WO2005015586A1 - Conducteur d'electrode positive pour condensateur electrolytique - Google Patents

Conducteur d'electrode positive pour condensateur electrolytique Download PDF

Info

Publication number
WO2005015586A1
WO2005015586A1 PCT/JP2004/011723 JP2004011723W WO2005015586A1 WO 2005015586 A1 WO2005015586 A1 WO 2005015586A1 JP 2004011723 W JP2004011723 W JP 2004011723W WO 2005015586 A1 WO2005015586 A1 WO 2005015586A1
Authority
WO
WIPO (PCT)
Prior art keywords
electrolytic capacitor
tantalum
niobium
anode
rare earth
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.)
Ceased
Application number
PCT/JP2004/011723
Other languages
English (en)
Japanese (ja)
Inventor
Makoto Masubuchi
Tsunenori Saji
Kazuyoshi Matsumoto
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cabotsupermetals KK
Original Assignee
Cabotsupermetals KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Cabotsupermetals KK filed Critical Cabotsupermetals KK
Publication of WO2005015586A1 publication Critical patent/WO2005015586A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/07—Alloys based on nickel or cobalt based on cobalt

Definitions

  • the present invention relates to an anode lead for an electrolytic capacitor, and an anode for an electrolytic capacitor and an electrolytic capacitor using the same.
  • anode conductors are usually used for electrolytic capacitors.
  • tantalum (T a) conductors two methods are common and one is manufactured by processing from a tantalum ingot. In other words, tantalum powder is melted, made into ingots, and then forged, mouth-ringed, etc. Most of the impurities evaporate since the melting point of tantalum is 300 ° C. Removed. The other is to press-mold tantalum powder by powder metallurgy and then sinter it. Although this method does not dissolve, it is somewhat difficult in terms of purity, but has the advantage that the necessary additives are mixed uniformly to easily control the properties.
  • the tantalum anode conductor manufactured by such a method has a so-called round cross section, but a flat band (tape) conductor has recently been proposed to increase the contact area with the anode body. (DE 1004 085 3).
  • a flat band (tape) conductor has recently been proposed to increase the contact area with the anode body.
  • such an improved conducting wire is not easily fixed to the anode body as compared with the round shape, and has a drawback in formability.
  • the demand for tantalum materials that can withstand severe repeated use at high temperatures and have an extended life is increasing along with the increase in the capacity of capacitors, and various other studies and proposals are being made. One of them is to reduce embrittlement due to coarse growth of crystal grains due to high temperature.
  • doping tantalum with a rare earth element has also been proposed (Japanese Patent Laid-Open No. 6-67070). Disclosure of the invention
  • An object of the present invention is to provide a tantalum or niobium (Nb) anode conductive wire which has improved sintering characteristics and thus can be stably fixed to the anode body and sufficiently exhibits the inherent characteristics of the conductive wire.
  • the gist of the present invention is an anode conductive wire for an electrolytic capacitor, which is made of a tantalum or niobium material containing 0.01 to 3 ppm of a rare earth element and has a tape-like shape.
  • the present invention dissolves a tantalum or niobium powder containing 0.5 to 3% of a rare earth element, obtains an ingot containing 0.01 to 3 ppm of a rare earth element, and then forges and rolls the ingot.
  • a tape-shaped conductor is obtained.
  • Shape is tape Method for producing an electrolytic capacitor anode wire, characterized in that to obtain a conductive wire is, and the gist. Further, the present invention provides an anode for an electrolytic capacitor including the above-described conductive wire, and an electrolytic capacitor further including the anode for an electrolytic capacitor.
  • Electrolysis anode lead wire capacitor of the present invention is properly be tantalum to 0. 0 1 ⁇ 3 pp m containing a rare earth element is made of niobium materials, shape is a tape.
  • rare earth elements include scandium (S c), yttrium (Y) and 15 lanthanide elements, that is, lanthanum (La) and cerium (Ce) with atomic numbers 57 to 71.
  • the tantalum material may further include one or more of tungsten, molybdenum, or niobium in order to further improve the insert characteristics during press molding, as described below. It is preferably contained in an amount of 0 to 500 ppm. Similarly, the niobium material preferably further contains 10 to 500 ppm of one or more of tungsten or molybdenum.
  • the tape shape varies depending on the application, but it is usually 10 to 500 / zm in thickness and 0.5 to 5 mm in width.
  • the cross section in the width direction is preferably rectangular or corrugated.
  • a tantalum material is annealed, and a micro Vickers hardness of 100 to 14 is used. 0, elongation 4 0% or more and tensile strength of 4 is 0 ON / mm 3 or less.
  • niobium and material is annealed, micro Vickers hardness 7 0-1 1 0 is the elongation 2 0-4 5% and tensile strength 3 0 0 N / mm 3 or less .
  • annealing can be performed by a conventional method. For example, in the case of a rolling method described later, it is preferable to perform vacuum annealing after reaching a final thickness.
  • anode conductor for an electrolytic capacitor according to the present invention is that the tantalum material is not annealed, has a micro Vickers hardness of 200 to 250, and an elongation of 10% or less. And the tensile strength is 60 ON / mm 3 or less.
  • niobium material is the green blunt, microphones Robikkasu hardness 1 5 0-2 0 0, an elongation of 4 5% or less and the tensile strength 4 0 ON / mm 3 or less.
  • a tantalum or niobium material containing 0.01 to 3 ppm of a rare earth element which is used as a raw material for producing an anode conductor for an electrolytic capacitor, can be obtained by an ordinary method.
  • tantalum or niobium powder is produced by diluting tantalum or niobium-containing metal salt such as tantalum calcium fluoride or niobium fluoride in dilute salt into sodium or potassium. It is common to use a method of reducing at a high temperature of 700 ° C. or more by using such methods. Examples of such a diluting salt include potassium fluoride, potassium chloride, sodium chloride or a mixture containing them.
