CA2285786A1 - Niobium powder and a process for the production of niobium and/or tantalum powders - Google Patents

Niobium powder and a process for the production of niobium and/or tantalum powders Download PDF

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Publication number
CA2285786A1
CA2285786A1 CA002285786A CA2285786A CA2285786A1 CA 2285786 A1 CA2285786 A1 CA 2285786A1 CA 002285786 A CA002285786 A CA 002285786A CA 2285786 A CA2285786 A CA 2285786A CA 2285786 A1 CA2285786 A1 CA 2285786A1
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Canada
Prior art keywords
reduction
niobium
stage
process according
oxide
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
Application number
CA002285786A
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French (fr)
Other versions
CA2285786C (en
Inventor
Josua Loffelholz
Frank Behrens
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HC Starck GmbH
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HC Starck GmbH
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Publication of CA2285786A1 publication Critical patent/CA2285786A1/en
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Publication of CA2285786C publication Critical patent/CA2285786C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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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
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052—Sintered electrodes
    • H01G9/0525—Powder therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G33/00—Compounds of niobium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G35/00—Compounds of tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/24—Obtaining niobium or tantalum
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/18—Reducing step-by-step
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/045—Alloys based on refractory metals
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

The process comprises the reduction of niobium and/or tantalum oxides by means of alkaline earth metals and/or rare earth metals, wherein the first reduction stage is carried out as far as an average composition corresponding to (Nb, Ta)O X
where x =
0.5 to 1.5 and before the second stage the reduction product from the first stage is freed from alkaline earth oxides and/or rare earth metal oxides which are formed (and optionally from excess alkaline earth metal and/or rare earth metal) by washing with mineral acids.

Claims (11)

1. A process for producing niobium and/or tantalum powders by the reduction of their corresponding niobium and/or tantalum oxides, wherein the reduction is carried out in two stages at a controlled temperature, the reductions being carried out by use of a reducing agent selected from the group consisting of alkaline earth metals and rare earth metals, the first reaction stage being carried out until an average composition corresponding to (Nb, Ta)O X where x = 0.5 to 1.5 is reached, then, before the second stage, freeing the reduction product from the first stage from oxides of the reducing agent by washing with one or more mineral acids, and then conducting the second reduction stage to produce powder of the metal.
2. A process according to Claim 1, wherein between the first and second stages the reduction product is also freed of excess reducing agent.
3. A process according to either of Claims 1 or 2, wherein in the first reduction stage the melt of the reducing agent metal is placed in a reaction vessel in at least a 1.25-fold excess with respect to the oxygen content of the niobium and/or tantalum oxide and the oxide is gradually metered into the melt in such a way that the reduction reaction exotherm-affected temperature of the first reduction stages does not fall below 750°C and does not exceed 950°C.
4. A process according to Claim 3, wherein the melt is stirred during the metered addition of the oxide.
5. A process according to Claim 4, wherein the first reduction stage is conducted continuously by the simultaneous or alternating metered addition of oxide and reducing metal into a melt of the reducing metal placed in a vessel with continuous or batch-wise discharge of the reduction product.
6. A process according to either of Claims 1 or 2, wherein following the first reduction stage and/or the second reduction stage the reduction product which is obtained is treated with dopant substances containing P, B, S, and/or N.
7. A process according to either of Claims 1 or 2, wherein the production of niobium powder Nb2O5 is used as the niobium oxide and magnesium is used as the reducing metal.
8. Niobium powder agglomerates with a primary grain size of diameter 0.1 to 1 µm and an agglomerate diameter distribution corresponding to a D50 of 100 to 300 µm as determined by Mastersizer.
9. Niobium powder agglomerates according to Claim 8 with a BET specific surface of 2 to 15 m2/g.
10. Niobium powder agglomerates according either of Claims 8 or 9 of a physical and electrical property set such that after sintering at 1,150°C for 20 minutes and forming at 40 volts the sintered products of such agglomerates exhibit a capacitance of 70,000 to 360,000 µFV/g and a leakage current density of 0.5 to 1.5 nA/µFV.
11. Niobium powder agglomerates according to either of Claims 8 or 9 of a physical and electrical property set such that after sintering at 1,150°C for 20 minutes and forming at 16 volts the sintered products of such agglomerates exhibit a capacitance of 120,000 to 380,000 µFV/g and a leakage current density of 0.7 to 2 nA/µFV.
CA002285786A 1998-10-13 1999-10-08 Niobium powder and a process for the production of niobium and/or tantalum powders Expired - Fee Related CA2285786C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19847012.6 1998-10-13
DE19847012A DE19847012A1 (en) 1998-10-13 1998-10-13 Niobium powder and process for its manufacture

Publications (2)

Publication Number Publication Date
CA2285786A1 true CA2285786A1 (en) 2000-04-13
CA2285786C CA2285786C (en) 2009-12-01

Family

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Family Applications (1)

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CA002285786A Expired - Fee Related CA2285786C (en) 1998-10-13 1999-10-08 Niobium powder and a process for the production of niobium and/or tantalum powders

Country Status (15)

Country Link
US (1) US6136062A (en)
EP (1) EP0997542B1 (en)
JP (3) JP4215911B2 (en)
KR (1) KR100625726B1 (en)
CN (1) CN1180910C (en)
AT (1) ATE235571T1 (en)
AU (1) AU755289B2 (en)
BR (1) BR9904431A (en)
CA (1) CA2285786C (en)
DE (2) DE19847012A1 (en)
EE (1) EE04160B1 (en)
HK (1) HK1027522A1 (en)
IL (1) IL132317A (en)
PT (1) PT997542E (en)
RU (1) RU2238821C2 (en)

Cited By (1)

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US6375704B1 (en) 1999-05-12 2002-04-23 Cabot Corporation High capacitance niobium powders and electrolytic capacitor anodes

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