WO2002034436A1 - Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates - Google Patents
Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates Download PDFInfo
- Publication number
- WO2002034436A1 WO2002034436A1 PCT/US2001/046281 US0146281W WO0234436A1 WO 2002034436 A1 WO2002034436 A1 WO 2002034436A1 US 0146281 W US0146281 W US 0146281W WO 0234436 A1 WO0234436 A1 WO 0234436A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- refractory metal
- powder
- mixture
- tantalum
- pellets
- Prior art date
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
- H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
- H01G9/052—Sintered electrodes
- H01G9/0525—Powder therefor
-
- 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
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/16—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on nitrides
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0068—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only nitrides
Definitions
- the pressure was maintained at near atmospheric with nitrogen additions as the temperature was increased over the next 25 minutes to 850°C.
- the pressure was reduced to 250 mm Hg and increased back to 760 mm Hg with nitrogen.
- the temperature was increased to 1030°C over a period of 50 minutes.
- the pressure was then reduced to ⁇ 0 mm Hg and the system filled with nitrogen to 810 mm Hg. The system was maintained at this temperature and pressure for five hours.
- the niobium powder was produced by magnesium reduction of a niobium pentoxide precursor.
- One kilogram of the powder was blended with 22 grams of magnesium and placed in a niobium foil lined stainless steel tray.
- the tray and its contents were put in a laboratory tube furnace.
- the tube was flushed with argon.
- the temperature of the furnace was raised to 950°C and the system maintained at this temperature for 2 hours under an argon atmosphere to deoxidize the powder.
- the furnace was allowed to cool overnight while maintaining a slight argon flow through the tube.
- the niobium nitride (NbN) powder was produced according to the same process as the niobium powder described above with the following additional steps. After the furnace cooled overnight, the powder was further processed by increasing the furnace temperature to 680°C as measured with a thermocouple inside the tube suspended over the sample and the pressure was reduced to 610 mm Hg. Using nitrogen, the pressure was increased to 760 mm Hg. Over the next thirty minutes, the temperature was increased to approximately 750°C and the pressure was maintained between 660 and 760 mm Hg by adding nitrogen gas to replace the nitrogen consumed in the reaction. At this point, the pressure was reduced to 460 mm Hg and then increased to 760 mm Hg using nitrogen.
- the powder was passivated by controlled exposure to air.
- the powder was then leached with dilute sulfuric acid to remove MgO, Mg 2 N 3 and residual Mg, and then with high purity water to remove traces of acid.
- the oxygen and nitrogen content of the powder were measured using a LECO 436 oxygen/nitrogen analyzer.
- the nitrogen concentration was 151,000 ppm corresponding to the compound NbN without excess nitrogen.
- the oxygen content was 4300 ppm.
- the tantalum and tantalum nitride powders were then blended together by a mechanical means.
- the Ta/TaN powders were mixed in proportions of 0, 25, 50, 75, and 100% TaN by weight (W/W%).
- niobium and niobium nitride powders were also blended together by a mechanical means in proportions of 0, 25, 50, 75, and 100% NbN by weight (W/W%). These powders were then used as capacitor substrates by pressing the mixtures into pellets and processing the pellets using procedures similar to those in place for making solid Ta or Nb capacitors. Similar considerations apply to other refractory metals (Ti, Zr, Hf) and refractory metal nitride mixtures and their use as capacitor substrates.
- FIGS. 4-7 show the results plotted as a function of TaN concentration and sintering temperature. Notice that the maximum pellet porosity occurs in the 50-75% TaN range. Also at any given sintering temperature, the total pellet pore surface area is relatively independent of the TaN concentration above 50%TaN and the total intrusion volume maximizes in the 50-75% TaN range.
- the tantalum agglomerates sinter faster than the tantalum nitride and shrink to leave a matrix of tantalum nitride.
- Capacitor manufactures believe that a large fraction of intra-agglomerate pores are necessary for making capacitors from high CV powders. Also, an open porosity will help to reduce the capacitor ESR.
- Table IV summarizes the wet test electrical properties of the powders. Even 25% TaN in the blend will increase the capacitance significantly relative to pure tantalum. This is especially significant in light of the fact that the dielectric constant of the anodic film in a TaN substrate is about one half that of the anodic oxide film on tantalum. The leakages were low up to 75% TaN at the 1600°C sinter condition but elevated above 25% TaN at 1700°C sinter.