  • the tantalum or niobium material of the present invention is usually obtained by adding a rare earth element to the tantalum or niobium material thus obtained.
  • the addition of the rare earth element is preferably a simple substance or an oxide. For example, when blending the raw material powder, they can be weighed and blended together.
  • the tantalum material is pressed as described below. (Pressure)
  • one or more of tungsten, molybdenum and niobium are further contained in an amount of 10 to 50 ppm.
  • the niobium material further contains at least one of tungsten and molybdenum at 10 to 50 Oppm. It is preferable that these elements are added alone.
  • the anode conductor for an electrolytic capacitor according to the present invention can be suitably manufactured by using an ingot method or a powder metallurgy method using such a tantalum or niobium material.
  • tantalum or niobium powder containing 0.5 to 3 wt% of a rare earth element is preferably melted by electron beam melting to obtain an ingot. Since the above-mentioned tantalum or niobium powder evaporates during dissolution, the rare earth element content is 0.5 in consideration of conditions such as the dissolution temperature so that the rare earth element remains in the ingot at 0.01 to 3 ppm. ⁇ 3 wt%.
  • the rare earth element content is determined in consideration of the sintering temperature and the like so that the rare earth element remains in the sintered body at 0.01 to 3 ppm. Is selected from 0.1 to 1 wt%. Then, the obtained sintered body is rolled and then slit or grooved to form a tantalum or niobium material containing 0.01 to 3 ppm of a rare earth element. Is tape-shaped A certain conductor can be obtained. Rolling, slitting or grooving can be carried out in a conventional manner. It is preferable that its cross section in the width direction is rectangular or corrugated.
  • the conductive wire thus obtained is particularly suitable as an anode for an electrolytic capacitor, and the anode for an electrolytic capacitor can be prepared by a conventional method.
  • the conductive wire of the present invention high-temperature embrittlement can be reduced, and the contact area with the anode body can be increased.
  • the insert characteristics are improved, the sintering characteristics with the powder are improved, and the pull-out strength of the conductor is improved.
  • An electrolytic capacitor including such an anode for an electrolytic capacitor can be manufactured by an ordinary method.
  • the nickel-made alloy reaction vessel After drying the nickel-made alloy reaction vessel at 130 ° C., it was dried using potassium fluoride as a diluting salt, and then filled into the reaction vessel from a dryer. Thereafter, the lid was closed and the atmosphere was sufficiently replaced with argon gas. This was heated to 800 ° C. and dried, and then the tantalum fluoride roll was reduced using sodium metal as a reducing agent. After cooling, the lid was opened and the product was washed with water and further washed with mixed acid to obtain a tantalum powder. A uniform mixed powder was obtained by adding a titanium oxide to this tantalum powder (ittrium content: about 1 wt%).
  • the yttrium-containing tantalum powder is melted in an electron beam at a temperature of 300 ° C. or more to form an ingot having an yttrium content of 0.05 ppm, and the surface of the ingot is cut. After removal, press forging to 3 O mm, Then, it was rolled to 0.15 mm by a roll rolling mill. Finally, it was cut to a predetermined width (2 mm) by a slit machine to produce a tape-like conductor (0.15 X 2 mm in cross section).
  • the tantalum powder and the organic binder resin were mixed, filled into a mold of a pressure molding machine, and one end of the above-mentioned tape-shaped wire was inserted therein, and pressure-molded into a specific shape. Then removed by heating the organic binder resin at 4 0 0 ° C Da argon stream, a higher vacuum atmosphere furnace ( ⁇ ⁇ 1 0 5 T 0 rr) in the high-temperature heat treatment (about 1 3 5 0 ° C) to obtain a porous sintered body.
  • the insert characteristics to the tantalum powder during the above molding and the sintering characteristics with the powder were remarkably improved as compared with the case of using tantalum powder containing no titanium (Comparative Example 1). . Table 1 shows these results as the insert linearity during press forming and the pellet strength (ie, the wire pull-out strength).
  • the test method was as follows.
  • Insert linearity during press molding Evaluated by the number of defects per 100 press molded articles.
  • the anode conductor is in a stable state with respect to the pressed body
  • Pellet strength that is, wire pull-out strength: Evaluated in an anode wire pull-out test of the press-formed body and the sintered body. It is an important item in the capacitor manufacturing process that the anode conductor is not detached (stripped) or broken in the pressed and sintered bodies.
  • this porous sintered body was used as an anode in a phosphoric acid aqueous solution to be anodized to form a dielectric film on the surface. Thereafter, a solid electrolyte layer, a carbon layer, and a metal layer were formed on the dielectric film to obtain a solid electrolytic capacitor element.
  • This capacitor element is further connected to a lead frame by a conventional method, and is molded with a thermosetting synthetic resin to form a tantalum solid electrolytic capacitor.
  • a press-formed body and a sintered body were obtained in the same manner as in Example 1 except that metal tungsten, molybdenum and niobium were further added in addition to the titanium oxide.
  • Table 1 also shows the results of insert linearity and pellet strength tested in the same manner as in Example 1.
  • the tape-shaped conductor of the present invention By using the tape-shaped conductor of the present invention, high-temperature embrittlement can be reduced, the contact area with the anode body can be increased, and the insert characteristics to the powder during molding and the sintering characteristics with the powder are improved. You. Accordingly, it is possible to provide a tantalum or niobium anode conductor that can sufficiently exhibit the inherent characteristics of the conductor because it can be stably fixed to the anode body.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

