JPS62268125A - Manufacture of porous unit for electrolytic capacitor - Google Patents
Manufacture of porous unit for electrolytic capacitorInfo
- Publication number
- JPS62268125A JPS62268125A JP11285886A JP11285886A JPS62268125A JP S62268125 A JPS62268125 A JP S62268125A JP 11285886 A JP11285886 A JP 11285886A JP 11285886 A JP11285886 A JP 11285886A JP S62268125 A JPS62268125 A JP S62268125A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- particle size
- tantalum
- tantalum powder
- porous
- 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.)
- Granted
Links
- 239000003990 capacitor Substances 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 14
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000011148 porous material Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 9
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 239000000843 powder Substances 0.000 description 8
- 229910052715 tantalum Inorganic materials 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000009700 powder processing Methods 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Powder Metallurgy (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、′電解コンデンサ用多孔質体の製造方法に関
し、特にタンタルを多孔質陽極体とする電解コンデンサ
の特性改良に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for manufacturing a porous body for an electrolytic capacitor, and particularly relates to improving the characteristics of an electrolytic capacitor using tantalum as a porous anode body.
一般にタンタル電解コンデンサは、その小型大容量性、
高性能という特徴から工業用、民生用電子鏡器用コンポ
ーネントとして広範に使用されている。しかし、最近の
各種部品の軽薄短小化、低価格化およびチップ部品を中
心とする自動実装技術の進歩の流れの中で今迄以上に小
型化、低価格化が望まれる情況になってきている。そし
て、この情況に対処する技術的な手段の一つとして、タ
ンタル電解コンデンサの基本部分である多孔質陽極体を
構成しているタンタル粉末の粒径を小さくすることによ
り、比表面積（単位体積当りの表面撰）を大きくし、同
−靜［容量に対し使用粉末量を低減するという、いわゆ
る粉末の高りｖ化技術の検討が進み、徐々に製品ベース
に適用されつつある。In general, tantalum electrolytic capacitors are characterized by their small size and large capacity.
Due to its high performance, it is widely used as a component for industrial and consumer electronic mirrors. However, with the recent trends of miniaturization and reduction in prices of various components and advances in automatic mounting technology centered on chip components, the situation has become more desirable than ever for miniaturization and lower prices. . One of the technical means to deal with this situation is to reduce the particle size of the tantalum powder that makes up the porous anode body, which is the basic part of tantalum electrolytic capacitors. Research is progressing on so-called high-v powder technology, which increases the surface area of the powder and reduces the amount of powder used relative to the volume, and is gradually being applied to product bases.
上述した粉末の高りｖ化技術は、従来と岡−の粉末処理
技術ペースで単純に粉末の粒径を小さくしていくという
方法をそのまま適用したのでは、ある一定粒径以下の粉
末で空孔構造が微細化し過ぎ、固体化方法として通常行
われている硝酸マンガンの熱分解による二酸化マンガン
の半導体陰極付けが困難となる。その結果、コンデンサ
としての等個直列抵抗（ＥＡＲ）おるいはｔａｎδが異
常に増大したり、漏れ電流（Ｌ Ｃ） １１が大きくな
る等充分な特性が確保できなくなるという問題が生じて
くる。The above-mentioned technology for increasing the height of V of powder cannot be achieved by applying the method of simply reducing the particle size of the powder at the same pace as Oka's conventional powder processing technology. The pore structure becomes too fine, making it difficult to attach a semiconductor cathode to manganese dioxide by thermally decomposing manganese nitrate, which is a usual solidification method. As a result, problems such as an abnormal increase in the equal series resistance (EAR) or tan δ of the capacitor and an increase in the leakage current (LC) 11 occur, making it impossible to ensure sufficient characteristics.
本発明の目的は、このような問題点を解決し、小石な粒
径のタンタル粉末を使用して、単位体積当りの静電容量
を大きくしてもコンデンサとして充分な固体化特性が得
られる電解コンデンサ用多孔質体の製造方法を提供する
ことにある。The purpose of the present invention is to solve these problems and to develop an electrolytic method that uses tantalum powder with a pebble particle size to obtain sufficient solidification characteristics as a capacitor even if the capacitance per unit volume is increased. An object of the present invention is to provide a method for manufacturing a porous body for a capacitor.
