US3415639A - Method for the manufacture of tantalum and/or niobium powder - Google Patents
Method for the manufacture of tantalum and/or niobium powder Download PDFInfo
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- US3415639A US3415639A US540179A US54017966A US3415639A US 3415639 A US3415639 A US 3415639A US 540179 A US540179 A US 540179A US 54017966 A US54017966 A US 54017966A US 3415639 A US3415639 A US 3415639A
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- tantalum
- niobium
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- per million
- metal
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- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 238000000034 method Methods 0.000 title claims description 9
- 229910052715 tantalum Inorganic materials 0.000 title claims description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims description 6
- WTKKCYNZRWIVKL-UHFFFAOYSA-N tantalum Chemical compound [Ta+5] WTKKCYNZRWIVKL-UHFFFAOYSA-N 0.000 title 1
- 239000000843 powder Substances 0.000 claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052758 niobium Inorganic materials 0.000 claims description 4
- 239000010955 niobium Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- OEIMLTQPLAGXMX-UHFFFAOYSA-I tantalum(v) chloride Chemical compound Cl[Ta](Cl)(Cl)(Cl)Cl OEIMLTQPLAGXMX-UHFFFAOYSA-I 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 3
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 claims description 3
- XITGHTRVSNMXOD-UHFFFAOYSA-N [Nb].ClOCl Chemical compound [Nb].ClOCl XITGHTRVSNMXOD-UHFFFAOYSA-N 0.000 claims description 2
- KSGWBGANTWHAEE-UHFFFAOYSA-N chloro hypochlorite tantalum Chemical compound [Ta].ClOCl KSGWBGANTWHAEE-UHFFFAOYSA-N 0.000 claims description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003832 thermite Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910001026 inconel Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002822 niobium compounds Chemical class 0.000 description 2
- 150000003482 tantalum compounds Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000002730 additional effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G9/042—Electrodes or formation of dielectric layers thereon characterised by the material
-
- 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
-
- 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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
-
- 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
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
Definitions
- the present invention therefore relates to a method for the manufacture of tantalum and/or niobium powders which are suitable for the manufacture of sintered anodes for electrolytic condensers, characterised by reducing tantalum chloride and/or niobium chloride and/or tantalum oxide and/ or niobium oxide with magnesium metal and/ or calcium metal, optionally in the presence of alkali chlorides and/or alkaline earth chlorides, mixing the resulting metal powder, after washing out the salts in a manner which is in itself known, with, at most, the stoichiometric amount of carbon and/or carbide necessary for the formation of CO relative to the amount of oxygen present, purifying the mixture by sintering in vacuo at temperatures of 1600 to 2200 C., hydrogenating the sintered powder in a manner which is in itself known, grinding it and dehydrogenating it.
- the reduction (or ignition) of the tantalum compounds and/or niobium compounds with magnesium metal and/ or calcium metal takes place in the manner which is usual for thermite reactions.
- the magnesium may be used in the form of filings, grit or powder, and an excess is advantageously employed.
- the reaction is preferably carried out in an inert gas atmosphere.
- the thermite composition may, if desired, also be diluted with alkali chloride and/or alkaline earth chlorides.
- the tantalum compounds and/or niobium compounds may be used in the form of oxychlorides or alternatively in the form of double chlorides with alkali chlorides.
- tantalum pentachloride is reduced with magnesium.
- the carbon may be added in the form of carbon 'black or graphite or metal carbide.
- Suitable sintering temperatures are those from 1600 to 2200 C.
- the powder is hydrogenated in a manner which is in itself known, ground, and again dehydrogenated.
- the subject of the present invention also comprises the use of the powders manufactured according to the invention for the manufacture of sintered anodes for electrolytic condensers, as well as the electrolytic condensers containing such sintered anodes.
- the manufacture of the 3,415,639 Patented Dec. 10, 1968 anodes and their incorporation into the electrolytic condensers takes place in a manner which is in itself known.
- EXAMPLE 1 360 parts of powdered TaCl and 74 parts of magnesium grit are mixed under argon and poured into an Inconel tube.
- the Inconel tube is provided with an argon bypass and fixed in a vertical position.
- the tube wall is now heated to red heat at the level of the end of the charge, by means of a burner, as a result of which the reaction mixture is ignited'and burns in a downward direction.
- the pipe wall is cooled with water and the product, which is a solidified salt melt pervaded with spongy metal, is taken out and broken up.
- the metal is isolated by several times leaching out the reaction mass with dilute hydrochloric acid followed by water, and subsequent filtration and drying in a vacuum cabinet.