L'invention concerne un conducteur d'électrode positive à base de tantale ou de niobium qui permet de réduire la fragilité à haute température, d'accroître la zone de contact avec un corps d'électrode positive et d'améliorer aussi, de façon inattendue, les caractéristiques d'insertion de poudre lors du moulage et du frittage de celle-ci, ce qui permet de la fixer de manière stable à un corps d'électrode positive et de tirer pleinement parti des propriétés inhérentes au conducteur. L'invention concerne en particulier un conducteur d'électrode positive obtenu à partir d'un matériau de tantale ou de niobium renfermant de 0,01 à 0,3 ppm d'un élément du groupe des terres rares, façonné en ruban de manière à former un conducteur d'électrode positive pour condensateur électrolytique. On peut produire par exemple un conducteur en forme de ruban, constitué d'un matériau de tantale ou de niobium renfermant de 0,01 à 0,3 ppm d'un élément du groupe des terres rares, en mettant en oeuvre les étapes consistant à : faire fondre une poudre de tantale ou de niobium contenant de 0,5 % à 3 % en poids d'un élément du groupe des terres rares ; former un lingot contenant 0,01 à 0,3 ppm d'un élément du groupe des terres rares ; forger et laminer séquentiellement le lingot ; et refendre ou réusiner celui-ci au cylindre cannelé.
PCT/JP2004/011723 2003-08-12 2004-08-10 Conducteur d'electrode positive pour condensateur electrolytique Ceased WO2005015586A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2003-207380 2003-08-12
JP2003207380A JP2005064038A (ja) 2003-08-12 2003-08-12 電解コンデンサ用陽極導線

Publications (1)

Publication Number Publication Date
WO2005015586A1 true WO2005015586A1 (fr) 2005-02-17

Family

ID=34131428

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2004/011723 Ceased WO2005015586A1 (fr) 2003-08-12 2004-08-10 Conducteur d'electrode positive pour condensateur electrolytique

Country Status (2)