本発明によれば、
タンタル粉末を圧縮成形、熱処理して得られる多孔質焼
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
、上記圧縮成形前のタンタル粉末に、タンタル粉末の平
均粒径よりも大きい平均粒径のアルミニウム粉末を一定
量添加、混合すること、および、タンタル粉末に添加す
る上記アルミニウムの量を５′かち；１０体積％、同平
均粒径をタンタル粉末の２倍から６倍の範囲とすること
を特徴とする電解コンデンサの製造方法が得られる。According to the present invention, in the method for manufacturing an electrolytic capacitor in which a porous sintered body obtained by compression molding and heat treating tantalum powder is used as an anode body, the tantalum powder before compression molding is added with Adding and mixing a certain amount of aluminum powder with a large average particle size, and increasing the amount of aluminum added to the tantalum powder to 10% by volume, with the same average particle size being 2 times to 6 times that of the tantalum powder. There is obtained a method for manufacturing an electrolytic capacitor, characterized in that the capacitance is within the range of .
タンタル粉末にアルミニウム粉末を添加、混合し、圧縮
成形したのち熱処理した場合の多孔質焼結体の形成過程
は次のようになる。タンタルに比べて融点の極端に低い
アルミニウム（融点約６６０”Ｏ）は、昇温過程の途中
、アルミニウムの融点近傍で周囲のタンタル粉末の粒子
に対して一方的に固相拡散あるいは融解して、タンタル
粒子と合金化する。そして最終熱処理温度に到達する過
程で、タンタルあるいはアルミニウムと合金化したタン
タルの粉末同志がシンター結合して、多孔質焼結体を形
成する。ここで注目すべきことは、もともとタンタル粒
子のあった部分が多孔質焼結体の基本構成枠として残９
、アルミニウム粒子の存在した部分が空孔になるという
多孔質体の生成過程を辿ることでわる。従って、存在し
たアルミニウム粒子の大小に応じた大きさの空孔が焼結
体内部に残るという特徴を有する。このことは、添加す
るアルミニウム粉末の飯と粒度を調整することにより、
多孔質体の内部空孔構造を容易にコントロールすること
が可能であることを示唆している。The process of forming a porous sintered body when aluminum powder is added and mixed with tantalum powder, compression molded, and then heat treated is as follows. Aluminum, which has an extremely low melting point compared to tantalum (melting point approximately 660"O), unilaterally solid-phase diffuses or melts into the surrounding tantalum powder particles near the melting point of aluminum during the heating process. It is alloyed with tantalum particles.Then, in the process of reaching the final heat treatment temperature, the tantalum or tantalum powder alloyed with aluminum sinter-bonds with each other to form a porous sintered body.What should be noted here is , the part where tantalum particles were originally located remains as the basic structural frame of the porous sintered body.
This occurs by following the formation process of a porous body in which the areas where aluminum particles were present become pores. Therefore, the sintered body is characterized in that pores of a size corresponding to the size of the existing aluminum particles remain inside the sintered body. This can be achieved by adjusting the size and particle size of the aluminum powder added.
This suggests that it is possible to easily control the internal pore structure of porous materials.
本発明者は、高融点金属であるタンタル粉末に低融点金
属であるアルミニウム粉末を添加すると、このような独
特の多孔質体形成過程を辿るという特徴に看目し、添加
するアルミニウム粉末の童と粒度調整を行うことによっ
て、多孔質体の内部空孔構造に意識的に分布を持たせ、
これがタンタル電解コンデンサの固体化特性の向上に著
しい効果をもたらすことを確認した。空孔を形成する穴
の大きさに大小の分布を有する多孔質体が得られる結果
、硝酸マンガンの含浸性が向上し、二酸化マンガン半導
体ａｆ＝にの等個直列抵抗が低減され、固体化特性が向
上することになる。The inventor of the present invention noticed that when aluminum powder, which is a low melting point metal, is added to tantalum powder, which is a high melting point metal, a unique porous body formation process occurs. By adjusting the particle size, we intentionally create a distribution in the internal pore structure of the porous material,
It was confirmed that this has a significant effect on improving the solid state properties of tantalum electrolytic capacitors. As a result of obtaining a porous body having a size distribution of the pores forming the pores, the impregnating property of manganese nitrate is improved, the series resistance of the manganese dioxide semiconductor af is reduced, and the solidification properties are improved. will improve.
