US20060174727A1 - Method for the production of metal powders or metal hydride powders of the elements ti,zr, hf,v,nb.ta and cr - Google Patents
Method for the production of metal powders or metal hydride powders of the elements ti,zr, hf,v,nb.ta and cr Download PDFInfo
- Publication number
- US20060174727A1 US20060174727A1 US10/564,427 US56442704A US2006174727A1 US 20060174727 A1 US20060174727 A1 US 20060174727A1 US 56442704 A US56442704 A US 56442704A US 2006174727 A1 US2006174727 A1 US 2006174727A1
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- United States
- Prior art keywords
- process according
- oxide
- metal
- proportion
- impurities
- Prior art date
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Classifications
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- 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
-
- 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
- B22F9/18—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
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/02—Hydrides of transition elements; Addition complexes thereof
-
- 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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
-
- 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
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
Description
- The invention provides a process for preparing metal powders and metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr.
- Metal powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr and powdered hydrides of these metals are used, for example, in the following areas of application: titanium for the production of titanium components for the aircraft and automobile industries, for the production of titanium alloys and for the production of sintered AlNiCo magnets; titanium, zirconium and hafnium in the pyro-industry, for the production of electric detonator systems (e.g. in airbags) and ignition delay elements, in getter materials in vacuum tubes, lamps, vacuum equipment and gas purification plants; hafnium as an alloying element in niobium, tantalum, titanium, molybdenum and tungsten alloys; vanadium as an alternative metal electrode in metal-hydride/nickel-hydride batteries and in TiAl6V4 alloys; niobium in the production of equipment for the chemicals industry and as an alloying element for ZrNb alloys (nuclear industry) and NbHfTi alloys (highly heat-resistant materials for jet engines or explosion chambers); tantalum in capacitors.
- As a result of the sometimes very high requirements placed on the reliability of the products mentioned above (e.g. airbag detonators), it is desirable to produce the metal powders or metal hydride powders reproducibly and with identical properties from batch to batch (in particular with respect to burning time, ignition point, mean particle size, particle size distribution and oxidation value).
- The metal powders can be produced by a reduction process. In this case, oxides of the metals (Ti, Zr, Hf, V, Nb, Ta and Cr) are reduced, for example with calcium or calcium hydride. The reduction process is performed in a vessel which can be sealed, rendered inert and evacuated. The reducing agents(s) are normally added in excess. After reduction, the oxides of the reducing agents being produced are removed by leaching with acid and then washing with water. The acid content of the metal powder obtained is between 1 and 5% when using this method.
- Alternatively, the metal powders can be obtained from the relevant metal by hydrogenation and dehydrogenation (HDH method). The relevant metal is hydrogenated and, in this then brittle form, can be crushed mechanically to give powders of the desired fineness. In order to avoid damage due to the uptake of oxygen and nitrogen, ultrapure hydrogen has to be used for the hydrogenation process. Crushing the hydrogenated metal to the desired particle size must also be performed in a pure protective gas atmosphere (e.g. helium or argon). Subsequent removal of the hydrogen is achieved by decomposing the metal hydride under vacuum at elevated temperature. Metal hydride powders are produced in the same way. The dehydrogenation process is then simply omitted.
- A disadvantage of the metal powders and hydrides produced in this way is, inter alia, that these do not have reproducible burning times, reproducible specific surface areas, reproducible particle size distributions or reproducible ignition points.
- The object of the invention is to overcome the disadvantages of the prior art and to provide metal powders and metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr that have a burning time of 4 s per 50 cm to 3000 s per 50 cm and an ignition point of 160° C. to 400° C. and above this in individual cases.