- the material still contains the following impurities, in parts per million:
- the product is hydrogenated in the known manner.
- the hydrogenated tablets are broken up in a tantalum-lined stamping mill and are then sieved. This material is dehydrogenated in a high vacuum at 700 C.
- the free flowing powder exhibits the .following characteristics:
- BET Specific surface Approx. 0.16 m. g. Oxygen content 1660 parts per million. Carbon content 25 parts per million. Nitrogen content 77 parts per million. Iron content 10 parts per million. Nickel content 10 parts per million. Chromium content .-e 10 parts per million. Magnesium content 1 part per million. Manganese content 1 part per million. Aluminum content 10 parts per million. Silicon content 10 parts per million.
- the two types of anodes are now jointly sintered, with the final sintering temperature being about 2050 C. They are subsequently formed in 0.01% strength phosphoric acid at 200 volt, and their capacity is measured.
- a specific capacity of 2800;f-v. per g. of tantalum was found for the product manufactured according to the invention, and a specific capacity of 2380 .f-v. per g. of tantalum was found for the comparison powder.
- EXAMPLE 2 Specific surface Approx. 0.15 mfl/ g. Oxygen content 2140 parts per million. Carbon content 108 parts per million. Nitrogen content 155 parts per million. Iron content 32 parts per million. Nickel content parts per million. Chromium content 10 parts per million.
- a process for the manufacture of tantalum powders and niobium powders suitable for the manufacture of sintered anodes for electrolytic condensers which oomprises reducing a member selected from the group consisting of tantalum chloride, tantalum oxychloride, niobium chloride, niobium oxychloride, tantalum oxide and niobium oxide with a member selected from the group consisting of magnesium metal and calcium metal, mixing the resulting metal powder, after washing out the salt in a manner which is in itself known, with at most the stoichiometric amount of a member selected from the group consisting of carbon and metal carbide required for the formation of CO relative to the oxygen content present, purifying by sintering in vacuo at temperatures of 1600 to 2200 C., hydrogenating the sintered powder in a manner which is in itself known, grinding it and dehydrogenating it.
- a process according to claim 1 which comprises reducing TaCl with magnesium.
- a process according to claim 1 which comprises using graphite.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Electrolytic Production Of Metals (AREA)
- Carbon And Carbon Compounds (AREA)
Description
United States Patent 3,415,639 METHOD FOR THE MANUFACTURE OF TAN- TALUM AND/0R NIOBIUM POWDER Gustav Daendliker, 'Birsfelden, Alex Jacob, Reinach,
Basel-Laud, and Walter Scheller, Muenclieustein, Switzerland, assignors to Ciba Limited, Basel, Switzerland, a company of Switzerland No Drawing. Filed'Apr. 5, 1966, Ser. No. 540,179 Claims priority, application Switzerland, May 25, 1965, 7,279/65 3 Claims. (Cl. 75-.5)
It is known to use sintered anodes of tantalum or niobium in the manufacture of electrolytic condensers. These anodes are manufactured from the corresponding metal powders. The electrical quality of the anode is affected by the chemical purity and particle size distr bution of the powder as well as by the surface in the sintered shape.
It has now been found that, especially for a high capacity yield, it is not only the 'abovementioned properties of the metal powder used for the anode manufacture which are important, but that additional properties which are determined by the method of manufacture of the metal powder are of great significance. It has been found that particularly advantageous metal powders for the manufacture of anodes may be obtained by thermite reduction. The present invention therefore relates to a method for the manufacture of tantalum and/or niobium powders which are suitable for the manufacture of sintered anodes for electrolytic condensers, characterised by reducing tantalum chloride and/or niobium chloride and/or tantalum oxide and/ or niobium oxide with magnesium metal and/ or calcium metal, optionally in the presence of alkali chlorides and/or alkaline earth chlorides, mixing the resulting metal powder, after washing out the salts in a manner which is in itself known, with, at most, the stoichiometric amount of carbon and/or carbide necessary for the formation of CO relative to the amount of oxygen present, purifying the mixture by sintering in vacuo at temperatures of 1600 to 2200 C., hydrogenating the sintered powder in a manner which is in itself known, grinding it and dehydrogenating it.