以下、本発明を実施例によし詳細に説明する。 Hereinafter, the present invention will be explained in detail with reference to Examples.
平均粒径３μｍのタンタル粉末に、アルミ粉末を第１表
中に示すような水準内容で添加し、各水準の添加済粉末
を充分に混合した後、圧縮成形し、Ｉ Ｘ １０ ”ｒ
ｒｒｎＨｌの減圧下４００’Ｏ／Ｈｒの昇温速度で１７
００″Ｃ−３０分の熱処理を行い、計２２水準の多孔質
焼結体を作製した。これら２２水準の多孔室体試料すべ
てを０．０５ ＶＯｆ１％ リフ酸水溶液中で８０Ｖの
陽＃、酸化を行い、１２０Ｈｚでの靜蛋容ｆｉｔ （Ｃ
ｘ２０）、単位体積当りのｃｖｆ値（ＣＶｔ／ＶＤ １
．）および１６Ｖ印加時の漏れ電流（Ｌｅ）特性を測定
した。また化成後の試料に対し、硝酸マンガンの含浸、
熱分解プロセスを７回繰り返し二酸化マンガン陰極付を
行い、更にグラファイト、銀ペースト付、半田付を行っ
て固体化した状態で、鼾篭８Ｍｍａ率、コンデンサ全体
としての１２０Ｈｚでの損失（ｊａｎδ１２ｏ）とｔａ
ｎａｘｚｏイｊＫのうちの二酸化マンガン等の外部陰極
の等１．１１貝列抵抗にもとづく損失成分（ｔａｎδｏ
）、および１６Ｖ印加時の濁れ電流を測定した。ここで
、靜電容を被覆率は、固体化後の静電容量と化成後ｗｅ
ｔでの静電容量（共に１２０Ｈｚｊ直）との比で定義し
た。Aluminum powder was added to tantalum powder with an average particle size of 3 μm at the levels shown in Table 1, and after thoroughly mixing the added powder at each level, compression molding was performed to form an I x 10” r
17 at a heating rate of 400'O/Hr under reduced pressure of rrnHl
A total of 22 levels of porous sintered bodies were prepared by heat treatment at 00"C for 30 minutes. All of these 22 levels of porous chamber body samples were oxidized at 80V in a 0.05 VOf1% refic acid aqueous solution. and a silent fit at 120Hz (C
x20), cvf value per unit volume (CVt/VD 1
．． ) and leakage current (Le) characteristics when 16V was applied were measured. In addition, the sample after chemical conversion was impregnated with manganese nitrate,
The thermal decomposition process was repeated 7 times and a manganese dioxide cathode was attached, followed by graphite, silver paste, and soldering to solidify the capacitor.
Loss component (tan δ o
), and the clouding current when 16V was applied were measured. Here, the coverage rate of the static capacitance is the capacitance after solidification and the we after formation.
It was defined as the ratio to the capacitance at t (both 120Hz direct).
以上の測定の結果刊もれたデータを第１表に示す。Table 1 shows the data that was left out as a result of the above measurements.
各試料水準について化成後、固体化後共５０個測定し、
その平均１筐をデータとして示した。For each sample level, 50 pieces were measured after chemical formation and after solidification.
The average of one box is shown as data.
第１表から次のことがわかる。The following can be seen from Table 1.