- The burning time, expressed in s/50 cm is determined as follows. The substance being tested is first sieved through two sieves with mesh sizes of 250 μm and 45 μm in order to eliminate problematic agglomerates. Optionally, the sample can be carefully moved about with a brush during this procedure. The fine material that has passed through the 45 μm sieve is used to determine the burning time. 15 g of the sample are placed loosely in a metal channel, described below, smoothed out with a piece of cardboard and any excess removed by wiping it off. The metal channel is provided with two marks that are located at a spacing of 500 mm from each other. Upstream of the first mark, an additional approximately pea-sized amount of substance is applied and is ignited with a burner. With the aid of a time-exposure photograph, the time required to pass through the distance between the first and the last mark is now determined. The analytical result for burning time is cited with the dimensions [s/50 cm].
- The ignition point is determined as follows: 10 g of the substance being tested are introduced into a pre-heated so-called “ignition block” and the temperature at which self-ignition occurs is measured. The ignition block, consisting of an iron cube with an edge-length of 70 mm and with drilled holes for the material and a thermocouple (20 mm and 8 mm diameter, each hole 35 mm deep, distance between mid-points of hole 18 mm), is preheated to a temperature slightly below the ignition temperature, using a blowlamp, after inserting the thermometer or thermocouple in the drilled hole provided for this purpose. This temperature is determined using a trial sample. A heaped spatula (10 g) of the metal powder or hydride being tested is now introduced into the material hole in the pre-heated ignition block and the block is heated with a full blowlamp flame until the powder self-ignites. The temperature reached at that time is the ignition point.
- Furthermore, it is desirable that the metal powder or metal hydride powder has a metal or metal hydride content of at least 75 wt. %, preferably at least 88 wt. %, particularly preferably 90 wt. %, a mean particle diameter of 1 to 15 μm, a preferred particle size distribution (measured by means of laser diffraction) of 1 to 20 μm and a BET specific surface area of 0.2 to 5 m2/g.
- The mean particle diameter is determined as follows using a “Fisher sub-sieve size particle sizer” (called FSSS in the following). A description of this method of measurement can be found in “Instructions, Fisher Model 95 Sub-Sieve Sizer, catalog number 14-311, part no. 14579 (rev. C), published 01-94” from Fisher Scientific. Express reference is made here to this description of the measurement process.
- The object is achieved by a process for preparing metal powders or metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr, in which an oxide of these elements is mixed with a reducing agent and this mixture is heated in an oven, optionally under an atmosphere of hydrogen (metal hydrides are then formed), until the reduction reaction starts, the reaction product is leached and then the product is washed and dried, wherein the oxide used has a mean particle size of 0.5 to 20 μm, preferably 1 to 6 μm, a BET specific surface area of 0.5 to 20 m2/g, preferably 1 to 12 m2/g, and particularly preferably 1 to 8 m2/g, and a minimum content of 94 wt. %, preferably 96 wt. % and particularly preferably 99 wt. %.
- The proportion of Fe and Al impurities in the oxide is preferably <0.2 wt. %, particularly preferably <0.1 wt. % each (each calculated as the oxide). The proportion of Si impurities in the oxide is preferably <1.5 wt. %, particularly preferably <0.3 wt. % (calculated as SiO2). The proportion of Na impurities in the oxide is preferably <0.05 wt. % (calculated as Na2O). The proportion of P impurities in the oxide is preferably <0.2 wt. % (calculated as P2O5). The loss on ignition of the oxide at 1000° C. (constant weight) is preferably <1 wt. %, particularly preferably <0.5 wt. %. The tamped down bulk density according to EN ISO 787-11 (previously DIN 53194) of the oxide is preferably 800 to 1600 kg/m3. A proportion of up to 15 wt. % of the oxide can be replaced by additives consisting of MgO, CaO, Y2O3 or CeO2.
- It was found that, by targeted selection of the oxidic raw materials with the properties described above and then performing the process, products are obtained that have a burning time of 4 s per 50 cm to 3000 s per 50 cm, an ignition energy of 1 μJ to 1 mJ, a mean particle size of 1 to 8 μm, a BET specific surface area of 0.2 to 5 m2/g, an ignition point of 160° C. to 400° C. and above that in individual cases, wherein reproducible particle size distributions are obtained in each case. The combination of average particle size and specific surface area within each of the ranges cited above for the oxidic starting compound, together with the minimum content cited, leads to the desired product.