The reduction (or ignition) of the tantalum compounds and/or niobium compounds with magnesium metal and/ or calcium metal takes place in the manner which is usual for thermite reactions. The magnesium may be used in the form of filings, grit or powder, and an excess is advantageously employed. The reaction is preferably carried out in an inert gas atmosphere. The thermite composition may, if desired, also be diluted with alkali chloride and/or alkaline earth chlorides. The tantalum compounds and/or niobium compounds may be used in the form of oxychlorides or alternatively in the form of double chlorides with alkali chlorides. In a preferred embodiment of the present method, tantalum pentachloride is reduced with magnesium.
The purification of the metal powder obtained after washing, by treatment with carbon and sintering in vacuo, takes place in a manner which is in itself known. The carbon may be added in the form of carbon 'black or graphite or metal carbide. The use of graphite is preferred. Suitable sintering temperatures are those from 1600 to 2200 C. As a result of the sintering the metal powder is largely freed of metallic and non-metallic contaminants. Following the sintering the powder is hydrogenated in a manner which is in itself known, ground, and again dehydrogenated.
The subject of the present invention also comprises the use of the powders manufactured according to the invention for the manufacture of sintered anodes for electrolytic condensers, as well as the electrolytic condensers containing such sintered anodes. The manufacture of the 3,415,639 Patented Dec. 10, 1968 anodes and their incorporation into the electrolytic condensers takes place in a manner which is in itself known.
EXAMPLE 1 360 parts of powdered TaCl and 74 parts of magnesium grit are mixed under argon and poured into an Inconel tube. The Inconel tube is provided with an argon bypass and fixed in a vertical position. The tube wall is now heated to red heat at the level of the end of the charge, by means of a burner, as a result of which the reaction mixture is ignited'and burns in a downward direction. When the reaction has taken place the pipe wall is cooled with water and the product, which is a solidified salt melt pervaded with spongy metal, is taken out and broken up. The metal is isolated by several times leaching out the reaction mass with dilute hydrochloric acid followed by water, and subsequent filtration and drying in a vacuum cabinet. The material still contains the following impurities, in parts per million:
parts of this material, whose particle size at most reaches 250 are thoroughly mixed with 0.67 part of a fine graphite (particle size less than 40 1) and then pressed into porous tablets. The tablets are slowly heated to 1800 C. (pyrometrically determined, uncorrected) in a high vacuum furnace, and are then kept at this temperature for 30 minutes. The vacuum at the end of the heating period is 10" mm. Hg.
After cooling, the product is hydrogenated in the known manner. The hydrogenated tablets are broken up in a tantalum-lined stamping mill and are then sieved. This material is dehydrogenated in a high vacuum at 700 C. The free flowing powder exhibits the .following characteristics:
Specific surface (BET) Approx. 0.16 m. g. Oxygen content 1660 parts per million. Carbon content 25 parts per million. Nitrogen content 77 parts per million. Iron content 10 parts per million. Nickel content 10 parts per million. Chromium content .-e 10 parts per million. Magnesium content 1 part per million. Manganese content 1 part per million. Aluminum content 10 parts per million. Silicon content 10 parts per million.
For comparison purposes, a powder of similar purity and similar surface was produced from electrolytically deposited tantalum consisting of massive dendrites, by
hydrogenation and grinding.
Specific surface Approx. 0.17 mP/g. Oxygen content 1430 parts per million. Carbon content 58 parts per million. Iron content 10 parts per million. Nickel content 10 parts per million. Chromium content 10 parts per million. Magnesium content 1 part per million. Manganese content 1 part per million. Aluminum content 10 parts per million. Silicon content 10 parts per million.
Crude anodes are pressed from both powders.
The two types of anodes are now jointly sintered, with the final sintering temperature being about 2050 C. They are subsequently formed in 0.01% strength phosphoric acid at 200 volt, and their capacity is measured. A specific capacity of 2800;f-v. per g. of tantalum was found for the product manufactured according to the invention, and a specific capacity of 2380 .f-v. per g. of tantalum was found for the comparison powder.
EXAMPLE 2 Specific surface Approx. 0.15 mfl/ g. Oxygen content 2140 parts per million. Carbon content 108 parts per million. Nitrogen content 155 parts per million. Iron content 32 parts per million. Nickel content parts per million. Chromium content 10 parts per million.
What is claimed is: 1. A process for the manufacture of tantalum powders and niobium powders suitable for the manufacture of sintered anodes for electrolytic condensers, which oomprises reducing a member selected from the group consisting of tantalum chloride, tantalum oxychloride, niobium chloride, niobium oxychloride, tantalum oxide and niobium oxide with a member selected from the group consisting of magnesium metal and calcium metal, mixing the resulting metal powder, after washing out the salt in a manner which is in itself known, with at most the stoichiometric amount of a member selected from the group consisting of carbon and metal carbide required for the formation of CO relative to the oxygen content present, purifying by sintering in vacuo at temperatures of 1600 to 2200 C., hydrogenating the sintered powder in a manner which is in itself known, grinding it and dehydrogenating it.