- Table NI summarizes the bias dependence (in percent) of the capacitors after heat treatment. Like Ta ⁇ substrate capacitors, the capacitance of the units made from Ta/Ta ⁇ blends is insensitive to bias indicating that they did not degrade due to oxygen depletion of the anodic film during heat treatment. TABLE NI
- Sintered pellets made from blends of tantalum and tantalum nitride powders have a higher fraction of intra-agglomerate pores than those made from tantalum or tantalum nitride alone.
- a substrate consisting of a 50/50 or a 25/75 mixture of Ta/Ta ⁇ should produce solid capacitors with higher capacitance recovery and lower ESR.
- Example 2 Various Ta/Ta ⁇ mixture combinations at a given pore area or capacitance Additional testing was conducted to compare the different composition sintered pellets at the same surface area. From the Ta/Ta ⁇ mixtures, sintered pellets were made according to the pellet preparation, formation and testing conditions summarized in Table NIL The press density was 5.5 g/cm 3 and the sintering time was 20 minutes. Capacitances were measured on 0.14 gm pellets sintered at appropriate temperatures to give equivalent pore area or capacitances.
- Example 2 As mentioned in Example 1, when pellets of different composition were sintered at the same temperature they had different capacitances. This is strong evidence that the total pellet surface area is different for each pellet composition. A more meaningful comparison for capacitor applications is between pellets with the same surface area. In this Example, two measures of surface area were used. One was the pore area as calculated from the porosimetry data and the other was the capacitance, which gives a measure of the "usable" surface area.
Abstract
Description
Claims
Priority Applications (10)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002425869A CA2425869A1 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
IL15521401A IL155214A0 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitor substrates |
KR1020037005613A KR100850386B1 (en) | 2000-10-24 | 2001-10-23 | Tantalum and Tantalum Nitride Powder Mixtures for Electrolytic Capacitors Substrates, Capacitor Using said Powder Mixtures and Their Preparation Method |
EP01988636A EP1337371B1 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
MXPA03003544A MXPA03003544A (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates. |
DE60112962T DE60112962T2 (en) | 2000-10-24 | 2001-10-23 | MIXTURES OF TANTALIUM AND TANTALINITRIDE POWDER FOR SUBSTRATES FOR ELECTROLYTIC CAPACITORS |
JP2002537471A JP4294951B2 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitor substrates |
AU2002228767A AU2002228767A1 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
IL155214A IL155214A (en) | 2000-10-24 | 2003-06-04 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitor substrates |
IL173587A IL173587A0 (en) | 2000-10-24 | 2006-02-07 | Refractory metal made of a refractory metal powder and a refractory metal nitride powder, processes for its preparation and use thereof |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/695,512 US6554884B1 (en) | 2000-10-24 | 2000-10-24 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
US09/695,512 | 2000-10-24 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002034436A1 true WO2002034436A1 (en) | 2002-05-02 |
Family
ID=24793302
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/046281 WO2002034436A1 (en) | 2000-10-24 | 2001-10-23 | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
Country Status (13)
Country | Link |
---|---|
US (2) | US6554884B1 (en) |
EP (2) | EP1337371B1 (en) |
JP (1) | JP4294951B2 (en) |
KR (1) | KR100850386B1 (en) |
CN (1) | CN1309513C (en) |
AU (1) | AU2002228767A1 (en) |
CA (1) | CA2425869A1 (en) |
CZ (1) | CZ305289B6 (en) |