- The reducing agents preferably used may be: alkaline earth metals and alkali metals and the hydrides of each. Magnesium, calcium, calcium hydride and barium or defined mixtures of these are particularly preferred. The reducing agent preferably has a minimum content of 99 wt. %, particularly preferably 99.5 wt. %.
- Powdered pure metals, partially hydrogenated metals or metal hydrides are obtained, depending on the amount of hydrogen added during the reduction process in the oven. The higher the hydrogen content of the process product, the greater is the burning time (i.e. the metal burns more slowly) and the higher the ignition point, and vice versa.
- Leaching the reaction product is preferably performed with hydrochloric acid and this is particularly preferably used in a slight excess.
- The invention is explained in more detail using the examples given below.
- 43 kg of ZrO2 (powdered zirconium oxide (natural baddeleyite) with the following properties: ZrO2+HfO2 min. 99.0%; HfO2 1.0-2.0%; SiO2 max. 0.5%; TiO2 max. 0.3%; Fe2O3 max. 0.1%; loss on ignition max. 0.5%; mean particle size (using FSSS) 4 -6 μm; proportion of monoclinic crystal structure min. 95%; specific surface area (BET) 0.5-1.5 m2/g) and
- 31.5 kg of Ca (calcium in the form of granules with the following properties: Ca min. 99.3%; Mg max. 0.7%)
- were mixed for 20 minutes under an atmosphere of argon. Then the mixture was introduced into a container. The container was placed in an oven that was subsequently closed and filled with argon up to a pressure of 100 hPa above atmospheric pressure. The reaction oven was heated to a temperature of about 1250° C. over the course of one hour. As soon as the reaction material had reached the temperature of the oven, the reduction reaction started:
ZrO2+2Ca→Zr+2CaO - 60 minutes after switching on the oven heating system, it was then switched off. When the temperature had dropped to <50° C., the reaction material was removed from the crucible and leached with concentrated hydrochloric acid. A zirconium powder with the following analytical characteristics was obtained: Zr+Hf 96.1%; Hf 2.2%; O 0.7%; Si 0.21%; H 0.16%; Mg 0.11%; Ca 0.13%; Fe 0.07%; Al 0.1%; Cl 0.002%; mean particle size 4.9 μm; particle size distribution d50 9.9 μm; specific surface area 0.5 m2/g; ignition point 220° C.; burning time 80 sec/50 cm.
- 36 kg of ZrO2 (powdered zirconium oxide with the following properties: ZrO2+HfO2 min. 99.0%; HfO2 1.0-2.0%; SiO2 max. 0.2%; TiO2 max. 0.25%; Fe2O3 max. 0.02%; loss on ignition max. 0.4%; mean particle size (using FSSS) 3-5 μm; proportion of monoclinic crystal structure min. 96%; specific surface area (BET) 3.0-4.0 m2/g) and
- 17 kg of Mg (magnesium in the form of granules with the following properties: Mg min. 99.8%; bulk density max. 0.4-0.5 g/cm3)
- were placed in a container in the oven, in the same way as described in example 1. The oven was heated to 1050° C. As soon as the reaction material reached the temperature of the oven, the reduction reaction started:
ZrO2+2Mg→Zr+2MgO - The oven heating system was switched off 20 minutes after the start of the reduction reaction. When the temperature had dropped to <50° C., the reaction material was removed from the crucible and leached with concentrated hydrochloric acid. A zirconium powder with the following analytical characteristics was obtained: Zr+Hf 91.7%; O 1.6%; Si 0.14%; H 0.13%; Mg 0.59%; Ca<0.001%; Fe 0.045%; mean particle size 2.5 μm; particle size distribution d50 4.3 μm; ignition point 175° C.; burning time 24 sec/50 cm.