2. A process according to claim 1 which comprises reducing TaCl with magnesium.
3. A process according to claim 1 which comprises using graphite.
References Cited UNITED STATES PATENTS 3,203,793 8/1965 Hand 174 3,295,951 1/1967 Fincham et a1. 750.5
FOREIGN PATENTS 657,781 2/1962 Canada.
L. DEWAYNE RUTLEDGE, Primary Examiner.
Claims (1)
1. A PROCESS FOR THE MANUFACTURE OF TANTALUM POWDERS AND NIOBIUM POWDERS SUITABLE FOR THE MANUFACTURE OF SINTERED ANODES FOR ELECTROLYTIC CONDENSERS, WHICH COMPRISES REDUCING A MEMBER SELECTED FROM THE GROUP CONSISTING OF TANTALUM CHLORIDE, TANTALUM OXYCHLORIDE, NIOBIUM CHLORIDE, NIOBIUM OXYCHLORIDE, TANTALUM OXIDE AND NIOBIUM OXIDE WITH A MEMBER SELECTED FROM THE GROUP CONSISTING OF MAGNESIUM METAL AND CALCIUM METAL, MIXING THE RESULTING METAL POWDER, AFTER WASHING OUT THE SALT IN A MANNER WHICH IS IN ITSELF KNOWN, WITH AT MOST THE STOICHIOMETRIC AMOUNT OF A MEMBER SELECTED FROM THE GROUP CONSISTING OF CARBON AND METAL CARBIDE REQUIRED FOR THE FORMATION OF CO RELATIVE TO THE OXYGEN CONTENT PRESENT, PURIFYING BY SINTERING IN VACUO AT TEMPERATURES OF 1600 TO 2200*C., HYDROGENATING THE SINTERING POWDER IN A MANNER WHICH IS IN ITSELF KNOWN, GRINDING IT AND DEHYDROGENATING IT.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH727965 | 1965-05-25 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3415639A true US3415639A (en) | 1968-12-10 |
Family
ID=4322630
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US540179A Expired - Lifetime US3415639A (en) | 1965-05-25 | 1966-04-05 | Method for the manufacture of tantalum and/or niobium powder |
Country Status (4)
Country | Link |
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US (1) | US3415639A (en) |
BE (1) | BE681427A (en) |
GB (1) | GB1094283A (en) |
NL (1) | NL6607155A (en) |
Cited By (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3473915A (en) * | 1968-08-30 | 1969-10-21 | Fansteel Inc | Method of making tantalum metal powder |
US3499753A (en) * | 1966-02-02 | 1970-03-10 | Starck Hermann C Fa | Process for the preparation of tantalum powder |
US3635693A (en) * | 1969-01-27 | 1972-01-18 | Starck Hermann C Fa | Method of producing tantalum or niobium powder from compact bodies |
US3647420A (en) * | 1968-06-06 | 1972-03-07 | Starck Hermann C Fa | Process for producing high-purity niobium and tantalum |
US3647415A (en) * | 1967-10-25 | 1972-03-07 | Show Denko Kk | Tantalum powder for sintered capacitors |
US3867129A (en) * | 1974-02-05 | 1975-02-18 | Metallurgie Hoboken | Anodically oxidizable metal powder |
US3914507A (en) * | 1970-03-20 | 1975-10-21 | Sherritt Gordon Mines Ltd | Method of preparing metal alloy coated composite powders |
US4017302A (en) * | 1976-02-04 | 1977-04-12 | Fansteel Inc. | Tantalum metal powder |
US4128421A (en) * | 1973-03-29 | 1978-12-05 | Marsh Harold G | Tantalum powder for producing an embrittlement-resistant wire |
US4445931A (en) * | 1980-10-24 | 1984-05-01 | The United States Of America As Represented By The Secretary Of The Interior | Production of metal powder |
US4508563A (en) * | 1984-03-19 | 1985-04-02 | Sprague Electric Company | Reducing the oxygen content of tantalum |
EP1075884A2 (en) * | 1996-11-07 | 2001-02-14 | Cabot Corporation | Niobium powders and niobium electrolytic capacitors |
US20050039577A1 (en) * | 1999-03-19 | 2005-02-24 | Habecker Kurt A. | Method of making niobium and other metal powders |
US20060107788A1 (en) * | 2002-06-13 | 2006-05-25 | Toru Okabe | Method for producing metal powder and formed product of raw material for metal |
WO2023109170A1 (en) * | 2021-12-15 | 2023-06-22 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder for capacitor by reducing tantalum oxide using alkaline earth metal |