Country Link
JP (1) JP2005064038A (fr)
WO (1) WO2005015586A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070044873A1 (en) * 2005-08-31 2007-03-01 H. C. Starck Inc. Fine grain niobium sheet via ingot metallurgy
JP4776522B2 (ja) * 2006-12-20 2011-09-21 三洋電機株式会社 固体電解コンデンサ
CN101477897B (zh) * 2009-01-20 2012-05-23 宁夏东方钽业股份有限公司 钽电容器阳极引线用钽丝及其制造方法
JP6412501B2 (ja) * 2013-10-08 2018-10-24 昭和電工株式会社 ニオブ造粒粉末の製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991019015A1 (fr) * 1990-06-06 1991-12-12 Cabot Corporation Alliages a base de tantale ou de niobium
JPH0665670A (ja) * 1992-08-20 1994-03-08 Showa Kiyabotsuto Suupaa Metal Kk タンタル材料及びその製造方法
JP2000012387A (ja) * 1998-06-19 2000-01-14 Matsushita Electric Ind Co Ltd 電解コンデンサ用電極

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991019015A1 (fr) * 1990-06-06 1991-12-12 Cabot Corporation Alliages a base de tantale ou de niobium
JPH0665670A (ja) * 1992-08-20 1994-03-08 Showa Kiyabotsuto Suupaa Metal Kk タンタル材料及びその製造方法
JP2000012387A (ja) * 1998-06-19 2000-01-14 Matsushita Electric Ind Co Ltd 電解コンデンサ用電極

Also Published As

Publication number Publication date
JP2005064038A (ja) 2005-03-10

Similar Documents

Publication Publication Date Title
JPWO2000049633A1 (ja) ニオブ粉、ニオブ焼結体、該焼結体を用いたコンデンサおよびそのコンデンサの製造方法
KR20030051734A (ko) 전해 커패시터 기판용의 탄탈과 질화탄탈 분말의 혼합물
JP2016522318A (ja) 高い表面積を有する酸素貧有のバルブ金属焼結体の製造法
EP1275124B1 (fr) Poudre de niobium pour condensateur, corps fritte de cette poudre et condensateur utilisant le corps fritte
EP1340235B1 (fr) Poudre pour condensateur, corps fritte et condensateur utilisant ce corps fritte
RU2341577C2 (ru) Стойкая к высоким температурам ниобиевая проволока
JPWO2001006525A1 (ja) ニオブ粉、その焼結体およびそれを使用したコンデンサ
US20030117766A1 (en) Niobium powder for capacitor, sintered body using the powder and capacitor using the same
WO2005015586A1 (fr) Conducteur d'electrode positive pour condensateur electrolytique
AU2002218510A1 (en) Powder for capacitor, sintered body thereof and capacitor using the sintered body
CN104495929B (zh) 低价氧化铌粉末及其制备方法
US7132006B2 (en) Niobium powder for capacitor, sintered body using the powder and capacitor using the same
JP4521849B2 (ja) コンデンサ用ニオブ粉と該ニオブ粉を用いた焼結体および該焼結体を用いたコンデンサ
EP1328952B1 (fr) Poudre pour condensateur, corps fritte et condensateur comprenant ledit corps fritte
EP1264321A1 (fr) Poudre de niobium pour condensateur, corps fritte de cette poudre et condensateur utilisant le corps fritte
JP2894661B2 (ja) タンタル材料及びその製造方法
JP6258222B2 (ja) ニオブコンデンサ陽極用化成体及びその製造方法
JP2552264B2 (ja) 高靱性を有するｗ基合金焼結体の製造法
AU2002241261A1 (en) Niobium for capacitor and capacitor using sintered body of the niobium
JPWO2001081029A1 (ja) ニオブ粉、その焼結体及びコンデンサ
JP4874039B2 (ja) 電解コンデンサ陰極用アルミニウム合金箔及びそれに用いる合金箔地
JP4647744B2 (ja) コンデンサ用ニオブ粉、それを用いた焼結体及びそれを用いたコンデンサ
JP2010265549A (ja) コンデンサ用ニオブ粉
JP2006176841A (ja) 電解コンデンサ用陽極導線
KR20260053523A (ko) 고전압 탄탈륨 분말과 이의 제조 방법, 및 커패시터 애노드

Legal Events

Date Code Title Description
AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BW BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE EG ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NA NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SY TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): BW GH GM KE LS MW MZ NA SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LU MC NL PL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
122 Ep: pct application non-entry in european phase