* In order to investigate the effects of the electrolytic capacitor of this example having such a configuration, the following experiment was conducted. That is, in order to investigate the leakage current characteristics after the formation of a chemical conversion film, tantalum powder with different phosphorus concentrations was placed in a 1.5 mm thick and 3.5 mm high layer.
The tantalum pellets were molded into a size of 5 mm and a width of 2.0 mm, into which a 0.3φ tantalum wire was planted, and used as a molded element.
Sintering was performed for 30 minutes. The tantalum pellets obtained in this way were formed into an oxide film in a phosphoric acid electrolyte at 40°C, 260°C, and 190°C at a formation voltage of 100V and a formation time of 3 hours, and then placed in a phosphoric acid aqueous solution at room temperature. 4
11 A constant voltage of 70 V was applied, and the leakage current was measured after 2 minutes.
その結果を第１図及び第２図に示した。即ち、第１図に
示した様に、燐濃度が７０ＰＰＭ付近に変曲点があるこ
とが判明し、また、燐濃度が５０ＰＰＭ以下においては
、漏れ電流に大きな影響を与えないという結果が得られ
た。また、第２図に示した様に、燐濃度が７０ＰＰＭ以
下のものにおいては、化成液の温度に左右されることは
少なく、特に、４３ＰＰＭ以下のものにおいては、漏れ
電流に大きな影響を与えないという結果が得られた。The results are shown in FIGS. 1 and 2. In other words, as shown in Figure 1, it was found that there was an inflection point near the phosphorus concentration of 70 PPM, and the results showed that the leakage current was not significantly affected when the phosphorus concentration was 50 PPM or less. Ta. In addition, as shown in Figure 2, when the phosphorus concentration is 70 PPM or less, it is not affected by the temperature of the chemical solution, and in particular, when the phosphorus concentration is 43 PPM or less, it does not have a large effect on the leakage current. The result was obtained.
次に、化成後陰極層を形成し、製品化した固体電解コン
デンサについて説明する。Next, a solid electrolytic capacitor manufactured by forming a cathode layer after chemical formation will be described.
即ち、コンデンサ用タンタル粉末のＣ■積が、１２００
０ＣＶ／ｇのタンタル粉末において、燐濃度が４０ＰＰ
Ｍ及び７０ＰＰＭの２種類について比較を行った。この
場合の固体電解コンデンサの製造条件は、まず、厚さ１
．５ｍｍ、高さ３゜５ｍｍ、幅２．０ｍｍ、タンタルリ
ード線０．３φで、タンクルペレットを角型の形状に成
形し、これをｌＸ１Ｏ−６Ｔｏｒｒの真空度で、１５５
０℃、３０分の真空焼結を行った。この焼結体を、６０
℃のリン酸水溶液中で化成電圧７０Ｖ、化成時間３時間
で化成処理し、酸化皮膜を形成し、その後、二酸化マン
ガン層、グラファイト層、銀ペースト層などを形成し、
陰極リードとして、洋白リードフレーム上に陽極はスポ
ット溶接、陰極部は導電性接着剤によって接続、その後
、トランスファモールドによりエポキシ樹脂にて外装を
施し、固体電解コンデンサを製造した。That is, the C product of tantalum powder for capacitors is 1200
In tantalum powder of 0CV/g, phosphorus concentration is 40PP
Two types, M and 70PPM, were compared. In this case, the manufacturing conditions for the solid electrolytic capacitor are as follows:
．． 5mm, height 3°5mm, width 2.0mm, and tantalum lead wire 0.3φ, a tankle pellet was formed into a square shape, and this was heated under a vacuum of 1×1 O-6 Torr to 155
Vacuum sintering was performed at 0°C for 30 minutes. This sintered body was
A chemical conversion treatment is performed in a phosphoric acid aqueous solution at a temperature of 70 V for a formation time of 3 hours to form an oxide film, and then a manganese dioxide layer, a graphite layer, a silver paste layer, etc. are formed.
As a cathode lead, the anode was spot welded onto a nickel silver lead frame, the cathode was connected with conductive adhesive, and then covered with epoxy resin by transfer molding to produce a solid electrolytic capacitor.
この様な電解コンデンサについて、以下の処理を施した
各試料について、１２０Ｈｚ容量における容量変化率（
％）、ＩＫＨｚ損失における損失角の正装（％）、漏れ
電流（μＡ）の測定を行い、特性の変化を調べた。Regarding such electrolytic capacitors, the capacitance change rate at 120Hz capacity (
%), formal loss angle (%) at IKHz loss, and leakage current (μA) were measured to examine changes in characteristics.
なお、測定に用いた各試料の処理条件は、以下に示す通
りである。Note that the processing conditions for each sample used in the measurement are as shown below.
（従来のタンタル粉末）
含有燐濃度ニア０ＰＰＭ
試料定格： １６Ｖ−６，８μＦ
試験条件：２７０°Ｃ−１０ｓ半田浸漬試料数：ｎ＝１
７
［試料番号コ し処理方法］
１ 未処理
２ 熱処理
３ ＰＣＴ２
４ ＰＣＴ４
５ ＰＣＴ６
６ ＰＣＴＩ
０時間
０時間
０時間
００時間
＊熱処理；２７０℃の半田に１０ｓ浸漬＊ＰＣＴ ：１
２１℃、２気圧、湿度９５〜１００％の高温、高圧、高
湿中に放置する。(Conventional tantalum powder) Phosphorus concentration near 0 PPM Sample rating: 16V-6,8μF Test conditions: 270°C - 10s solder immersion number of samples: n=1
7 [Sample number processing method] 1 Untreated 2 Heat treated 3 PCT2 4 PCT4 5 PCT6 6 PCTI 0 hours 0 hours 0 hours 00 hours *Heat treatment; Immersed in solder at 270°C for 10 seconds *PCT: 1
Leave it in a high temperature, high pressure, and high humidity environment of 21°C, 2 atm, and 95 to 100% humidity.