DE (2) | DE60112962T2 (en) |
IL (3) | IL155214A0 (en) |
MX (1) | MXPA03003544A (en) |
PT (1) | PT1527834E (en) |
WO (1) | WO2002034436A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6554884B1 (en) | 2000-10-24 | 2003-04-29 | H.C. Starck, Inc. | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
US6689187B2 (en) | 1999-02-03 | 2004-02-10 | Cabot Supermetals K.K. | Tantalum powder for capacitors |
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JP3718412B2 (en) * | 2000-06-01 | 2005-11-24 | キャボットスーパーメタル株式会社 | Niobium or tantalum powder and method for producing the same |
KR100663735B1 (en) * | 2001-05-15 | 2007-01-03 | 쇼와 덴코 가부시키가이샤 | Niobium powder, niobium sintered body and capacitor using the sintered body |
US7361202B2 (en) * | 2001-10-01 | 2008-04-22 | Showa Denko K.K. | Tantalum sintered body and capacitor using the sintered body |
US7648553B2 (en) * | 2001-12-10 | 2010-01-19 | Showa Denko K.K. | Niobium alloy, sintered body thereof, and capacitor using the same |
JP2003338433A (en) * | 2002-05-22 | 2003-11-28 | Nec Tokin Corp | Solid electrolytic capacitor, anode body therefor and its manufacturing method |
US6965510B1 (en) * | 2003-12-11 | 2005-11-15 | Wilson Greatbatch Technologies, Inc. | Sintered valve metal powders for implantable capacitors |
US7682362B2 (en) * | 2005-02-01 | 2010-03-23 | Smith & Nephew, Inc. | Lockable orientation stylus |
CN100415640C (en) * | 2005-05-24 | 2008-09-03 | 株洲硬质合金集团有限公司 | Ultra-fine high-nitrogen tantalum nitride powder and its preparation method |
JP5289669B2 (en) * | 2005-06-10 | 2013-09-11 | ローム株式会社 | Method for producing fine powder of Nb compound, method for producing solid electrolytic capacitor using fine powder of Nb compound |
FR2894597B1 (en) * | 2005-12-12 | 2008-04-11 | Ceramique Plastique Sa | MASSIVE MECHANICAL PIECE, IN FRITTE CERAMIC MATERIAL, AND METHOD FOR MANUFACTURING SUCH A BRAKE |
JP2009536266A (en) * | 2006-05-05 | 2009-10-08 | キャボット コーポレイション | Tantalum powder and method for producing the same |
GB0622463D0 (en) * | 2006-11-10 | 2006-12-20 | Avx Ltd | Powder modification in the manufacture of solid state capacitor anodes |
US20080144257A1 (en) * | 2006-12-18 | 2008-06-19 | Yuri Freeman | Anodes for electrolytic capacitors with high volumetric efficiency |
US7731893B2 (en) * | 2006-12-18 | 2010-06-08 | Kemet Electronics Corporation | Method for making anodes for electrolytic capacitor with high volumetric efficiency |
KR20080085294A (en) * | 2007-03-19 | 2008-09-24 | 삼성전기주식회사 | Manufacturing method of tantal condenser |
KR20080085293A (en) * | 2007-03-19 | 2008-09-24 | 삼성전기주식회사 | Manufacturing method of tantal condenser |
US20090279233A1 (en) * | 2008-05-12 | 2009-11-12 | Yuri Freeman | High volumetric efficiency anodes for electrolytic capacitors |
DE102011109756A1 (en) * | 2011-08-09 | 2013-02-14 | H.C. Starck Gmbh | Process for the preparation of electrolytic capacitors made of valve metal powders |
US8349030B1 (en) | 2011-09-21 | 2013-01-08 | Kemet Electronics Corporation | Method for making anodes for high voltage electrolytic capacitors with high volumetric efficiency and stable D.C. leakage |
USRE48439E1 (en) | 2013-09-06 | 2021-02-16 | Greatbatch Ltd. | High voltage tantalum anode and method of manufacture |
US9312075B1 (en) | 2013-09-06 | 2016-04-12 | Greatbatch Ltd. | High voltage tantalum anode and method of manufacture |
US9764388B2 (en) | 2013-12-10 | 2017-09-19 | Ningxia Orient Tantalum Industry Co., Ltd. | Method for preparing tantalum powder of capacitor grade with high nitrogen content, tantalum powder of capacitor grade prepared thereby, and anode and capacitor prepared from tantalum powder |
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US4154609A (en) * | 1976-03-11 | 1979-05-15 | Hermann C. Starck Berlin | Method of producing porous metal bodies for use in the electronic industry |