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CN114210973B (en) * | 2021-12-15 | 2023-03-24 | 宁夏东方钽业股份有限公司 | Production method of tantalum powder and tantalum powder obtained by same |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA657781A (en) * | 1963-02-12 | Schussler Mortimer | Tantalum powder and process for making same | |
US3203793A (en) * | 1963-01-28 | 1965-08-31 | Du Pont | Porous columbium and tantalum materials |
US3295951A (en) * | 1965-02-02 | 1967-01-03 | Nat Res Corp | Production of metals |
-
1966
- 1966-03-30 GB GB14169/66A patent/GB1094283A/en not_active Expired
- 1966-04-05 US US540179A patent/US3415639A/en not_active Expired - Lifetime
- 1966-05-23 BE BE681427D patent/BE681427A/xx unknown
- 1966-05-24 NL NL6607155A patent/NL6607155A/xx unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA657781A (en) * | 1963-02-12 | Schussler Mortimer | Tantalum powder and process for making same | |
US3203793A (en) * | 1963-01-28 | 1965-08-31 | Du Pont | Porous columbium and tantalum materials |
US3295951A (en) * | 1965-02-02 | 1967-01-03 | Nat Res Corp | Production of metals |
Cited By (18)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3499753A (en) * | 1966-02-02 | 1970-03-10 | Starck Hermann C Fa | Process for the preparation of tantalum powder |
US3647415A (en) * | 1967-10-25 | 1972-03-07 | Show Denko Kk | Tantalum powder for sintered capacitors |
US3647420A (en) * | 1968-06-06 | 1972-03-07 | Starck Hermann C Fa | Process for producing high-purity niobium and tantalum |
US3473915A (en) * | 1968-08-30 | 1969-10-21 | Fansteel Inc | Method of making tantalum metal powder |
US3635693A (en) * | 1969-01-27 | 1972-01-18 | Starck Hermann C Fa | Method of producing tantalum or niobium powder from compact bodies |
US3914507A (en) * | 1970-03-20 | 1975-10-21 | Sherritt Gordon Mines Ltd | Method of preparing metal alloy coated composite powders |
US4128421A (en) * | 1973-03-29 | 1978-12-05 | Marsh Harold G | Tantalum powder for producing an embrittlement-resistant wire |
US3867129A (en) * | 1974-02-05 | 1975-02-18 | Metallurgie Hoboken | Anodically oxidizable metal powder |
US4017302A (en) * | 1976-02-04 | 1977-04-12 | Fansteel Inc. | Tantalum metal powder |
US4445931A (en) * | 1980-10-24 | 1984-05-01 | The United States Of America As Represented By The Secretary Of The Interior | Production of metal powder |
US4508563A (en) * | 1984-03-19 | 1985-04-02 | Sprague Electric Company | Reducing the oxygen content of tantalum |
FR2561258A1 (en) * | 1984-03-19 | 1985-09-20 | Sprague Electric Co | PROCESS FOR REDUCING THE OXYGEN CONTENT OF THE TANTALE |
EP1075884A2 (en) * | 1996-11-07 | 2001-02-14 | Cabot Corporation | Niobium powders and niobium electrolytic capacitors |
EP1075884A3 (en) * | 1996-11-07 | 2005-10-05 | Cabot Corporation | Niobium powders and niobium electrolytic capacitors |
US20050039577A1 (en) * | 1999-03-19 | 2005-02-24 | Habecker Kurt A. | Method of making niobium and other metal powders |
US7156893B2 (en) * | 1999-03-19 | 2007-01-02 | Cabot Corporation | Method of making niobium and other metal powders |
US20060107788A1 (en) * | 2002-06-13 | 2006-05-25 | Toru Okabe | Method for producing metal powder and formed product of raw material for metal |
WO2023109170A1 (en) * | 2021-12-15 | 2023-06-22 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder for capacitor by reducing tantalum oxide using alkaline earth metal |
Also Published As
Publication number | Publication date |
---|---|
BE681427A (en) | 1966-11-23 |
GB1094283A (en) | 1967-12-06 |
NL6607155A (en) | 1966-11-28 |
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