Claims (23)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US15/705,721 US20180094336A1 (en) | 2003-07-15 | 2017-09-15 | Process for preparing metal powders and metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10332033A DE10332033A1 (en) | 2003-07-15 | 2003-07-15 | Process for the preparation of metal powders or of metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr |
DE10332033.4 | 2003-07-15 | ||
PCT/EP2004/007032 WO2005007906A1 (en) | 2003-07-15 | 2004-06-29 | Method for the production of metal powders or metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2004/007032 A-371-Of-International WO2005007906A1 (en) | 2003-07-15 | 2004-06-29 | Method for the production of metal powders or metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US15/705,721 Continuation US20180094336A1 (en) | 2003-07-15 | 2017-09-15 | Process for preparing metal powders and metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Publications (1)
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US20060174727A1 true US20060174727A1 (en) | 2006-08-10 |
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Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
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US10/564,427 Abandoned US20060174727A1 (en) | 2003-07-15 | 2004-06-29 | Method for the production of metal powders or metal hydride powders of the elements ti,zr, hf,v,nb.ta and cr |
US15/705,721 Abandoned US20180094336A1 (en) | 2003-07-15 | 2017-09-15 | Process for preparing metal powders and metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
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US15/705,721 Abandoned US20180094336A1 (en) | 2003-07-15 | 2017-09-15 | Process for preparing metal powders and metal hydride powders of the elements ti, zr, hf, v, nb, ta and cr |
Country Status (10)
Country | Link |
---|---|
US (2) | US20060174727A1 (en) |
EP (1) | EP1644544B1 (en) |
JP (2) | JP5692950B2 (en) |
KR (1) | KR100969116B1 (en) |
AT (1) | ATE348197T1 (en) |
CA (1) | CA2532128C (en) |
DE (2) | DE10332033A1 (en) |
RU (1) | RU2369651C2 (en) |
UA (1) | UA91494C2 (en) |
WO (1) | WO2005007906A1 (en) |
Cited By (13)
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US20060279924A1 (en) * | 2001-11-19 | 2006-12-14 | Otter Products, Llc | Protective enclosure for personal digital assistant case having integrated back lighted keyboard |
US7263032B2 (en) | 1999-10-04 | 2007-08-28 | H2O Audio, Inc. | System for housing an audio system in an aquatic environment |
US20090095130A1 (en) * | 2007-10-15 | 2009-04-16 | Joseph Smokovich | Method for the production of tantalum powder using reclaimed scrap as source material |
US20100272999A1 (en) * | 2008-01-23 | 2010-10-28 | Ulrich Gerhard Baudis | Phlegmatized metal powder or alloy powder and method and reaction vessel for the production thereof |
US20100313709A1 (en) * | 2008-02-28 | 2010-12-16 | Ikarashi Yasushi | Method for manufacturing alloy powders based on titanium, zirconium and hafnium, alloyed with the elements ni, cu, ta, w, re, os and ir |
WO2013006600A1 (en) * | 2011-07-05 | 2013-01-10 | Orchard Material Technology, Llc | Retrieval of high value refractory metals from alloys and mixtures |
WO2015050637A1 (en) * | 2013-08-19 | 2015-04-09 | University Of Utah Research Foundation | Producing a titanium product |
CN105063394A (en) * | 2015-08-06 | 2015-11-18 | 王海英 | Titanium or titanium alloy material preparing method |
CN105525108A (en) * | 2015-12-16 | 2016-04-27 | 东北大学 | Method for preparing magnesium-calcium alloy through aluminothermic reduction |