アルミニウム粉末を無添加の試料（ｍｚ ２ ）は、固
体化後の静電容量被覆率が９０％と低く、ｔａｎδ１２
０が４チと大きくなっている。また、ＬＣも化成後ｗｅ
ｔに対し固体化時の劣化程度が太きい。これに対し、タ
ンタル粉末の平均粒径より大きいアルミニウム粉末を添
加した試料（Ｎ１１〜に２１）では、静電容量板＆率が
同上し、固体化後のｔａｎδ１２０およびＬＣが低減さ
れ、全体としてアルミニウム粉末を無添加の試料と比べ
特性が向上し、改良されていることがわかる。The sample (mz 2 ) with no aluminum powder added had a low capacitance coverage of 90% after solidification, and tan δ12
0 is large at 4chi. In addition, LC is also used after chemical formation.
The degree of deterioration during solidification is greater than t. On the other hand, in the samples (N11 to 21) in which aluminum powder larger than the average particle size of tantalum powder was added, the capacitance plate & ratio were the same as above, the tan δ120 and LC after solidification were reduced, and the aluminum powder as a whole It can be seen that the powder has improved properties compared to the sample without additives.
但し、アルミニウム粉末の添加量が多過ぎると、１５体
ｔＪ［％の例（試料用１９〜２１）に見るように、小型
大容量性を表わすＣＶｆ／ＶＯ１値が極端に低下してし
まい、粉末扁Ｃ■化の意味が実質的に失われてしまうほ
か、ｔａｎδ、２ＩＩＩ、ＬＣ特性改良効果がそれ程得
られなくなってしまう。However, if the amount of aluminum powder added is too large, as shown in the example of 15 body tJ[% (19 to 21 for samples)], the CVf/VO1 value, which indicates small size and large capacity, will be extremely reduced, and the powder In addition to substantially losing the meaning of flattening the C2, the effects of improving tan δ, 2III, and LC characteristics are no longer obtained.
また、アルミニウム粉末の添加量が少な過き′ても、２
体積俤の例（試料順１〜Ｎα３）に見るように、アルミ
ニウム粉末を無添加の試料（Ｎ１１２２ ）の特性と殆
ど変わらず、改良効果が失われてしまう。これは、アル
ミニウム粉末が少ないと実質的に多孔λ体の空孔構造に
分布を持たせることができなくなってしまうためである
。In addition, even if the amount of aluminum powder added is too small, 2
As seen in the volumetric example (sample order 1 to Nα3), the properties are almost the same as those of the sample (N1122) to which no aluminum powder is added, and the improvement effect is lost. This is because if the amount of aluminum powder is small, it becomes virtually impossible to provide a distribution in the pore structure of the porous λ body.
更に、アルミニウム粉末の添加量が適当な範囲の５体積
チから１０体槓うの範囲（試料順４〜ト亀１８）でも、
アルミニウム粉末粒径がタンタル粉末粒径に比べである
範囲を逸脱すると特性改良効果がそれ程得られなくなっ
てしまう。すなわち、アルミニウム粉末粒径がタンタル
粉末粒径の４倍の２４ ｔｔｍの場合（試料１＠８，１
３．１８）には、ＬＣ特性改善効効果それ程得られない
ことのほか、ＣＶｆ／ＶＯＩ値も低下する傾向がある。Furthermore, even if the amount of aluminum powder added is in the appropriate range of 5 volumes to 10 volumes (sample order 4 to 18),
If the particle size of the aluminum powder exceeds a certain range compared to the particle size of the tantalum powder, the effect of improving the properties will not be obtained as much. That is, when the aluminum powder particle size is 24 ttm, which is four times the tantalum powder particle size (sample 1 @ 8, 1
3.18), in addition to not being able to obtain much of an LC characteristic improvement effect, there is also a tendency for the CVf/VOI value to decrease.
また、アルミニウム粉末粒径が小さく、タンタル粉末ト
同じ場合（試料Ｎ１４，９．１４）には、ｔａｎδ１２
０およびＬＣ特性改善効果が失われる。この場合の原因
はアルミニウム粉末粒径が小さいと、アルミニウムが融
解、拡散合金化して抜けたあとに残る空孔径が小さく、
結果として空孔構造に分布を持たせることができなくな
るためである。In addition, when the aluminum powder particle size is small and the tantalum powder is the same (sample N14, 9.14), tan δ12
The effect of improving 0 and LC characteristics is lost. The reason for this is that when the aluminum powder particle size is small, the pore size remaining after the aluminum melts, diffuses and alloys and escapes is small.