US5448447A (en) * | 1993-04-26 | 1995-09-05 | Cabot Corporation | Process for making an improved tantalum powder and high capacitance low leakage electrode made therefrom |
US5825611A (en) * | 1997-01-29 | 1998-10-20 | Vishay Sprague, Inc. | Doped sintered tantalum pellets with nitrogen in a capacitor |
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-
2000
- 2000-10-24 US US09/695,512 patent/US6554884B1/en not_active Expired - Lifetime
-
2001
- 2001-10-23 IL IL15521401A patent/IL155214A0/en active IP Right Grant
- 2001-10-23 DE DE60112962T patent/DE60112962T2/en not_active Expired - Lifetime
- 2001-10-23 JP JP2002537471A patent/JP4294951B2/en not_active Expired - Fee Related
- 2001-10-23 EP EP01988636A patent/EP1337371B1/en not_active Expired - Lifetime
- 2001-10-23 EP EP05001377A patent/EP1527834B1/en not_active Expired - Lifetime
- 2001-10-23 WO PCT/US2001/046281 patent/WO2002034436A1/en active IP Right Grant
- 2001-10-23 DE DE60133143T patent/DE60133143T2/en not_active Expired - Lifetime
- 2001-10-23 CZ CZ2003-1149A patent/CZ305289B6/en not_active IP Right Cessation
- 2001-10-23 MX MXPA03003544A patent/MXPA03003544A/en active IP Right Grant
- 2001-10-23 PT PT05001377T patent/PT1527834E/en unknown
- 2001-10-23 KR KR1020037005613A patent/KR100850386B1/en not_active IP Right Cessation
- 2001-10-23 AU AU2002228767A patent/AU2002228767A1/en not_active Abandoned
- 2001-10-23 CA CA002425869A patent/CA2425869A1/en not_active Abandoned
- 2001-10-23 CN CNB018178855A patent/CN1309513C/en not_active Expired - Fee Related
-
2002
- 2002-10-25 US US10/280,295 patent/US6716389B2/en not_active Expired - Fee Related
-
2003
- 2003-06-04 IL IL155214A patent/IL155214A/en not_active IP Right Cessation
-
2006
- 2006-02-07 IL IL173587A patent/IL173587A0/en not_active IP Right Cessation
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US4154609A (en) * | 1976-03-11 | 1979-05-15 | Hermann C. Starck Berlin | Method of producing porous metal bodies for use in the electronic industry |
US5448447A (en) * | 1993-04-26 | 1995-09-05 | Cabot Corporation | Process for making an improved tantalum powder and high capacitance low leakage electrode made therefrom |
US5825611A (en) * | 1997-01-29 | 1998-10-20 | Vishay Sprague, Inc. | Doped sintered tantalum pellets with nitrogen in a capacitor |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6689187B2 (en) | 1999-02-03 | 2004-02-10 | Cabot Supermetals K.K. | Tantalum powder for capacitors |
US6554884B1 (en) | 2000-10-24 | 2003-04-29 | H.C. Starck, Inc. | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
US6716389B2 (en) | 2000-10-24 | 2004-04-06 | H. C. Starck Inc | Tantalum and tantalum nitride powder mixtures for electrolytic capacitors substrates |
Also Published As
Publication number | Publication date |
---|---|
IL173587A0 (en) | 2006-07-05 |
EP1527834A1 (en) | 2005-05-04 |
AU2002228767A1 (en) | 2002-05-06 |
JP4294951B2 (en) | 2009-07-15 |
KR100850386B1 (en) | 2008-08-04 |
US6716389B2 (en) | 2004-04-06 |
IL155214A0 (en) | 2003-11-23 |
MXPA03003544A (en) | 2004-09-10 |
JP2004524674A (en) | 2004-08-12 |
CZ20031149A3 (en) | 2003-10-15 |
DE60133143D1 (en) | 2008-04-17 |
EP1337371A1 (en) | 2003-08-27 |
CN1498144A (en) | 2004-05-19 |
US6554884B1 (en) | 2003-04-29 |
CZ305289B6 (en) | 2015-07-22 |
DE60112962T2 (en) | 2006-05-18 |
EP1337371B1 (en) | 2005-08-24 |
US20030126944A1 (en) | 2003-07-10 |
PT1527834E (en) | 2008-04-23 |
EP1337371A4 (en) | 2004-05-26 |
KR20030051734A (en) | 2003-06-25 |
IL155214A (en) | 2006-08-20 |
CN1309513C (en) | 2007-04-11 |
DE60133143T2 (en) | 2009-03-12 |
EP1527834B1 (en) | 2008-03-05 |
CA2425869A1 (en) | 2002-05-02 |
DE60112962D1 (en) | 2005-09-29 |
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