CN109290586A (en) * | 2018-10-19 | 2019-02-01 | 重庆大学 | A kind of preparation method of high-purity vanadium powder |
WO2020115568A1 (en) * | 2018-12-04 | 2020-06-11 | Surendra Kumar Saxena | A method of producing hydrogen from water |
US10907239B1 (en) | 2020-03-16 | 2021-02-02 | University Of Utah Research Foundation | Methods of producing a titanium alloy product |
US11033965B2 (en) * | 2017-05-23 | 2021-06-15 | Northeastern University | Method for preparing reduced titanium powder by multistage deep reduction |
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US7399335B2 (en) | 2005-03-22 | 2008-07-15 | H.C. Starck Inc. | Method of preparing primary refractory metal |
DE102008009133B4 (en) * | 2008-02-06 | 2012-04-12 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Process for the production of metal powders and metal powder produced in this way |
GB201218675D0 (en) * | 2012-10-17 | 2012-11-28 | Univ Bradford | Improved method for metal production |
KR101476308B1 (en) * | 2013-04-30 | 2014-12-24 | 한국기계연구원 | Apparatus for reducing metal oxide with magnesium, and the method for reducing metal oxide using the same |
GB201309173D0 (en) * | 2013-05-21 | 2013-07-03 | Roberts Mark P | Novel process and product |
CN105014089B (en) * | 2014-04-28 | 2017-06-06 | 湖南华威景程材料科技有限公司 | A kind of method that vacuum carbon reduction prepares hafnium metal powder |
JP6842079B2 (en) * | 2016-08-26 | 2021-03-17 | 白畑 實隆 | Method for producing reduced minerals and method for producing reduced minerals having intracellular sugar uptake activity |
KR101991499B1 (en) * | 2018-12-18 | 2019-06-20 | 주식회사 엔에이피 | Method for preparing calcium hydride |
RU2725652C1 (en) * | 2019-06-14 | 2020-07-03 | Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "Кольский научный центр Российской академии наук" (ФИЦ КНЦ РАН) | Method of producing zirconium powder |
KR102205493B1 (en) * | 2019-09-25 | 2021-01-21 | 주식회사 엔에이피 | Method for preparing nonferrous metal powderr |
RU2737103C1 (en) * | 2020-07-15 | 2020-11-24 | Федеральное государственное бюджетное учреждение науки Федеральный исследовательский центр "Кольский научный центр Российской академии наук" (ФИЦ КНЦ РАН) | Method of producing zirconium powder |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1602542A (en) * | 1921-01-06 | 1926-10-12 | Westinghouse Lamp Co | Reduction of rare-metal oxides |
US2411524A (en) * | 1943-10-04 | 1946-11-26 | Mctal Hydrides Inc | Process for the production of zirconium hydride |
US4681623A (en) * | 1985-06-24 | 1987-07-21 | Sumitomo Metal Mining Company Limited | Process for producing alloy powder containing rare earth metals |
US6136062A (en) * | 1998-10-13 | 2000-10-24 | H. C. Starck Gmbh & Co. Kg | Niobium powder and a process for the production of niobium and/or tantalum powders |
US20020066338A1 (en) * | 2000-10-10 | 2002-06-06 | Shekhter Leonid N. | Metalothermic reduction of refractory metal oxides |
US20030082097A1 (en) * | 1995-10-12 | 2003-05-01 | Brown Patrick M. | Process for producing niobium and tantalum compounds |
US6558447B1 (en) * | 1999-05-05 | 2003-05-06 | H.C. Starck, Inc. | Metal powders produced by the reduction of the oxides with gaseous magnesium |
US20030110890A1 (en) * | 2001-09-29 | 2003-06-19 | Jilin He | Process for the production of high surface area tantalum and/or niobium powders |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH05163511A (en) * | 1991-12-10 | 1993-06-29 | Mitsui Mining & Smelting Co Ltd | Production of alloy powder |
WO2000067936A1 (en) * | 1998-05-06 | 2000-11-16 | H.C. Starck, Inc. | Metal powders produced by the reduction of the oxides with gaseous magnesium |