This is because, as a result, the pore structure cannot be distributed.
以上説明して来たことかられかるように、本発明の製造
方法による特性改善効果が極立って発現するためには、
タンタル粉末に添刀口するアルミニウム粉末の景を５体
積チから１０体槓％、同平均粒径をタンタル粉末の２倍
から６倍の範囲とするのが好ましい。As can be seen from what has been explained above, in order for the production method of the present invention to exhibit the characteristic improvement effect to the utmost, it is necessary to
It is preferable that the size of the aluminum powder added to the tantalum powder is 5 to 10% by volume, and the average particle size is in the range of 2 to 6 times that of the tantalum powder.
以上説明したように本発明は、粒径の小さいタンタルの
高ＣＶ粉末にタンタル粉床より粒径の大きいアルミニウ
ム粉末を一定量添加、混合することによって多孔質陽極
体の空孔構造が改哲され、優れた固体化特性を確株する
ことできる効果がある。As explained above, the present invention improves the pore structure of the porous anode by adding and mixing a certain amount of aluminum powder, which has a larger particle size than the tantalum powder bed, to a high CV tantalum powder with a small particle size. This has the effect of ensuring excellent solidification properties.
従って、本発明の有用性の高いことは明らかである。Therefore, it is clear that the present invention is highly useful.
代理人 弁理士 内 原 −−”′ゝ・「３Agent Patent Attorney Uchihara --"'"・"3
Claims (2)
孔質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、前記圧縮成形前のタンタル粉末に、タンタル粉
末の平均粒径よりも大きい平均粒径を有するアルミニウ
ム粉末の一定量を添加・混合することを特徴とする電解
コンデンサ用多孔質体の製造方法。(1) In a method for manufacturing an electrolytic capacitor in which a porous sintered body obtained by compression molding and heat treating tantalum powder is used as an anode body, the tantalum powder before compression molding has an average particle size larger than the average particle size of the tantalum powder. A method for producing a porous body for an electrolytic capacitor, which comprises adding and mixing a certain amount of aluminum powder having a particle size.
量を５体積％から１０体積％、同平均粒径をタンタル粉
末の２倍から６倍の範囲とすることを特徴とする特許請
求範囲第１項記載の電解コンデンサ用多孔質体の製造方
法。(2) The amount of aluminum powder added to the tantalum powder is from 5% by volume to 10% by volume, and the average particle size is from 2 times to 6 times that of the tantalum powder. The method for manufacturing the porous body for electrolytic capacitors described above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11285886A JPS62268125A (en) | 1986-05-16 | 1986-05-16 | Manufacture of porous unit for electrolytic capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11285886A JPS62268125A (en) | 1986-05-16 | 1986-05-16 | Manufacture of porous unit for electrolytic capacitor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62268125A true JPS62268125A (en) | 1987-11-20 |
| JPH0553052B2 JPH0553052B2 (en) | 1993-08-09 |
Family
ID=14597294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11285886A Granted JPS62268125A (en) | 1986-05-16 | 1986-05-16 | Manufacture of porous unit for electrolytic capacitor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62268125A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001091953A1 (en) * | 2000-06-01 | 2001-12-06 | Cabot Supermetals K.K. | Niobium or tantalum powder and method for production thereof, and solid electrolytic capacitor |
-
1986
- 1986-05-16 JP JP11285886A patent/JPS62268125A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001091953A1 (en) * | 2000-06-01 | 2001-12-06 | Cabot Supermetals K.K. | Niobium or tantalum powder and method for production thereof, and solid electrolytic capacitor |
| US7204866B2 (en) | 2000-06-01 | 2007-04-17 | Cabot Supermetals K.K. | Niobium or tantalum powder and method for production thereof, and solid electrolytic capacitor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0553052B2 (en) | 1993-08-09 |
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