（改良後のタンタル粉末）
含有燐濃度：４ＱＰＰＭ
試料定格： １６Ｖ−６，８μＦ
試、験条件：２７０°Ｃ−１０ｓ半田浸漬試料数： ｎ
＝１６
［試料番号］
［処理方法］
未処理
熱処理
ＰＣＴ２０ＣＴ
２０時間０時間
ＰＣＴ６０ＣＴ
６０時間００時間
＊熱処理：２７０℃の半田に１０ｓ浸漬＊ＰＣＴ：１２
１℃、２気圧、湿度９５〜１００％の高温、高圧、高湿
中に放置する。(Tantalum powder after improvement) Concentration of phosphorus: 4QPPM Sample rating: 16V-6,8μF Test, test conditions: 270°C - 10s solder immersion Number of samples: n
=16 [Sample number] [Treatment method] Untreated heat treated PCT20CT 20 hours 0 hours PCT60CT 60 hours 00 hours *Heat treatment: Immersed in solder at 270°C for 10 seconds *PCT: 12
Leave it in a high temperature, high pressure, and high humidity environment of 1°C, 2 atm, and 95 to 100% humidity.
以上の結果を第３図〜第５図
（従来例）
及び第
６図〜第８図（改良例）に示した。即ち、改良例である
含有燐濃度が４０ＰＰＭのタンタル粉末においては、従
来例の７０ＰＰＭのタンタル粉末を用いたものに比べて
、高温、高圧、高湿度中に長時間放置した場合において
も、漏れ電流の劣化が小さいことが判明した。The above results are shown in FIGS. 3 to 5 (conventional example) and FIGS. 6 to 8 (improved example). In other words, the improved tantalum powder with a phosphorus concentration of 40 PPM has a lower leakage current than the conventional tantalum powder with a 70 PPM concentration even when left in high temperature, high pressure, and high humidity for a long time. It was found that the deterioration was small.
この様に含有燐濃度がタンタル固体電解コンデンサに与
える影響は非常に大きく、そのため、含有燐濃度を低減
することによって、酸化皮膜形成後の外部ストレスによ
る酸化皮膜の亀裂の発生を防ぐことができ、また、それ
に伴ない、漏れ電流の増加や耐電圧劣化を防ぐことがで
きるで、電解コンデンサの信頼性を大幅に向上できる。As described above, the phosphorus concentration has a very large effect on tantalum solid electrolytic capacitors. Therefore, by reducing the phosphorus concentration, it is possible to prevent cracks in the oxide film caused by external stress after the oxide film is formed. Additionally, it is possible to prevent an increase in leakage current and deterioration of withstand voltage, thereby greatly improving the reliability of the electrolytic capacitor.
［発明の効果］
以上の通り、本発明によれば、弁作用金属粉末として、
その中に含有される燐濃度を４０ＰＰＭ以下に抑えたも
のを用いるという簡単な手段によって、漏れ電流の少な
い、高品質の電解コンデンサを提供することができる。[Effects of the Invention] As described above, according to the present invention, as a valve metal powder,
A high-quality electrolytic capacitor with low leakage current can be provided by simply using a capacitor whose phosphorus concentration is suppressed to 40 PPM or less.
ル粉末を用いた場合のＰＣＴ条件下における特性をそれ
ぞれ示す特性図、第６図乃至第８図は本発明によるタン
タル粉末を用いた場合のＰＣＴ条件下における特性をそ
れぞれ示す特性図である。Figures 6 to 8 are characteristic diagrams showing the characteristics under PCT conditions when tantalum powder according to the present invention is used, respectively.
Claims (1)
て得られる焼結体を陽極体とする電解コンデンサの製造
方法において、 前記弁作用金属粉末として、その中に含有される燐濃度
を４０ＰＰＭ以下に抑えたものを用いたことを特徴とす
る電解コンデンサの製造方法。[Scope of Claim] A method for manufacturing an electrolytic capacitor in which an anode body is a sintered body obtained by sintering a molded body of valve metal powder in a high temperature and high vacuum, as the valve metal powder, A method for manufacturing an electrolytic capacitor, characterized in that the phosphorus concentration contained therein is suppressed to 40 PPM or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7894589A JPH02256224A (en) | 1989-03-29 | 1989-03-29 | Manufacture of electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7894589A JPH02256224A (en) | 1989-03-29 | 1989-03-29 | Manufacture of electrolytic capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02256224A true JPH02256224A (en) | 1990-10-17 |
Family
ID=13676028
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7894589A Pending JPH02256224A (en) | 1989-03-29 | 1989-03-29 | Manufacture of electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02256224A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08162372A (en) * | 1994-12-08 | 1996-06-21 | Nec Corp | Manufacture of electrolytic capacitor |
-
1989
- 1989-03-29 JP JP7894589A patent/JPH02256224A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08162372A (en) * | 1994-12-08 | 1996-06-21 | Nec Corp | Manufacture of electrolytic capacitor |
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