US6171363B1 (en) * | 1998-05-06 | 2001-01-09 | H. C. Starck, Inc. | Method for producing tantallum/niobium metal powders by the reduction of their oxides with gaseous magnesium |
JPH11335702A (en) * | 1998-05-28 | 1999-12-07 | Nichia Chem Ind Ltd | Magnetic powder |
JP3610942B2 (en) * | 2001-10-12 | 2005-01-19 | 住友金属鉱山株式会社 | Method for producing niobium and / or tantalum powder |
DE102008000433A1 (en) * | 2008-02-28 | 2009-09-03 | Chemetall Gmbh | Process for the production of alloy powders based on titanium, zirconium and hafnium alloyed with the elements Ni, Cu, Ta, W, Re, Os and Ir |
-
2003
- 2003-07-15 DE DE10332033A patent/DE10332033A1/en not_active Ceased
-
2004
- 2004-06-29 US US10/564,427 patent/US20060174727A1/en not_active Abandoned
- 2004-06-29 RU RU2006104309/02A patent/RU2369651C2/en active
- 2004-06-29 AT AT04740425T patent/ATE348197T1/en not_active IP Right Cessation
- 2004-06-29 DE DE502004002325T patent/DE502004002325D1/en active Active
- 2004-06-29 JP JP2006519794A patent/JP5692950B2/en active Active
- 2004-06-29 UA UAA200601576A patent/UA91494C2/en unknown
- 2004-06-29 EP EP04740425A patent/EP1644544B1/en active Active
- 2004-06-29 CA CA2532128A patent/CA2532128C/en active Active
- 2004-06-29 KR KR1020067000962A patent/KR100969116B1/en active IP Right Grant
- 2004-06-29 WO PCT/EP2004/007032 patent/WO2005007906A1/en active IP Right Grant
-
2011
- 2011-12-26 JP JP2011283751A patent/JP2012107337A/en active Pending
-
2017
- 2017-09-15 US US15/705,721 patent/US20180094336A1/en not_active Abandoned
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1602542A (en) * | 1921-01-06 | 1926-10-12 | Westinghouse Lamp Co | Reduction of rare-metal oxides |
US2411524A (en) * | 1943-10-04 | 1946-11-26 | Mctal Hydrides Inc | Process for the production of zirconium hydride |
US4681623A (en) * | 1985-06-24 | 1987-07-21 | Sumitomo Metal Mining Company Limited | Process for producing alloy powder containing rare earth metals |
US20030082097A1 (en) * | 1995-10-12 | 2003-05-01 | Brown Patrick M. | Process for producing niobium and tantalum compounds |
US6136062A (en) * | 1998-10-13 | 2000-10-24 | H. C. Starck Gmbh & Co. Kg | Niobium powder and a process for the production of niobium and/or tantalum powders |
US6558447B1 (en) * | 1999-05-05 | 2003-05-06 | H.C. Starck, Inc. | Metal powders produced by the reduction of the oxides with gaseous magnesium |
US20020066338A1 (en) * | 2000-10-10 | 2002-06-06 | Shekhter Leonid N. | Metalothermic reduction of refractory metal oxides |
US20030110890A1 (en) * | 2001-09-29 | 2003-06-19 | Jilin He | Process for the production of high surface area tantalum and/or niobium powders |
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US7981191B2 (en) | 2007-10-15 | 2011-07-19 | Hi-Temp Specialty Metals, Inc. | Method for the production of tantalum powder using reclaimed scrap as source material |
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Also Published As
Publication number | Publication date |
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ATE348197T1 (en) | 2007-01-15 |
JP5692950B2 (en) | 2015-04-01 |
EP1644544B1 (en) | 2006-12-13 |
KR100969116B1 (en) | 2010-07-09 |
US20180094336A1 (en) | 2018-04-05 |
CA2532128C (en) | 2016-04-05 |
KR20060032637A (en) | 2006-04-17 |
RU2006104309A (en) | 2006-07-10 |
JP2009513819A (en) | 2009-04-02 |
WO2005007906A1 (en) | 2005-01-27 |
EP1644544A1 (en) | 2006-04-12 |
DE502004002325D1 (en) | 2007-01-25 |
CA2532128A1 (en) | 2005-01-27 |
JP2012107337A (en) | 2012-06-07 |
DE10332033A1 (en) | 2005-02-03 |
RU2369651C2 (en) | 2009-10-10 |
UA91494C2 (en) | 2010-08-10 |
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